WO1996028043A1 - Continuous chewing gum base manufacturing process using addition of lubricating agents at a plurality of feed inlet locations - Google Patents

Continuous chewing gum base manufacturing process using addition of lubricating agents at a plurality of feed inlet locations Download PDF

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Publication number
WO1996028043A1
WO1996028043A1 PCT/US1995/003172 US9503172W WO9628043A1 WO 1996028043 A1 WO1996028043 A1 WO 1996028043A1 US 9503172 W US9503172 W US 9503172W WO 9628043 A1 WO9628043 A1 WO 9628043A1
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WO
WIPO (PCT)
Prior art keywords
mixer
chewing gum
gum base
mixing
zone
Prior art date
Application number
PCT/US1995/003172
Other languages
French (fr)
Inventor
Joo H. Song
Donald J. Townsend
Original Assignee
Wm. Wrigley Jr. Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wm. Wrigley Jr. Company filed Critical Wm. Wrigley Jr. Company
Priority to EP95913684A priority Critical patent/EP0759700A4/en
Priority to PCT/US1995/003172 priority patent/WO1996028043A1/en
Publication of WO1996028043A1 publication Critical patent/WO1996028043A1/en

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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23GCOCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G4/00Chewing gum
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23GCOCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G4/00Chewing gum
    • A23G4/06Chewing gum characterised by the composition containing organic or inorganic compounds
    • A23G4/08Chewing gum characterised by the composition containing organic or inorganic compounds of the chewing gum base

Definitions

  • This invention is directed to a continuous process for the manufacture of chewing gum bases.
  • a typical chewing gum base includes one or more elastomers, one or more fillers, one or more elastomer solvents, softening agents and optional plastic polymers and miscellaneous colors, flavors and antioxidants. Due primarily to the difficulty in melting and dispersing the elastomers homogeneously among the other gum base ingredients, gum base manufacture has typically been a tedious and time-consuming batch process. For example, one such conventional process uses a sigma blade batch mixer having a front to rear blade speed ratio of 2:1, and a mixing temperature of about 80-125°C.
  • 0 273 809 in the name of General Foods France, discloses a process for making nonadhesive chewing gum base by blending elastomer and filler components together in an industrial mill type mixer to form a nonadhesive premix, dividing the premix into fragments, and blending the premix fragments and at least one other nonadhesive gum base component together in a powder mixer.
  • the premix fragments and other base components can be added to an extruder along with other chewing gum components to accomplish direct manufacture of chewing gum.
  • French Patent Publication No. 2 635 44 also in the name of General Foods France, discloses a process for making a gum base concentrate using a twin screw extruder.
  • the concentrate is prepared by mixing high molecular weight elastomers and plasticizers in desired proportions and feeding them into the extruder. Mineral fillers are added to the extruder downstream of the feed inlet of the elastomer/plasticizer blend.
  • the resulting gum base concentrate has a high level of elastomers.
  • the concentrate can then be mixed with the other gum base ingredients to provide a complete gum base.
  • U.S. Patent No. 3,995,064, issued to Ehrgott et al. discloses the continuous manufacture of gum base using a sequence of mixers or a single variable mixer.
  • Patent No. 4,187,320 issued to Koch et al., discloses a two stage process for preparing a chewing gum base.
  • a solid elastomer, an elastomer solvent, and an oleaginous plasticizer are combined and mixed together under high shear.
  • a hydrophobic plasticizer, a non-toxic vinyl polymer, and an emulsifier are added to the mixture and mixed using high shear.
  • U.S. Patent No. 4,305,962 issued to Del Angel, discloses an elastomer/resin masterbatch formed by mixing a finely ground ester gum resin with a latex elastomer to form an emulsion, coagulating the emulsion using sodium chloride and sulfuric acid, separating the coagulated solid crumbs from the liquid phase, washing the solid crumbs, and removing the excess water.
  • U.S. Patent No. 4,459,311 issued to DeTora et al., discloses making gum base using two separate mixers - a high intensity mixer for pre-plasticizing the elastomer in the presence of a filler, followed by a medium intensity mixer for ultimately blending all the gum base components together.
  • U.S. Patent No. 4,968,511 issued to D'Amelia et al., discloses that chewing gum can be made directly in a one-step compounding process (without making an intermediate gum base) if certain vinyl polymers are used as the elastomer portion.
  • Continuous gum base manufacturing processes while desirable, present a number of difficulties.
  • One of these is that continuous equipment has a given processing length once set up for operation. This length is limited in practice by what is commercially available, and is often less than what may be desired from the gum base manufacture's standpoint.
  • continuous mixing operations have less degrees of freedom than traditional batch processes. For example, in a batch process, if longer mixing times are needed, it is a simple matter to continue mixing. However, the residence time in a continuous mixer is a function of the operating speed and feed rates. Therefore, to change the mixing time, some other factor must be adjusted and accommodated. Further, in a batch process, additional ingredients can be added at any time. Commercial continuous mixers have a limited number of feed inlets at fixed positions. Therefore the additional ingredients can be added at only preset points in the mixing process.
  • dispersive and distributive mixing can be independently varied and controlled.
  • changes to one type of mixing will often also affect the other type of mixing. If the amount of the machine used for high shear mixing is increased, there is less machine available for distributive mixing. Also, if the speed is increased, heat may be generated beyond the ability of the cooling capabilities of the equipment.
  • the properties of the chewing gum base is a function of the gum base ingredients and the mixing conditions that are applied to those ingredients.
  • the mixing conditions are also a function of the gum base ingredients, as well as the type of mixing elements being used, the temperature and viscosity of the ingredients and the fullness of the mixer barrel. For example, if there is a high content of elastomer solvent in the base, less aggressive mixing occurs in the mixer because the elastomer solvent acts as a lubricant. Conversely, if the filler level in the gum base is high, the mixing is very aggressive, and may cause excessive breakup of the elastomer.
  • the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having at least one dispersive mixing zone and at least one distributive mixing zone and a plurality of spatially separated feed inlets, at least a portion of the hard elastomer and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located before the end of the dispersive mixing zone and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located downstream of the dispersive mixing zone and before the end of the distributive mixing zone; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
  • chewing gum base ingredients including a hard elastomer, filler and one or more
  • the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer comprising a plurality of spatially separated feed inlets and a barrel having a predetermined length, at least a portion of the hard elastomer and a portion of the lubricating agents being introduced into one or more feed inlet ⁇ located within the first 40% of the barrel length and a portion of the lubricating agents being introduced through one or more feed inlets located within the last 60% of the barrel length; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
  • chewing gum base ingredients including a hard elastomer, filler and one or more lubricating agents
  • the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having a plurality of spatially separated feed inlets, high shear mixing elements and low shear mixing elements downstream from the high shear mixing elements, at least a portion of the hard elastomer and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located at or before the high shear mixing elements and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located downstream of the high shear mixing elements and at or before the low shear mixing elements; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
  • chewing gum base ingredients including a hard elastomer, filler and one or
  • the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having at least one dispersive mixing zone and at least one distributive mixing zone and a plurality of spatially separated feed inlets, at least a portion of the hard elastomer, a portion of the lubricating agents and at least a portion of the filler being introduced into the mixer through one or more feed inlets located before the end of the dispersive mixing zone and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located downstream of the dispersive mixing zone and before the end of the distributive mixing zone, the ratio of the amount of lubricating agents added before the end of the dispersive mixing zone to the amount of lubricating agents added downstream of the dispersive mixing zone being optimized so that the gum base contains a desired amount of lubricating agents and the dispersive mixing
  • chewing gum base is produced in a continuous process. If desired, the output can be used to supply a continuous chewing gum production line or, if sufficient mixing can be accomplished in the first part of the mixer, the complete chewing gum can be produced in one mixer. Second, the average residence time for gum base ingredients is reduced from hours to minutes. Third, all of the necessary addition and gum base compounding steps can be performed in sequence, preferably using a single continuous mixing apparatus. Fourth, the preferred embodiment provides improved metering and mixing of intermediate and low viscosity gum base ingredients by adding these ingredients in the liquid state under pressure.
  • the invention is effective for a wide range of gum base compositions, including different gum base elastomers and elastomer percentages, without requiring preblending or other pretreatment of the elastomers.
  • the gum base can be produced on demand, eliminating finished base inventory. This allows maximum flexibility to react to market demands and formula changes.
  • high quality gum bases including those containing high levels of fats, oil and/or low melting point waxes, can be made on a continuous basis.
  • FIG. 1 depicts a schematic representation of a twin screw extruder set up for use in practicing the present invention.
  • FIG. 2 depicts a set of shearing disks used in the extruder of FIG. 1.
  • FIG. 3 depicts a set of toothed elements used in the extruder of FIG. 1.
  • FIG. 4 depicts a set of kneading disks used in the extruder of FIG. 1.
  • FIG. 5 depicts a plurality of kneading disks, set up in a helical fashion, to form kneading blocks.
  • FIGS. 6a-e depict schematic sequential representations of gum base ingredients during the mixing process.
  • FIG. 7 is a perspective view of a single flat mixing paddle as used in practicing another embodiment of the invention.
  • FIG. 8 is a side view of the mixing paddle of FIG. 1.
  • FIG. 9a is a front view of the mixing paddle of
  • FIG. 7, shown at zero degrees rotation (referred to as the no. 1 position) .
  • FIG. 9b is a front view of the mixing paddle of FIG. 7, shown at 45 degrees counter-clockwise rotation (referred to as the no. 2 position) .
  • FIG. 9c is a front view of the mixing paddle of FIG. 7, shown at 90 degrees counter-clockwise rotation (referred to as the no. 3 position) .
  • FIG. 9d is a front view of the mixing paddle of FIG. 1, shown at 135 degrees counter-clockwise rotation (referred to as the no. 4 position) .
  • FIG. 10a is a perspective view of a feeding element (not a paddle element) used in the feed areas of a paddle mixer.
  • FIG. 10b is a front view of the feed element of FIG. 10a.
  • FIG. 11a is a perspective view of a forward helical mixing paddle which can be used in a paddle mixer.
  • FIG. lib is a front view of the forward helical mixing paddle of FIG. 11a.
  • FIG. lie is based on a top view of the forward helical mixing paddle of 11a, showing only the top intersection line 92 superimposed over the bottom intersection line 90, and a reference line 91.
  • FIG. 12a is a perspective view of a reverse helical mixing paddle which can be used in a paddle mixer.
  • FIG. 12b is a front view of the reverse helical mixing paddle of FIG. 12a.
  • FIG. 12c is based on a top view of the reverse helical mixing paddle of FIG. 12a, showing only the top intersection line 92 superimposed over the bottom intersection line 90, and a reference line 91.
  • FIG. 13 is a perspective view of an overall paddle mixing configuration of a paddle mixer.
  • FIG. 14 is a schematic illustration of a barrel and feeder arrangement which can be used in conjunction with the paddle mixer configuration shown in FIG. 13.
  • FIG. 15 is a cross-sectional view taken along line 15-15 of FIG. 14, showing the relationship between the rotating paddles and the barrel wall.
  • FIG. 16 is a schematic illustration of two paddle mixers arranged in series.
  • FIG. 17 is a partial exploded perspective view of a Buss high efficiency, blade-and-pin mixer used to practice another embodiment of the invention, illustrating a mixing barrel and mixing screw arrangement.
  • FIG. 18a is a perspective view of an on-screw element used on the upstream side of a restriction ring assembly in the high efficiency mixer of FIG. 17.
  • FIG. 18b is a perspective view of an on-screw element used on the downstream side of the restriction ring assembly in the high efficiency mixer of FIG. 17.
  • FIG. 18c is a perspective view of a restriction ring assembly used in the high efficiency mixer of FIG. 17.
  • FIG. 19 is a perspective view showing the relative positioning of the elements of FIGS. 18a, 18b and 18c in the high efficiency mixer of FIG. 17.
  • FIG. 20 is a perspective view of a low-shear mixing screw element used in the high efficiency mixer of FIG. 17.
  • FIG. 21 is a perspective view of a high-shear mixing screw element used in the high efficiency mixer of FIG. 17.
  • FIG. 22 is a perspective view of a barrel pin element used in the high efficiency mixer of FIG. 17.
  • FIG. 23 is a schematic diagram of an arrangement of mixing barrel pins and ingredient feed ports used with the high efficiency mixer of FIG. 17.
  • FIG. 24 is a schematic diagram of a presently preferred mixing screw configuration used with the high efficiency mixer of FIG. 17. DETAILED DESCRIPTION OF THE DRAWINGS AND PREFERRED EMBODIMENTS OF THE INVENTION
  • gum base ingredients play a functional role during both mixing of the gum base and in the final chew characteristics of the chewing gum made from the base.
  • the filler acts to increase the shear.
  • Some of the other gum base ingredients act as lubricating agents, reducing the shear.
  • Most elastomer solvents, soft elastomers, plastic polymers and softening agents generally act as lubricating agents in continuous gum base manufacturing processes.
  • Some lubricating agents such as polyisobutylene and the elastomer solvents cause the elastomer to disentangle, while others are not miscible with the elastomer and act only to lubricate the mixing and shearing operations.
  • the amount of lubricating agents introduced into the mixer prior to the distributive mixing zone may therefore often be less than the amount of the lubricating agents desired in the final gum base.
  • the methods of the present invention introduce the lubricating agents at a plurality of feed inlets so that a desired amount of shear can be achieved in a limited portion of the mixer, yet the final gum base can include all of the elastomer, filler and lubricating agents desired from a ⁇ ensory and cost standpoint.
  • the portion of the lubricating agent added before the dispersive mixing will be one that acts as a solvent for the hard elastomer.
  • the dispersive mixing can be accomplished in the first 40% of the barrel length of a continuous mixer. Therefore, in one embodiment of the invention, the first portion of lubricating agents will be introduced within the first 40% of the barrel length, and the second portion is added in the last 60% of the barrel length.
  • the split of lubricating agents between one feed inlet and another can be split between types of lubricating agents, such as elastomer solvents and soft elastomers, or more preferably a split of one particular lubricating agent.
  • the terpene resin used in the gum base may preferably be split and added at two or more feed inlets.
  • the invention also contemplates a method of optimizing the process for making chewing gum base in a continuous process by adjusting the ratio of lubricating agents being introduced at the different feed inlets until the proper mixing is achieved. For instance, in one set of experiments, the same gum base ingredients were added at the same places in the mixer for each run, except that the elastomer solvent was split at various ratios between 85:15 and 55:45 as it was added at two different points to the mixer. The desired ratio that will result in optimum processing, and the range of ratios that will be experimented with, will of course depend on the gum base formulation, the type of mixer being used, and the arrangement of mixing elements in the mixer.
  • the chewing gum base made by the process of the present invention will be the same as bases made by conventional processes, and can thereafter be made into conventional chewing gums, including bubble gum, by conventional methods.
  • the methods of production are well known and therefore not repeated here.
  • specialized chewing gum such as nonadhesive chewing gum and bubble gum, will use specialized gum base ingredients.
  • those gum base ingredients can be combined using the processes herein described.
  • a chewing gum composition typically comprises a water-soluble bulk portion, a water-insoluble chewable gum base portion and typically water-insoluble flavoring agents.
  • the water-soluble portion dissipates with a portion of the flavoring agent over a period of time during chewing.
  • the gum base portion is retained in the mouth throughout the chew.
  • the insoluble gum base generally comprises elastomers, elastomer solvents, softening agents and inorganic fillers.
  • Plastic polymers such as polyvinyl acetate, which behave somewhat as plasticizers, are also often included.
  • Other plastic polymers that may be used include polyvinyl laurate, polyvinyl alcohol and polyvinyl pyrrolidone.
  • Elastomers may constitute about 5 to about 95 percent by weight of the gum base, preferably between 10 and 70 percent by weight and most preferably between 15 and 45 percent by weight.
  • Elastomers may include polyisobutylene, butyl rubber (isobutylene-isoprene copolymer) , styrene butadiene rubber, polyisoprene and butadiene rubber, as well as natural rubbers such as smoked or liquid latex and guayule, as well as natural gums such as jelutong, lechi caspi, perillo, massaranduba balata, massaranduba chocolate, nispero, rosindinha, chicle, gutta hang kang or mixtures thereof.
  • Elastomer used in chewing gum base can generally be categorized as hard elastomers or soft elastomers.
  • Hard elastomers which are most commonly butyl rubber and styrene butadiene rubber, generally have a high molecular weight, typically a Flory molecular weight over 200,000.
  • a typical butyl rubber used in chewing gum base has a Flory molecular weight of about 400,000.
  • Hard elastomers are those which require high shear, dispersive mixing to be utilized in chewing gum base. Hard elastomers generally do not flow at room temperature, even over an extended period of time, and are not pumpable even when heated to temperatures just below which substantial degradation occurs.
  • Soft elastomers have a lower molecular weight, typically a Flory molecular weight under 100,000.
  • Polyisobutylene and polybutadiene are typically soft elastomers.
  • a typical polyisobutylene used in chewing gum base has a Flory molecular weight of about 53,000.
  • Soft elastomers are generally pumpable at temperatures normally used to make chewing gum base, and will flow at room temperature, though often very slowly.
  • Flory molecular weight sometimes a Stodinger molecular weight is specified. Stodinger molecular weights are generally 1/3 to 1/5 of Flory molecular weights.
  • the polyisobutylene having a Flory molecular weight of 53,000 has a Stodinger molecular weight of about 12,000.
  • Elastomer solvents may constitute from about 0 to about 75 percent by weight of the gum base, preferably 5 to 45 percent by weight and most preferably 10 to 30 percent by weight.
  • Elastomer solvents include natural rosin esters such as glycerol ester of wood rosin, glycerol ester of partially hydrogenated rosin, glycerol ester of polymerized rosin, glycerol ester of partially dimerized rosin, glycerol ester of rosin, pentaerythritol esters of partially hydrogenated rosin, methyl and partially hydrogenated methyl esters of rosin, pentaerythritol ester of rosin, resin ester of glycerol abietate or mixtures thereof.
  • Elastomer solvents also include synthetics such as terpene resins derived from alpha-pinene, beta-pinene and/or d-limonene.
  • Softening agents include oils, fats, waxes and emulsifiers.
  • Oils and fats sometimes referred to as plasticizers, include tallow, lard, hydrogenated and partially hydrogenated vegetable oils, such as soybean oil, cotton seed oil, palm oil, palm kernel oil, coconut oil, sunflower oil and corn oil, cocoa butter, and lipids made from triglycerides of fatty acids.
  • Commonly employed waxes include polywax, paraffin, microcrystalline and natural waxes such as candelilla, beeswax and carnauba. Paraffin waxes may be considered to be plasticizers.
  • Microcrystalline waxes, especially those with a high degree of crystallinity may be considered as bodying agents or textural modifiers.
  • Emulsifiers which also sometimes have plasticizing properties, include glycerol monostearate, lecithin, mono and diglycerides of fatty acids, glycerol mono and distearate, triacetin, acetylated monoglyceride, and glycerol triacetate.
  • the gum base typically also includes a filler component.
  • the filler component may be calcium carbonate, magnesium carbonate, talc, dicalcium phosphate or the like.
  • the filler may constitute between about 5 and about 60 percent by weight of the gum base.
  • the filler comprises about 5 to about 50 percent by weight of the gum base.
  • gum bases may also contain optional ingredients such as antioxidants, colors and flavors.
  • the temperature attained in the mixer often varies over the length of the mixer.
  • the peak temperature in the dispersive mixing zone where high shear mixing elements are located will preferably be over 175°F, more preferably over 250°F and most preferably over 300°F, and even 350°F for some gum base manufacturing processes.
  • the insoluble gum base may constitute between about 5 to about 80 percent by weight of the gum. More typically the insoluble gum base comprises between 10 and 50 percent by weight of the gum and most often about 20 to about 35 percent by weight of the gum.
  • the water soluble portion of the chewing gum may include softeners, bulk sweeteners, high intensity sweeteners, flavoring agents and combinations thereof.
  • Softeners are added to the chewing gum in order to optimize the chewability and mouth feel of the gum.
  • the softeners which are also known as plasticizers or plasticizing agents, generally constitute between about 0.5-15% by weight of the chewing gum.
  • the softeners may include glycerin, lecithin, and combinations thereof.
  • Aqueous sweetener solutions such as those containing sorbitol, hydrogenated starch hydrolysates, corn syrup and combinations thereof, may also be used as softeners and binding agents in chewing gum.
  • Bulk sweeteners constitute between 5-95% by weight of the chewing gum, more typically 20-80% by weight of the chewing gum and most commonly 30-60% by weight of the chewing gum.
  • Bulk sweeteners may include both sugar and sugarless sweeteners and components.
  • Sugar sweeteners may include saccharide containing components including but not limited to sucrose, dextrose, maltose, dextrin, dried invert sugar, fructose, levulose, galactose, corn syrup solids, and the like, alone or in combination.
  • Sugarless sweeteners include components with sweetening characteristics but are devoid of the commonly known sugars.
  • Sugarless sweeteners include but are not limited to sugar alcohols such as sorbitol, mannitol, xylitol, hydrogenated starch hydrolysates, maltitol, and the like, alone or in combination.
  • High intensity sweeteners may also be present and are commonly used with sugarless sweeteners. When used, high intensity sweeteners typically constitute between 0.001-5% by weight of the chewing gum, preferably between 0.01-1% by weight of the chewing gum. Typically, high intensity sweeteners are at least 20 times sweeter than sucrose.
  • sucralose aspartame, salts of acesulfame, alitame, saccharin and its salts, cyclamic acid and its salts, glycyrrhizin, dihydrochalcones, thaumatin, monellin, and the like, alone or in combination.
  • Combinations of sugar and/or sugarless sweeteners may be used in chewing gum.
  • the sweetener may also function in the chewing gum in whole or in part as a water soluble bulking agent. Additionally, the softener may provide additional sweetness such as with aqueous sugar or alditol solutions.
  • Flavor should generally be present in the chewing gum in an amount within the range of about 0.l- 15% by weight of the chewing gum, preferably between about 0.2-5% by weight of the chewing gum, most preferably between about 0.5-3% by weight of the chewing gum.
  • Flavoring agents may include essential oils, synthetic flavors or mixtures thereof including but not limited to oils derived from plants and fruits such as citrus oils, fruit essences, peppermint oil, spearmint oil, other mint oils, clove oil, oil of wintergreen, anise and the like. Artificial flavoring agents and components may also be used in the flavor ingredient of the invention. Natural and artificial flavoring agents may be combined in any sensorially acceptable fashion. Optional ingredients such as colors, emulsifiers, pharmaceutical agents and additional flavoring agents may also be included in chewing gum.
  • a continuous mixer means one mixer or a plurality of mixers in series.
  • Three specific types of continuous mixing equipment are described in detail below and are shown in the attached drawings: twin screw extruders, paddle mixers and blade-and-pin mixers, which are specialized single screw extruders. Extruders are preferred for use in the present invention, particularly the blade-and-pin mixer.
  • Twin Screw Extruders are preferred for use in the present invention, particularly the blade-and-pin mixer.
  • the invention may be carried out on a twin screw extruder such as depicted schematically in FIG. 1.
  • the twin screw extruder used to practice the preferred embodiment of the invention will be set up with several different feed inlet locations where chewing gum base ingredients can be added.
  • the screws inside the barrel of the extruder are equipped with different types of elements along the length of the screws.
  • the different mixing zones are sometimes referred to as processing zones, and described by the type of elements employed in the zones.
  • the barrel is typically made up of different sections. These sections may be heated or cooled independent of other sections. Heating and cooling is thus typically done by region of the extruder barrel, which generally coincides with the barrel sections. These regions of heating or cooling may or may not coincide with processing zones, depending on the lengths of the barrel sections and the elements in the processing zones.
  • Conveying elements generally have flights spiraling along the elements with wide gaps between the flights. These elements are used at feed inlet zones to quickly move material into the body of the extruder.
  • Compression elements have flights with a pitch that narrows as the material moves along the flights. This results in compression and high pressure in the forward direction, which is required to force material downstream and through the other elements.
  • Reverse conveyance elements have flights that are angled opposite those of the conveying elements. The flights rotate in a direction that would force material upstream.
  • Shearing disks impart high shearing forces on the material in the extruder, resulting in highly dispersive mixing.
  • the shearing disks opposite one another on the two different screws have close fitting disk/slot elements, as depicted in FIG. 2.
  • Toothed elements as depicted in FIG. 3, have gear-like teeth that oppose a cylindrical spacer shaft on the other screw. Toothed elements impart highly distributive mixing. Often the toothed elements are made in matched sets, with a cylindrical shaft portion and a toothed portion as one unit.
  • Kneading disks, as shown in FIG. 4 have an elliptical shape, and produce a kneading action in the material passing through the extruder. Often a plurality of kneading disks will be placed next to each other in a helical arrangement, as shown in FIG. 5, referred to as kneading blocks.
  • Highly distributive mixing can also be accomplished using reverse conveyance elements that have portions missing from the flights to allow flow counter to the direction of compression. These missing portions may be arranged as a groove through the flights cut parallel to the length of the element. Also, kneading blocks followed by reverse conveyance elements, to build up high back pressure, also produce highly distributive mixing.
  • Mixing-restriction elements produce a high back pressure and some mixing without overly restricting throughput. For this reason, nozzles or orifices are not suitable as mixing-restriction elements.
  • reverse conveyance elements provide back pressure, and are thus mixing-restriction elements.
  • Shearing disks like those shown in FIG. 2, also produce a high back pressure and are thus another example of a mixing- restriction element.
  • the high back pressure is important so that other elements, such as those that produce highly distributive or highly dispersive mixing, will be able to function properly.
  • mixing-restriction elements are used after each mixing zone. It is most preferable to use a mixing- restriction element just prior to the gum base exiting the extruder.
  • twin screw extruders These various types of elements, and other elements useful in twin screw extruders, are well known in the art and are commercially available. The elements are often specifically designed for the different types of commonly available twin screw extruders, which include co-rotation, counter rotation, intermeshing and tangential twin screw extruders. Elements intended for similar functions will vary in design depending on the type of extruder for which they are intended.
  • Non-intermeshing polygon element sold by the Farrel Corporation, 25 Main Street, Ansonia, Conn. 06401, for the Farrel-Rockstedt co-rotating twin screw extruder. It is believed that the non-intermeshing polygons produce dispersive mixing.
  • the dispersive mixing disentangles the elastomers with a minimum amount of degradation of the polymer chains.
  • the average molecular weight will not be reduced below the average molecular weight of the same polymers mixed into gum base using conventional processes.
  • An adequate dispersive mixing will produce a smooth, rubbery fluid, with no detectable lumps of rubber. If only a few lumps of rubber are present they may be screened out or dispersed during subsequent mixing steps. However, if the number or size of lumps is excessive, or the processed elastomers and fillers are in the form of an agglomeration or grainy mass, the dispersive mixing applied is inadequate.
  • the distributive mixing should be sufficient to produce a homogeneous gum base, rather than a material that appears to be "sweating", or that has a marbled or swiss cheese texture.
  • the highly distributive mixing is sufficient to incorporate softening agents, particularly fats, oils and waxes, to the same degree these softening agents are incorporated in conventional chewing gum base manufacturing processes.
  • a twin screw extruder 10 is set up with a first feed inlet location 12 adjacent a first processing zone 21 fitted with conveying elements 31, conveying and compres ⁇ ion elements 32 and compression elements 35.
  • the second processing zone 23 is equipped with a combination of toothed elements 33, as depicted in FIG. 3, and several sets of shearing disks 34, as depicted in FIG. 2.
  • the extruder 10 is equipped with a port 16 which is connected to a vacuum source (not shown) .
  • the third processing zone 24 contains additional conveying elements 31, conveying and compression elements 32 and compression elements 35.
  • a second feed inlet 13 is provided in the extruder adjacent this second set of conveying elements 31, for feeding additional gum base ingredients into the third processing zone 24. Feed inlet 13 allows for the addition of powdered ingredients as well as liquid ingredients from pump 41.
  • the fourth processing zone 25 is fitted with kneading disks 36.
  • the twin screw extruder 10 has another inlet 15 connected to a pump 43 and a feed inlet 14 in the form of a port connected to a side feeder 42, which may be a single or twin screw extruder, or even a gear pump which can generate high pressure.
  • the fifth processing zone 26 is fitted with conveying elements 31, conveying and compression elements 32 and compression elements 35, which force the gum base ingredients into the sixth and final processing zone 28. Zone 28 contains two sets of toothed elements 33, followed by reverse elements 39 and shearing disks 34. After passing through the shearing disks 34, the gum base ingredients exit the extruder 10.
  • the extruder 10 may be set up with heated tanks 44 and 45, connected respectively to pumps 41 and 43, for this purpose.
  • Other commonly used equipment such as equipment to monitor the temperature and heat or cool the extruder, is not shown in FIG. 1.
  • the equipment will also include conventional weighing and feeding devices for continuously adding granulated or powdered ingredients. All of the ingredients are preferably fed into the extruder by equipment that is controlled to operate at a steady state; although during startup it may be preferable to start feeding some ingredients before others, and to feed the ingredients in at different rates than those desired for steady-state operation. It will be understood that FIG.
  • FIG. 1 shows the various components in their respective order from the standpoint of flow through the extruder 10.
  • the screws are mounted in a horizontal side-to-side position and feed inlets, especially those open to the atmosphere like the inlet 12 and 13, are placed vertically above the screws.
  • FIG. 1 is preferred for particular gum bases outlined in the examples below, other arrangements may be preferred for other gum bases.
  • FIG. l depicts an extruder with three general areas of ingredient addition and six processing zones. For some gum bases, two, four or more ingredient feeding zones may be used, with different numbers of processing zones.
  • FIG. l depicts an extruder with three general areas of ingredient addition and six processing zones. For some gum bases, two, four or more ingredient feeding zones may be used, with different numbers of processing zones.
  • FIG. 1 also depicts the use of one set each of long conveying elements 31, conveying and compression elements 32 and compression elements 35 in the first processing zone 21, a short set of conveying and compression elements 32 in zones 24 and 26, and a short set of conveying elements 31 and compression elements 35 in zone 26. In reality, one, two or more elements of different types and length may be used in these zones.
  • FIG. 1 also depicts one set of toothed elements 33 and three sets of shearing disks 34 in zone 23, but different numbers of these elements, or different elements all together, may be used.
  • zones 25 and 28 different types of elements that produce distributive mixing may be used, dependent on the gum ingredients being mixed in those zones and the type of extruder being used.
  • FIGS. 6a-e represent the state of various gum base ingredients as they are compounded into chewing gum base.
  • the high molecular weight (hard) elastomer 51 and medium molecular weight elastomer 52 are both in the form of granules or particles in which the elastomer molecules are tightly bound together.
  • the filler 53 is in particulate form, but may not be homogeneously mixed with the elastomers 51 and 52.
  • the elastomer solvent 54 may be present in the form of droplets. As mixing begins, depicted in FIG. 6b, the elastomer solvent 54 becomes associated with the elastomers 51 and 52.
  • the filler 53 With the presence of the filler 53, elastomer solvent 54 and heat, the granules begin to come apart into individual elastomer molecules. Also, the filler 53 becomes more evenly distributed, and may have its particle size reduced. As the process continues, the elastomers 51 and 52 become disentangled, as shown in FIG. 6c. This disentangling is the result of subjecting the elastomers 51 and 52 to highly dispersive mixing.
  • the lower viscosity ingredients such as polyvinyl acetate 55
  • this material will also be in discrete particles, or droplets as it melts.
  • Further mixing and further ingredient additions, such as waxes 56 and emulsifiers 57, are subjected to distrib ⁇ utive mixing, as depicted in FIG. 6e.
  • Continued highly distributive mixing produces a homogeneous chewing gum base, wherein discrete particles or droplets are not detectible by sensory perception.
  • the elastomer may be added at the first feed inlet 12 along with elastomer solvent such as resins and the filler. However, especially lower weight elastomers may be added at least partially at the second feed inlet 13. Portions of the filler may also be added at the second feed inlet 13. Polyvinyl acetate may be added via a powder feeder or the single screw extruder 42, or a twin screw extruder or gear pump, at the feed inlet port 14, while melted fats and waxes and oils are added at the last feed inlet 15. This will result in the filler, elastomer and some lubricating agents being subjected to highly dispersive mixing first before lower viscosity ingredients are added.
  • the toothed elements 38, reverse elements 39 and shearing disk 40 after feed inlet 15 result in highly distributive mixing of all of the low viscosity gum base ingredients with the other gum base ingredients.
  • a preferred small scale extruder is a model LSM 30.34 counter-rotational, intermeshing and tangential twin screw extruder from Leistritz, N ⁇ renberg, Germany.
  • Other acceptable twin screw extruders include the Japan Steel Works Model TEX30HSS32.5PW-2V intermeshing co- and counter-rotating twin screw extruder, also known as the Davis Standard D-Tex Model, distributed by Crompton & Knowles Corporation, #1 Extrusion Dr. , Pawcatuck, CT 06379, and either the co-rotating or counter-rotating intermeshing twin screw extruders from Werner &
  • a Werner & Pfleiderer co-rotational twin screw extruder can go up to a length to diameter (L/D) ratio of 48.
  • the Japan Steel Works Model TEX30HSS32.5PW-2V extruder may be equipped to have an L/D of 58.
  • a mixing paddle 85 having a flat (non-helical) configuration is shown in FIGS. 7-9.
  • the term "mixing paddle” is defined herein as a four-sided mixing element having two flat surfaces 86 and 87, and two concave surfaces 88 and 89.
  • the flat surfaces are parallel to each other and intersect only the concave surfaces.
  • the concave surfaces oppose each other and intersect each other at two lines 90 and 91.
  • a non-circular (preferably square) opening 94 passes through the center of each mixing paddle 85, in a direction perpendicular to the flat surfaces 86 and 87, and intersects both flat surfaces.
  • the openings 94 are used for mounting a plurality of paddles on rotating shafts, in a predetermined sequence (FIG. 13) .
  • the mixing paddles 85 can be positioned on a shaft at the same or different rotational angles relative to each other.
  • the "No. 1 position" is defined pursuant to FIG. 9a, wherein a straight line drawn on the flat surface 87 and intersecting the lines
  • the "No. 2 position” is defined pursuant to FIG. 9b, wherein a straight line drawn on the flat surface 87 and intersecting the lines 90 and 92 is 45 degrees counter-clockwise from the reference line.
  • the "No. 3 position” is defined pursuant to FIG. 9c, wherein a straight line drawn on the flat surface 87 and intersecting the lines 90 and 92 is 90 degrees counter ⁇ clockwise from the reference line.
  • the "No. 4 position” is defined pursuant to FIG. 9d, wherein a straight line drawn on the flat surface 87 and intersecting the lines 90 and 92 is 135 degrees counter-clockwise from the reference line.
  • paddles 85 in FIGS. 9a-d are symmetrical, there is no need to further define the relative rotational positions of the paddles for angles of 180, 225, 270 and 315 degrees from the reference line.
  • a paddle having a rotational position of 180 degrees coincides exactly with a paddle having a rotational angle of zero (FIG. 9a) .
  • a paddle having a rotational angle of 225 degrees coincides exactly with a paddle having a rotation angle of 45 degrees (FIG. 9b) ;
  • a paddle having a rotational angle of 270 degrees coincides exactly with a paddle having a rotational angle of 90 degrees (FIG. 9c)
  • a paddle having a rotational angle of 315 degrees coincides exactly with a paddle having a rotational angle of 135 degrees (FIG. 9d) .
  • each mixing paddle 85 will be in constant rotation during operation of the paddle mixer, due to the rotation of the shafts supporting the paddles (FIG. 13) .
  • the reference line should be deemed to rotate as the paddles rotate. For example, if the mixing paddles shown in FIGS. 9a-d are positioned sequentially on a single shaft, and if the shaft is rotated 90 degrees, then the chosen reference line, initially vertical, would rotate to a horizontal position. In other words, the relative rotational positions of the mixing paddles in FIGS. 9a-d, defined respectively as 1-2-3-4, will not change during operation of the paddle mixer.
  • each feed element 50 has a flat front surface 48, a flat back surface 49 parallel to the front surface, and a non-circular (preferably square) opening 46 perpendicular to and intersecting the front and back surfaces.
  • the feed elements do not have two concave surfaces intersecting at two lines. Instead, each feed element 50 includes portions of two alternating helical channels 47 and 59. The helical channels are more apparent in FIG. 13 wherein a plurality of feed elements 50 are combined in sequence on the rotating shafts 110 to form feed zones in the mixer.
  • the primary purpose of the feed elements 50 is to convey chewing gum base ingredients forward to the regions of the mixer where paddle mixing takes place.
  • a type of mixing paddle known as a forward helical paddle 95 can also be used with the method of the invention.
  • the forward helical paddle 95 imparts a slight forward conveying action while mixing the gum base ingredients.
  • each forward helical paddle 95 has two flat surfaces and two concave surfaces 88 and 89.
  • the flat surfaces are parallel to each other and intersect only the concave surfaces.
  • the concave surfaces oppose each other and intersect at two lines 90 and 92.
  • a non-circular (preferably square) opening 94 passes through the center of each mixing paddle 95 and intersects both flat surfaces.
  • the difference between the forward helical paddle 95 and the flat mixing paddle 85 is that, in the flat mixing paddle 85, the lines 90 and 92 (defining the intersections of concave surfaces 88 and 89) are parallel to each other as shown in FIG. 8.
  • the line 90 has been rotated counter-clockwise with respect to the line 92 so that the lines are no longer parallel, a ⁇ shown in FIG. lib.
  • the line 92 has been rotated clockwise with respect to the line 90. The effect of this rotation is to bend the concave surfaces 88 and 89 so that these surfaces have a mildly helical configuration.
  • a type of mixing paddle known as a reverse helical paddle 96 can also be used with the method of the invention.
  • the reverse helical paddle 96 imparts a slight resistance to forward conveying of the gum base ingredients while mixing the ingredients. This causes a locally higher degree of mixer fill and slight elevation in pressure, in the vicinity of the reverse helical paddle 96.
  • the reverse helical paddle 96 is configured in the same fashion as the forward helical pattern 95 discussed above, except that the lines 90 and 92 (defining the intersections of concave surfaces 88 and
  • FIGS, lie and 12c the helical paddles have been viewed from above and only the lines 90 and 92 of the paddles are shown, superimposed one on top of the other.
  • a reference line 91 is also shown, indicating the positions of lines 90 and 92 if there were no rotation, as in a flat paddle 85.
  • the angle "a" is the amount of counter-clockwise rotation of line 90 present in a forward helical paddle 95.
  • the angle “a” should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds.
  • the angle “b” is the amount of clockwise rotation of line 92 present in a forward helical paddle 95.
  • the angle “b” should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds.
  • the angle "a” is the amount of clockwise rotation of line 90 present in a reverse helical paddle 96.
  • the angle “a” should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds.
  • the angle “b” is the amount of counter-clockwise rotation of line 92 present in a reverse helical paddle 96.
  • the angle “b” should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds.
  • each of the shafts 110 has an active length of 36 inches and a square cross-sectional area of 1.375 inches x 1.375 inches (1.891 square inches) .
  • the parallel shafts 110 are spaced apart at a distance of 3.5 inches (center to center) .
  • the shafts 110 are adapted for co-rotation (rotation in the same direction) inside a mixing barrel.
  • Each of the shafts 110 supports an identical arrangement of mixing paddles and feed elements.
  • the mixing paddles and feed elements on the adjacent shafts may intermesh, as shown in FIG. 13, but do not touch each other, as the shafts rotate.
  • Each of the shafts 110 is long enough to accommodate thirty-six inches of elements, each having a length of 1 inch, a maximum diameter of 4.874 inches and a minimum diameter of 2 inches. Two or more 1-inch segments may be combined to make longer elements without affecting the operation. For instance, the feed elements 50 often have a length of 2 inches.
  • a large portion of each shaft should be covered with mixing paddles. Generally, at least about 40 percent of each shaft should be covered with mixing paddles. Preferably at least about 50 percent of each shaft is covered with mixing paddles, most preferably at least about 60 percent. Of the mixing paddles, a majority should be flat mixing paddles as opposed to forward helical or reverse helical paddles. In the embodiment shown in FIG. 13, 67 percent of the shaft length is covered with mixing paddles (24 one-inch elements) and 33 percent of the shaft length is covered with feed elements (6 two-inch elements) .
  • the mixer configuration 102 in FIG. 13 includes two feed zones 125 and 135, and two paddle mixing zones 130 and 150.
  • the specific mixer configuration is indicated in Table 1 below. In Table 1 and other tables, the following abbreviations are used:
  • FC - feed conveying element (each occupying two 1-inch positions)
  • FP - flat mixing paddle (each occupying one 1-inch position)
  • FH - forward helical mixing paddle (each occupying one 1-inch position)
  • RH - reverse helical mixing paddle (each occupying one 1-inch position)
  • Table 1 Mixer Confi ⁇ uration (Per Shaft I - FIG. 13
  • a high viscosity portion including elastomer, filler, and some resin or polyvinyl acetate can be continuously fed to the first feed zone 125 in FIG. 13. These ingredients can then be thoroughly mixed in the first paddle mixing zone 130 before being combined with additional ingredients.
  • a lower viscosity portion including waxes (when used) , fats, oils, colorants and additional resin or polyvinyl acetate can be continuously fed to the second feed zone 135. All gum base ingredients can then be thoroughly mixed in the second paddle mixing zone 150.
  • the mixer configuration 102 shown in FIG. 13 is, in practice, surrounded by one or more barrel seg ⁇ ments extending the length of the mixer configuration 102.
  • FIG. 14 illustrates, schematically, a typical barrel 105 surrounding the mixer configuration 102.
  • a motor 101 drives the shafts 110 which support the mixer elements.
  • the gum base ingredients are fed through feed ports 103 and 123 in the barrel 105.
  • the gum base remains in the mixer for a sufficient time to ensure homogeneity, ' for example, a time on the order of about 20-30 minutes, and exits through an exit nozzle 155.
  • the barrel 105 may be heated or cooled. Heating may be accomplished using hot water or a steam jacket surrounding the barrel (not shown) . Cooling may be accomplished by supplying cooling water to a jacket surrounding the barrel 105. Alternative methods of heating and cooling may also be employed. Generally, heating is applied at the start up, but cooling i ⁇ applied in the latter stages to prevent overheating and base degradation.
  • the heating and cooling of the barrel should be supplied, as necessary, to maintain the product exit temperatures at about 90°C-150°C, preferably at about 100-135°C, during mixing of the gum base ingredients.
  • FIG. 15 is a sectional view of the barrel 105 which indicates how the paddle mixer is able to operate with longer residence times, compared to a conventional twin screw extruder.
  • the barrel wall 116 has the shape of two intersecting cylinders, each cylinder having a diameter larger than the largest diameter of the mixing paddle 85 contained therein. This barrel configuration resembles that of a standard twin screw extruder. However, unlike the screws of a twin screw extruder, the paddles 85 do not mostly fill the space defined by the barrel wall 116.
  • the mixing paddles 85 have a typically close tolerance with the barrel wall 116, and with each other, in the vicinity of the lines 90 and 92 where the concave surfaces intersect.
  • the close ⁇ t tolerance between each paddle and the barrel wall 116 may be on the order of about 0.048 inch to about 0.078 inch, and the closest tolerance between the two paddles may be on the order of about 0.060 inch to about 0.090 inch.
  • the distance between each paddle 85 and the barrel wall 116 is much greater. Due to the unique design of the paddles 85, the percentage of barrel space occupied by the paddles 85 is much smaller than for a conventional twin screw extruder.
  • the pressure in the paddle mixer should remain below about 50 psig, preferably below about 20 psig, when there is a large percentage of paddles compared to other elements.
  • Each paddle 85 when viewed from the front a ⁇ in FIG. 15, has a smaller width than height.
  • the ratio of height to width of each mixing paddle is more than 1.5:1.
  • the ratio of height to width for each mixing paddle is more than 2:1.
  • the large amount of available barrel space also allows the method of the invention to be practiced at high residence times in paddle mixers.
  • the high proportion of mixing paddles, especially flat paddles, also contributes to the longer residence times and lower pressure.
  • the average residence time in the paddle mixer should be at least about 10 minutes, preferably more than 15 minutes, mo ⁇ t preferably more than 20 minute ⁇ .
  • the remaining operating parameters e.g., mixer rpm, feed rates, production rates, etc. vary depending on the size of the mixer and on the specific gum base composition.
  • a commercially available paddle mixer suitable for practicing the invention is a Teledyne Readco Continuous Processor, available from Teledyne Readco in York, Pennsylvania. These paddle mixers are available in a wide variety of sizes. Paddle diameters for the different size mixers range from 2 to 24 inches, and the ratios of mixer length to diameter (L/D) range from 4:1 to 14:1.
  • the maximum paddle diameter is preferably between 2 inche ⁇ and 5 inches, and the L/D is preferably about 7:1.
  • the paddle mixer configuration and process conditions should be selected so that a homogeneous gum base product is achieved.
  • two or more paddle mixers may be used in series, in the manner illustrated in FIG. 16.
  • the use of two mixers in series allows greater flexibility for feeding different gum base ingredients at different locations.
  • a combination of elastomer, filler and resin can be continuously fed via feed port 103 to the feed barrel 105 of the first mixer. These materials are mixed in the first mixer, after which additional resin can be added to the first mixer via feed port 123.
  • the combined ingredients are blended in the first mixer, and leave the first mixer at the exit 155, whereupon they are immediately fed into the barrel 205 of the second mixer 208 (powered by motor 201) via the feed port 203.
  • Polyvinyl acetate can also be continuously fed to the barrel 205 from hopper 207, via feed conveyor 209 and feed port 203.
  • ingredients such as waxes or oils
  • feed tanks 211 and 231, via pumps 213 and 233 can be injected into the second mixer from feed tanks 211 and 231, via pumps 213 and 233.
  • a portion of ingredients can be added into a downstream feed port 204.
  • the gum base leaves the second mixer via exit 255.
  • a wide variety of different feeding and mixing arrangement ⁇ can also be employed using two or more paddle mixers in series, in order to achieve good dispersion of ingredients and a wide variety of gum base products.
  • Paddles In addition to the paddles described above, a wide variety of mixing paddles, available from various extruder companies, can be used. Paddles, often called kneading elements, must have the effect of mixing in an extruder. Paddles can be two-sided, three-sided, or multiple sided.
  • the paddle mixer which may be referred to as a compounder, has different characteristics than a typical extruder even though the same equipment may be used. The difference between an extruder and a compounder is the ratio of paddles or kneading elements to the conveying elements. Conveying elements and compression elements cause an extruder to build up pressure.
  • Paddles or kneading elements do not build as much pressure in the extruder, thus there is more mixing with low pressure. If the extruder contains at least 40% kneading elements, then the pressure can be about one-fifth to one-tenth that of a typical extruder which uses more conveying and compression elements.
  • the residence time is much higher than in typical extruders. Many extruders provide a residence time of less than 2 minutes or even less than 1 minute. However, in the preferred paddle mixer described above, a residence time of at lea ⁇ t 10 minutes, and preferably at least 15-20 minutes, can be provided.
  • the method of the present invention may also be advantageously performed using a continuous mixer whose mixing screw is composed primarily of precisely arranged mixing elements with only a minor fraction of simple conveying elements.
  • a presently preferred mixer is a blade-and-pin mixer exemplified in Fig. 17. This mixer may be used to produce not only gum base, but an entire chewing gum composition.
  • a blade-and-pin mixer uses a combination of selectively configured rotating mixer blades and stationary barrel pins to provide efficient mixing over a relatively short distance.
  • a commercially available blade-and-pin mixer is the Buss kneader, manufactured by Buss AG in Switzerland, and available from Buss America, located in Bloomingdale, Illinois.
  • a presently preferred blade-and-pin mixer 100 includes a single mixing screw 120 turning inside a barrel 140 which, during use, is generally closed and completely ⁇ urrounds the mixing ⁇ crew 120.
  • the mixing screw 120 includes a generally cylindrical shaft 122 and three rows of mixing blades 124 arranged at evenly spaced locations around the screw shaft 122 (with only two of the rows being visible in FIG. 1) .
  • the mixing blades 124 protrude radially outward from the shaft 122, with each one resembling the blade of an axe.
  • the mixing barrel 140 includes an inner barrel housing 142 which is generally cylindrical when the barrel 140 i ⁇ clo ⁇ ed around the ⁇ crew 120 during operation of the mixer 100.
  • Three row ⁇ of ⁇ tationary pins 144 are arranged at evenly spaced locations around the ⁇ crew ⁇ haft 142, and protrude radially inward from the barrel housing 142.
  • the pins 144 are generally cylindrical in shape, and may have rounded or bevelled ends 146.
  • the mixing screw 120 with blades 124 rotates in ⁇ ide the barrel 140 and is driven by a variable speed motor (not ⁇ hown) .
  • the mixing ⁇ crew 120 also moves back and forth in an axial direction, creating a combination of rotational and axial mixing which is highly efficient.
  • the mixing blades 124 continually pass between the stationary pins 144, yet the blades and the pins never touch each other.
  • the radial edges- 126 of the blade ⁇ 124 never touch the barrel inner ⁇ urface 142, and the ends 146 of the pins 144 never touch the mixing screw shaft 122.
  • FIGS. 18-22 illustrate various screw elements which can be used to configure the mixing screw 120 for optimum use. Figs.
  • the on-screw elements 60 and 61 each include a cylindrical outer ⁇ urface 62, a plurality of blades 64 projecting outward from the surface 62, and an inner opening 66 with a keyway 68 for receiving and engaging a mixing screw shaft (not shown) .
  • the ⁇ econd on-screw element 61 is about twice as long as the first on-screw element 60.
  • FIG. 18c illustrates a restriction ring assembly 70 used to build back pre ⁇ sure at selected locations along the mixing screw 120.
  • the restriction ring assembly 70 includes two halves 77 and 79 mounted to the barrel housing 142, which halves engage during use to form a clo ⁇ ed ring.
  • the restriction ring assembly 70 includes a circular outer rim 72, an inner ring 74 angled as shown, and an opening 76 in the inner ring which receives, but does not touch, the on-screw elements 60 and 61 mounted to the screw shaft.
  • Mounting openings 75 in the surface 72 of both halve ⁇ of the restriction ring assembly 70 are used to mount the halves to the barrel housing 142.
  • FIG. 19 illustrates the relationship between the restriction ring as ⁇ embly 70 and the on-screw elements 60 and 61 during operation.
  • the clearances between the on- screw element ⁇ 60 and 61 and the inner ring 74 provide the primary means of passage of material from one side of the re ⁇ triction ring a ⁇ sembly 70 to the other.
  • the on- screw element 60 on the upstream side of the restriction ring assembly includes a modified blade 67 permitting clearance of the inner ring 74.
  • the other on-screw element 61 is placed generally downstream of the restriction ring assembly 70, and has an end blade (not visible) which move ⁇ close to and wipes the oppo ⁇ ite surface of the inner ring 74.
  • the clearances between outer ⁇ urfaces 62 of the on-screw elements 60 and 61 and the inner ring 74 of the restriction ring assembly 70 determine to a large extent how much pressure build-up will occur in the upstream region of the restriction ring as ⁇ embly 70 during operation of the mixer 100.
  • the up ⁇ tream on- ⁇ crew element 60 has an L/D of about 1/3
  • the downstream on-screw element 61 has an L/D of about 2/3, re ⁇ ulting in a total L/D of about 1.0 for the on-screw elements.
  • the restriction ring a ⁇ embly 70 has a smaller L/D of about 0.45 which coincide ⁇ with the L/D of the on-screw elements 60 and 61, which engage each other but do not touch the restriction ring as ⁇ embly.
  • Fig ⁇ . 20 and 21 illu ⁇ trate the mixing or "kneading" element ⁇ which perform mo ⁇ t of the mixing work.
  • the primary difference between the lower ⁇ hear mixing element 80 of FIG. 20 and the higher ⁇ hear mixing element 78 of FIG. 21 i ⁇ the ⁇ ize of the mixing blade ⁇ which project outward on the mixing elements.
  • the higher shear mixing blades 83 which project outward from the surface 81 are larger and thicker than the lower shear mixing blades 84 projecting outward from the surface 82 in FIG. 20.
  • the mixing blades are arranged in three circumferentially-spaced rows, as explained above with respect to FIG. 17.
  • FIG. 21 means that there is less axial distance between the blades and also less clearance between the blades 83 and the stationary pin ⁇ 144 a ⁇ the screw 120 rotates and reciprocates axially (FIG. 17) . This reduction in clearance causes inherently higher shear in the vicinity of the mixing element ⁇ 78.
  • FIG. 22 illu ⁇ trate ⁇ a ⁇ ingle stationary pin 144 detached from the barrel 140.
  • the pin 144 includes a threaded base 145 which permits attachment at selected locations along the inner barrel shaft 142. It is also possible to configure some of the pins 144 as liquid injection ports by providing them with hollow center openings.
  • FIG. 23 is a schematic view showing the pre ⁇ ently preferred barrel configuration, including the presently preferred arrangement of barrel pins 144.
  • FIG. 24 is a corresponding schematic view illustrating the presently preferred mixing screw configuration.
  • the mixer 200 whose preferred configuration is illu ⁇ trated in FIGS. 23 and 24 has an overall active mixing L/D of about 19.
  • the mixer 200 includes an initial feed zone 210 and five mixing zones 220, 230, 240, 250 and 260.
  • the zones 210, 230, 240, 250 and 260 include five possible large feed ports 212, 232, 242, 252 and 262, respectively, which can be used to add major (e.g. solid) ingredients to the mixer 200.
  • the zones 240 and 260 are also configured with five ⁇ maller liquid injection port ⁇ 241, 243, 261, 263 and 264 which are u ⁇ ed to add liquid ingredients.
  • the liquid injection ports 241, 243, 261, 263 and 264 include special barrel pins 144 formed with hollow centers, as explained above.
  • barrel pins 144 are preferably present in most or all of the available locations, in all three rows as shown.
  • Zone 210 which i ⁇ the initial feed zone, is configured with about 1-1/3 L/D of low shear elements, such as the element 40 shown in FIG. 4.
  • the L/D of the initial feed zone 210 is not counted as part of the overall active mixing L/D of 19, discussed above, because its purpose i ⁇ merely to convey ingredient ⁇ into the mixing zone ⁇ .
  • the first mixing zone 220 is configured, from left to right (FIG. 24) , with two low shear mixing elements 80 (FIG. 20) followed by two high shear element ⁇ 78 (FIG. 21) .
  • the two low ⁇ hear mixing element ⁇ contribute about 1-1/3 L/D of mixing
  • the two high ⁇ hear mixing element ⁇ contribute about 1-1/3 L/D of mixing.
  • Zone 220 ha ⁇ a total mixing L/D of about 3.0, including the end part covered by a 57mm re ⁇ triction ring as ⁇ embly 70 with cooperating on-screw elements 60 and 61 (not separately designated in FIG. 24) .
  • zone 230 is configured, from left to right, with three low shear mixing elements 80 and 1.5 high shear mixing elements 78.
  • the three low shear mixing elements contribute about 2.0 L/D of mixing, and the 1.5 high shear mixing elements contribute about 1.0 L/D of mixing.
  • Zone 230 has a total mixing L/D of about 4.0.
  • Straddling the end of the second mixing zone 230 and the start of the third mixing zone 240 is a 60mm restriction ring assembly 70 with cooperating on-screw elements 60 and 61 having an L/D of about l.o. Then, zone 240 i ⁇ configured, from left to right, with 4.5 high shear mixing elements 78 contributing a mixing L/D of about 3.0. Zone 240 also has a total mixing L/D of about 4.0. Straddling the end of the third mixing zone 240 and the start of the fourth mixing zone 250 is another 60mm re ⁇ triction ring a ⁇ embly 70 with cooperating on- ⁇ crew element ⁇ having an L/D of about 1.0.
  • Zone 250 has a total mixing L/D of about 4.0
  • zone 260 has a total mixing L/D of about 4.0.
  • Gum base was made on a continuous basis using a Leistritz model LSM 30.34 counter-rotational, intermeshing and tangential extruder in intermeshing mode with a barrel diameter of 30.3 mm set up with the following elements (given in order proceeding from first feed inlet to the output end of the extruder and using the Leistritz part designation for each element) : FF-1-30-120 (conveying element)
  • the die at the end of the extruder had a 1mm hole.
  • the extruder had two feeding zone ⁇ , each one adjacent the FF-1-30-120 conveying element ⁇ .
  • a powder blend of ground butyl rubber, calcium carbonate and terpene resin at a ratio of 6:23:17 was fed at a rate of 3 kg/hr in the first feed zone.
  • a powder blend of 5 part ⁇ glycerol monostearate, 8 parts hydrogenated cottonseed oil, 5 part ⁇ hydrogenated ⁇ oybean oil, 3 part ⁇ high molecular weight polyvinyl acetate and 21 part ⁇ low molecular weight polyvinyl acetate was fed into the second feeding zone at a rate of 2.74 kg/hr, along with a blend of 3 parts partially hydrogenated ⁇ oybean oil and 3 parts lecithin heated to 30°C and fed at a rate of 0.4 kg/hr.
  • the ratio of elastomers to fats and oils was 0.75:1.
  • the set temperature (except for the die, which did not have a temperature control) and actual temperature of the extruder housing during operation were as follow ⁇ :
  • the extruder was operated at a speed of 100 rpm and drew 9 amps.
  • a chewing gum base was produced which had no rubber particles or segregated oil.
  • some of the polyvinyl acetate was not fully incorporated. This would be incorporated as the base was used to make chewing gum, or if desired, could be eliminated by using a single screw extruder as a side feeder/pre-melter for the polyvinyl acetate.
  • Example 2 The same extruder set up and temperature ⁇ a ⁇ u ⁇ ed in Example 1 were u ⁇ ed to continuously make another chewing gum base.
  • a powder blend of 22 parts low molecular weight polyvinyl acetate, 13 parts hydrogenated cottonseed oil, 3 part ⁇ glycerol monostearate and 13 part ⁇ hydrogenated soybean oil was fed into the second feed inlet at a rate of 6.63 kg/hr, along with partially hydrogenated soybean oil heated to 30-60°C and fed at a rate of 1.3 kg/hr.
  • the ratio of elastomer to fats and oils was 0.65:1.
  • the extruder was operated at lOOrpm, and drew 7-8 amps.
  • a complete chewing gum base was prepared, although it was not as well mixed as the base of Example 1 and there were difficulties in material accumulating at the second feed zone.
  • the overall length of these elements is 1060 mm, giving a
  • gum base ingredients are added at the specified rates to the extruder 10 at the locations specified.
  • the rate ⁇ li ⁇ ted are for steady state operation.
  • the ratio of elastomer ⁇ to fat ⁇ and oils is 0.92:1.
  • Example 1 When conducting the experiment relating to Example l, the polyisobutylene was originally added at the second feed inlet. This was possible during startup, but when the blend of fats and polyvinyl acetate were also added, the fat ⁇ melted and lubricated the screws so that they no longer drew in the polyisobutylene. This i ⁇ why the polyisobutylene is introduced at the first feed zone in Example 1.
  • Example ⁇ l and 2 ⁇ ince the butyl rubber was ground before it was used, a portion of the filler and the ground butyl rubber were premixed (at a ratio of filler to butyl rubber of 1:3) to help keep the ground butyl rubber in a form that allowed it to be fed into the extruder as a powder blend.
  • This filler was included in the overall ratios cited in the examples.
  • chewing gum ba ⁇ e wa ⁇ made a ⁇ follow ⁇ .
  • the production rate for the gum base was 50 pounds per hour.
  • the gum base was manufactured using an extruder rpm of 400, initial barrel temperatures of 270-275°F, and a product exit temperature of about 128°C.
  • the average residence time in the paddle mixer wa ⁇ about 30-40 minute ⁇ .
  • This example was performed using a 2-inch paddle diameter Teledyne Readco Continuous Mixer and a 5-inch paddle diameter Teledyne Readco Continuous Mixer in series, similar to the arrangement shown in FIG. 16, with the 2-inch paddle diameter mixer being first.
  • the mixers were configured with the objective of accomplishing disper ⁇ ive mixing of rubber using the 2-inch compounder, and distributive mixing of oil using the 5-inch compounder.
  • the 2-inch and 5-inch compounders were configured as described in Tables 3 and 4.
  • the 2-inch compounder included 4 inches of conveying elements, and a balance of reverse helical and flat paddles, each 0.53 inch long. Overall, twenty-five reverse helical and flat paddle ⁇ (total) were used, for a total paddle length of 13.25 inches. The total active length of each of the shafts carrying the paddles was 17.25 inches.
  • the 5-inch compounder used paddles and conveying element ⁇ with the dimensions described above.
  • the feed ports were arranged as follows Feed Port No. 1 - above longitudinal posi ⁇ tions 1 - 4 on 2-inch mixer
  • chewing gum ba ⁇ e was made as follows.
  • a mixture of ground i ⁇ obutylene-isoprene copolymer (2-7 mm particle size) and calcium carbonate at a ratio of 10:13 was fed at a rate of 0.192 lb/min. to feed port No. 1. Also added at feed port No. 1 was 16 parts polyisobutylene at 130°C at a rate of 0.133 lb/min. At feed port No. 2, 22 parts polyvinyl acetate and 29 parts of a powder blend of hydrogenated vegetable oil, glyorol monostearate, and hydrogenated soybean oil at a ratio of 13:3:13 were added at a rate of 0.425 lb/min. Also added at feed port No. 2 wa ⁇ a liquid blend at 70°C of 5 part ⁇ hydrogenated cotton ⁇ eed oil and 5 part ⁇ lecithin at a rate of 0.083 lb/min. Feed port No. 3 wa ⁇ not used.
  • the gum base had normal color, a smooth texture, and a homogeneous con ⁇ istency, except for an occasional wood sliver resulting from a previous use of the equipment.
  • Example 6 This example was performed using the same two- mixer arrangement described in Example 5.
  • the 2-inch and 5-inch Teledyne Readco Continuous Mixers were configured as described in Tables 3 and 4, above.
  • the feed ports were arranged as described in Example 5.
  • U ⁇ ing the above mixer arrangement, bubble gum base was made as follows.
  • a mixture of styrene-butadiene rubber, calcium carbonate ( ⁇ 12 micron particle size) , and glycerol ester of wood rosin at a ratio of 9:46:18 was added at feed port No. l at a rate of 0.608 lb/min.
  • the production rate for the bubble gum base was 47 pounds per hour.
  • the gum base was manufactured using the following process conditions:
  • the gum ba ⁇ e had normal color, a ⁇ mooth texture, and a homogeneous consi ⁇ tency.
  • Continuous Mixer was configured as described in Table 1 (Example 4) except that a reverse helical paddle was placed in position 19.
  • the feed ports were arranged a ⁇ follow ⁇ :
  • chewing gum base wa ⁇ made as follows. A mixture of ground isobutylene-isoprene copolymer (2-7 mm particle size) , calcium carbonate ( ⁇ 12 micron particle size) , and terpene resin at a ratio of 8:21:17 was fed at a rate of 0.383 lb/min. at the first feed inlet. In the second feed inlet, a powder blend of polyvinyl acetate, glycerol monostearate, and hydrogenated ⁇ oybean and vegetable oil at a ratio of 24:5:13 were fed at a rate of 0.35 lb/min.
  • the gum base was manufactured using the following proce ⁇ condition ⁇ :
  • the gum base had normal color, a smooth texture, and a homogeneous con ⁇ istency, except for an occasional isolated undispersed particle.
  • paddle mixing is an effective technique for manufacturing gum base on a continuous basis.
  • the optimum process conditions, and the use of one or two mixers, vary depending on the specific gum base composition and the desired output rate.
  • Example 8 Gum base wa ⁇ made on a continuou ⁇ basis using a
  • Japan Steel Works Incorporated model TEX30HSS32.5PW-2V twin screw extruder set up in a co-rotating mode with extremely aggressive kneading elements and two feed inlets.
  • Extremely aggressive kneading elements means that most of the extruder shaft ⁇ were covered with kneading element ⁇ as paddle ⁇ .
  • the arrangement was: 1/6 conveying elements at the first feed inlet, 1/3 kneading elements, then 1/6 conveying elements at the second feed inlet and 1/3 kneading elements. This results in paddles covering 67% of the shafts.
  • a mixture of ground styrene - butadiene rubber (2-7 mm particle size) , calcium carbonate ( ⁇ 12 micron particle size) and resin ester of glycerol abietate at a ratio of 9:46:18 was fed at a rate of 5.4 kg/hr at the first feed inlet.
  • a mixture of resin ester of glycerol abietate, glycerol mono ⁇ tearate and microcry ⁇ talline wax at a ratio of 20:1:6 was fed at a rate of 2 kg/hr at the second feed inlet.
  • the extruder wa ⁇ operated with temperature controls for seven heating zones and the die. The set point and actual temperatures were as follows:
  • the machine was run at 200 rpm, drawing 21 amp ⁇ .
  • the extrudate was a finished gum base that had no lumps.
  • Thi ⁇ example wa ⁇ performed u ⁇ ing a two-mixer arrangement with two 5-inch Teledyne Readco Continuous Mixer Compounders.
  • the first compounder was configured the same as in Table 4 of Example 5.
  • the second compounder was configured based on Table 1, shown previously. This configuration is also shown in Figure
  • the feed port ⁇ were arranged as follows:
  • chewing gum base was made as follows:
  • a mixture of ground isobutylene-i ⁇ oprene copolymer (2-7 mm particle size) , calcium carbonate ( ⁇ 12 micron particle size) , terpene resin, and powder color at a ratio of 11:18:17:1 was fed at a rate of 1.435 lb/min. in the first feed inlet.
  • a powder blend of polyvinyl acetate, glycerol mono ⁇ tearate, and hydrogenated ⁇ oybean and vegetable oil at a ratio of 24:5:12 was fed at a rate of 1.264 lb/min.
  • 6 parts of polyisobutylene at 95°C at a feed rate of 0.181 lb/min. and 6 parts of a 50/50 mixture of hydrogenated cottonseed oil/lecithin at 80°C at a feed rate of 0.203 lb/min. were added.
  • the gum base had normal color, no lumps, no unincorporate oil, but had a burnt off taste and odor.
  • Thi ⁇ example wa ⁇ performed u ⁇ ing a two-mixer arrangement with two 5-inch Teledyne Readco Continuous Mixer Compounder ⁇ . Both compounders were configured with the same paddle configuration that wa ⁇ shown in Table 1.
  • Four feed ports were arranged as follows:
  • chewing gum ba ⁇ e wa ⁇ made as follows:
  • a mixture of ground isobutylene-i ⁇ oprene copolymer (2-7 mm particle ⁇ ize) , calcium carbonate ( ⁇ 12 micron particle size) , and polyvinyl acetate at a ratio of 13:10:7 was fed at a rate of 0.75 lb/min. in the first feed inlet.
  • 15 parts of polyvinyl acetate was added at 0.375 lb/min.
  • hydrogenated vegetable oil, hydrogenated soybean oil, and glycerol monostearate at a ratio of 13:13:3 were added at a rate of 0.725 lb/min.
  • 10 parts of partially hydrogenated vegetable oil at 0.25 lb/min., and 16 parts of polyisobutylene at 130°C at a rate of 0.40 lb/min. were added.
  • the production rate for the gum base was 150 pounds per hour.
  • the gum base was manufactured using the following proces ⁇ conditions: Fir ⁇ t 5-Inch Second 5-Inch
  • the gum base had normal color, no lump ⁇ , no unincorporated oil, and clean ta ⁇ te and odor.
  • a mixture of ground isobutylene-i ⁇ oprene copolymer (2-7 mm particle ⁇ ize) , calcium carbonate ( ⁇ 12 micron particle ⁇ ize) , terpene resin, and polyvinyl acetate at a ratio of 11:18:17:6 was fed at a rate of 1.30 lb/min. in the first feed inlet.
  • a powder blend of polyvinyl acetate, glycerol monostearate, hydrogenated soybean oil and vegetable oil, and powdered color at a ratio of 18:5:12:1 was fed at a rate of 0.90 lb/min.
  • the gum base had normal color, no lumps, no unincorporated oil, and clean ta ⁇ te and odor.
  • Gum ba ⁇ es of Examples 10 and 11 were analyzed by Gel Permeation chromatography (GPC) and compared to the same formulation of base made by conventional batch processe ⁇ . Analy ⁇ e ⁇ ⁇ howed that the i ⁇ obutylene-isoprene copolymer of Examples 10 and 11 was over-sheared and degraded. Sugar gum formulations were made to compare sensory attribute ⁇ of ba ⁇ es from Examples 10 and 11 to base made by the conventional batch proces ⁇ . Tests showed that bases of Examples 10 and 11 gave a much softer texture than the base ⁇ from conventional batch proce ⁇ s.
  • chewing gum base was made as follows.
  • a mixture of ground isobutylene-isoprene copolymer (2-7 mm particle size) , and calcium carbonate, terpene resins, and polyvinyl acetate at a ratio of 11:18:17:1 was added at a rate of 1.175 lb/min. to feed inlet No. 1.
  • a powder blend of polyvinyl acetate, glycerol monostearate, hydrogenated soybean and vegetable oils, and powdered color at a ratio of 23:5:12:1 was fed at a rate of 1.025 lb/min.
  • gum base had normal color, no lump ⁇ , no unincorporated oil, and clean taste and odor.
  • Analysi ⁇ of the gum ba ⁇ e by GPC indicated it is very similar to the same base formula made by a conventional batch proces ⁇ . Also, gum made from base of this example had sensory properties virtually the same as gum made with base made by conventional batch proces ⁇ .
  • the chewing gum base is made in a blade-and-pin mixer, which is then also u ⁇ ed to complete the making of the chewing gum composition.
  • a blade-and-pin mixer In order to accomplish the total chewing gum manufacture using the preferred blade-and-pin mixer 200 (Fig. 17) , it is advantageous to maintain the rpm of the mixing screw 120 at less than about 150, preferably less than about 100.
  • the mixer temperature i ⁇ preferably optimized so that the gum base is at about 130°F or lower when it initially meets the other chewing gum ingredient ⁇ , and the chewing gum product i ⁇ at about 130°F or lower (preferably 125°F or lower) when it exits the mixer.
  • This temperature optimization can be accomplished, in part, by selectively heating and/or water cooling the barrel sections surrounding the mixing zones 220, 230, 240, 250 and 260 (Fig. 23).
  • the elastomer, filler, and at least some of the elastomer solvent are added to the fir ⁇ t large feed port 212 in the feed zone 210 of the mixer 200, and are ⁇ ubjected to highly di ⁇ per ⁇ ive mixing in the fir ⁇ t mixing zone 220 while being conveyed in the direction of the arrow 122.
  • the remaining elastomer solvent (if any) and polyvinyl acetate are added to the second large feed port 232 in the second mixing zone 230, and the ingredients are subjected to a more distributive mixing in the remainder of the mixing zone 230.
  • Fats, oils, waxes (if used) , emulsifiers and, optionally, colors and antioxidants, are added to the liquid injection ports 241 and 243 in the third mixing zone 240, and the ingredient ⁇ are ⁇ ubjected to distributive mixing in the mixing zone 240 while being conveyed in the direction of the arrow 122.
  • the gum base manufacture ⁇ hould be complete, and the gum ba ⁇ e ⁇ hould leave the third mixing zone 240 as a substantially homogeneous, lump-free compound with a uniform color.
  • the fourth mixing zone 250 is used primarily to cool the gum base, although minor ingredient addition may be accomplished. Then, to manufacture the final chewing gum product, glycerin, corn syrup, other bulk sugar sweeteners, high intensity sweetener ⁇ , and flavors can be added to the fifth mixing zone 260, and the ingredients are subjected to di ⁇ tributive mixing. If the gum product is to be sugarless, hydrogenated starch hydrolyzate or sorbitol solution can be substituted for the corn syrup and powdered alditol ⁇ can be ⁇ ub ⁇ tituted for the ⁇ ugar ⁇ .
  • glycerin i ⁇ added to the fir ⁇ t liquid injection port 261 in the fifth mixing zone 260.
  • Solid ingredients (bulk sweetener ⁇ , encap ⁇ ulated high intensity sweeteners, etc.) are added to the large feed port 262.
  • Syrups corn syrup, hydrogenated starch hydrolyzate, sorbitol solution, etc.) are added to the next liquid injection port 263, and flavors are added to the final liquid injection port 264.
  • Flavors can alternatively be added at ports 261 and 263 in order to help plasticize the gum base, thereby reducing the temperature and torque on the screw. This may permit running of the mixer at higher rpm and throughput.
  • the gum ingredients are compounded to a homogeneous mass which is discharged from the mixer as a continuou ⁇ stream or "rope".
  • the continuous stream or rope can be deposited onto a moving conveyor and carried to a forming station, where the gum i ⁇ ⁇ haped into the desired form such as by pre ⁇ ing it into ⁇ heet ⁇ , ⁇ coring, and cutting into ⁇ tick ⁇ . Because the entire gum manufacturing proce ⁇ s is integrated into a single continuous mixer, there is less variation in the product, and the product is cleaner and more stable due to its ⁇ implified mechanical and thermal hi ⁇ torie ⁇ .
  • Examples 13-22 were run u ⁇ ing a Buss kneader with a 100mm mixer screw diameter, configured in the preferred manner described above (unless indicated otherwise) , with five mixing zones, a total mixing L/D of 19, and an initial conveying L/D of 1-1/3. No die was used at the end of the mixer, unless indicated otherwise, and the product mixture exited as a continuou ⁇ rope.
  • Each example wa ⁇ de ⁇ igned with feed rate ⁇ to yield chewing gum product at the rate of 300 pound ⁇ per hour.
  • Liquid ingredients were fed using volumetric pumps into the large feed ports and/or smaller liquid injection ports generally positioned as described above, unles ⁇ otherwi ⁇ e indicated.
  • the pump ⁇ were appropriately ⁇ ized and adju ⁇ ted to achieve the de ⁇ ired feed rate ⁇ .
  • Dry ingredient ⁇ were added u ⁇ ing gravimetric ⁇ crew feeders into the large addition ports positioned a ⁇ de ⁇ cribed above. Again, the feeders were appropriately sized and adju ⁇ ted to achieve the de ⁇ ired feed rate ⁇ .
  • Temperature control wa ⁇ accomplished by circulating fluids through jackets surrounding each mixing barrel zone and inside the mixing screw. Water cooling was used where temperatures did not exceed 200°F, and oil cooling wa ⁇ used at higher temperatures. Where water cooling wa ⁇ desired, tap water (typically at about 57°F) was used without additional chilling.
  • Fluid temperatures were set for each barrel mixing zone (corresponding to zones 220, 230, 240, 250 and 260 in Figs. 23 and 24) , and are reported below as Zl, Z2, Z3, Z4 and Z5, respectively. Fluid temperatures were al ⁇ o ⁇ et for the mixing ⁇ crew 120, and are reported below a ⁇ SI. Actual mixture temperature ⁇ were recorded near the downstream end of mixing zones 220, 230, 240 and 250; near the middle of mixing zone 260; and near the end of mixing zone 260. The ⁇ e mixture temperature ⁇ are reported below a ⁇ TI, T2, T3, T4, T5 and T6, re ⁇ pectively.
  • Actual mixture temperatures are influenced by the temperatures of the circulating fluid, the heat exchange properties of the mixture and ⁇ urrounding barrel, and the mechanical heating from the mixing proce ⁇ , and often differ from the set temperatures due to the additional factors. All ingredients were added to the continuous mixer at ambient temperature (about 77°F) unle ⁇ otherwise noted.
  • Example 13 This example illustrates the preparation of a spearmint flavored non-tack ⁇ ugar chewing gum.
  • a mixture of 24.2% terpene re ⁇ in, 29.7% dusted ground butyl rubber (75% rubber with 25% fine ground calcium carbonate as an anti-blocking aid) and 46.1% fine ground calcium carbonate was fed at 25 lb/hr into the first large feed port (port 212 in Figs. 23 and 24) .
  • Low molecular weight polyisobutylene (mol. wt. 12,000) , preheated to 100°C, was al ⁇ o added at 6.3 lb/hr into thi ⁇ port.
  • Ground low molecular weight polyvinyl acetate was added at 13.3 lb/hr into the second large feed port (por 232 in Figs. 23 and 24) .
  • a fat mixture preheated to 83°C, was injected into the liquid injection port ⁇ in the third mixing zone (port ⁇ 241 and 243 in Fig. 23) , at a total rate of 18.4 lb/hr, with 50% of the mixture being fed through each port.
  • the fat mixture included 30.4% hydrogenated ⁇ oybean oil, 35.4% hydrogenated cotton ⁇ eed oil, 13.6% partially hydrogenated ⁇ oybean oil, 18.6% glycerol mono ⁇ tearate, 1.7% cocoa powder, and 0.2% BHT.
  • Glycerin was injected into the first liquid injection port in the fifth mixing zone (port 261 in Fig. 23) at 3.9 lb/hr.
  • a mixture of 1.1% sorbitol and 98.9% sugar was added into the large feed port in the fifth mixing zone (port 262 in Fig. 23) at 185.7 lb/hr.
  • Corn syrup, preheated to 44°C, was added into the second liquid injection port in the fifth mixing zone (port 263 in Fig. 23) at 44.4 lb/hr.
  • Spearmint flavor was added into the third liquid injection port in the fifth mixing zone (port 264 in Fig. 23) at 3.0 lb/hr.
  • the zone temperatures Z1-Z5 were set (in °F) at 350, 350, 150, 57 and 57, re ⁇ pectively.
  • the mixing ⁇ crew temperature SI was set at 120°F.
  • the mixture temperatures T1-T6 were mea ⁇ ured at ⁇ teady ⁇ tate (in °F) a ⁇ 235, 209, 177, 101 and 100, and fluctuated ⁇ lightly during the trial.
  • the screw rotation was 80 rpm.
  • the product was comparable to that produced by conventional pilot scale batch proces ⁇ ing.
  • the chew wa ⁇ ⁇ lightly rubbery but no ba ⁇ e lumps were visible.
  • This example illustrate ⁇ the preparation of a peppermint flavored non-tack sugar chewing gum.
  • Molten polyi ⁇ obutylene (preheated to 100°C) wa ⁇ also added to port 212 at 9.5 lb/hr.
  • a fat mixture (preheated to 82°C) was pumped 50/50 into port ⁇ 241 and 243 at a total rate of 23.6 lb/hr.
  • the fat mixture included 33.6% hydrogenated cottonseed oil, 33.6% hydrogenated soybean oil, 24.9% partially hydrogenated ⁇ oybean oil, 6.6% glycerol monostearate, 1.3% cocoa powder and 0.1% BHT.
  • Glycerin was added to port 261 at 2.1 lb/hr.
  • a mixture of 98.6% sugar and 1.4% sorbitol was added to port 262 at 196 lb/hr.
  • Corn syrup (preheated to 40°C) was added to port 263 at 39.9 lb/hr.
  • Peppermint flavor wa ⁇ added to port 264 at 2.1 lb/hr.
  • the zone temperatures (Z1-Z5, °F) were set at
  • the ⁇ crew temperature (SI) was set at 200°F.
  • the mixture temperatures (T1-T6, °F) were measured as 297, 228, 258, 122, 98 and 106, respectively.
  • the screw rotation was 85 rpm.
  • the finished product was free of lumps but was dry and lacked tensile strength. These defects were attributed to the formula rather than the proce ⁇ ing.
  • Thi ⁇ example illu ⁇ trates the preparation of a ⁇ pearmint flavored gum for pellet coating.
  • a blend of 27.4% high molecular weight terpene resin, 26.9% low molecular weight terpene resin, 28.6% dusted ground butyl rubber (75% rubber, 25% calcium carbonate) and 17.1% fine ground calcium carbonate was fed into the first large port 212 (Fig. 23), at 33.5 lb/hr. Molten polyisobutylene (100°C) was pumped into the same port at 1.3 lb/hr.
  • a fat mixture (82°C) was added 50/50 into ports 241 and 243, at a total rate of 17.4 lb/hr.
  • the fat mixture included 22.6% hydrogenated cottonseed oil, 21.0% partially hydrogenated soybean oil, 21.0% hydrogenated soybean oil, 19.9% glycerol mono ⁇ tearate, 15.4% lecithin and 0.2% BHT.
  • the screw temperature (SI) was set at 68°F.
  • the mixture temperature ⁇ (T1-T6, °F) were mea ⁇ ured a ⁇ 230, 215, 166, 105, 109 and 111, respectively.
  • the screw rotation was 80 rpm.
  • the product was firm and cohesive when chewed (normal for a pellet center) . No base lumps were visible.
  • This example illu ⁇ trate ⁇ the preparation of a peppermint flavored sugar chewing gum.
  • a blend of 11.1% high molecular weight polyvinyl acetate and 88.9% low molecular weight polyvinyl acetate was added into the second large feed port 232 at 14.4 lb/hr.
  • This fat mixture included 31.9% hydrogenated cottonseed oil, 18.7% hydrogenated soybean oil, 13.2% partially hydrogenated cottonseed oil, 19.8% glycerol monostearate, 13.7% soy lecithin, 2.5% cocoa powder and 0.2% BHT.
  • Glycerin wa ⁇ injected into port 261 at 3.9 lb/hr.
  • a mixture of 84.6% sucrose and 15.4% dextrose monohydrate was added to port 262 at 203.1 lb/hr.
  • Corn syrup (40°C) was injected into port 263 at 30.0 lb/hr.
  • a mixture of 90% peppermint flavor and 10% soy lecithin was injected into port 264 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F) were set at
  • the screw rotation was set at 55 rpm.
  • the finished product had good chew characteri ⁇ tic ⁇ and there wa ⁇ no evidence of rubber lump ⁇ .
  • This example illustrate ⁇ the preparation of a fruit-flavored sugar gum.
  • a mixture of 39.3% du ⁇ ted ground butyl rubber (75% rubber, 25% calcium carbonate) , 39.1% low molecular weight terpene re ⁇ in and 21.6% fine ground calcium carbonate was added to the first large feed port 212 (Fig. 23) at 20.6 lb/hr.
  • Polyisobutylene preheated to 100°C was also added at 1.0 lb/hr into the port 232.
  • a fat/wax composition (82°C) was injected 50/50 into the liquid injection ports 241 and 243, at a total rate of 14.0 lb/hr.
  • Glycerin was injected into the liquid injection port 261 at 3.3 lb/hr.
  • a mixture of 88.5% sucrose and 11.5% dextrose monohydrate was added at 201.0 lb/hr into the large port 262.
  • Corn syrup (40°C) wa ⁇ injected at 3.0 lb/hr into the liquid injection port 263, and a mixture of 88.9% fruit flavor and 11.1% soy lecithin was injected at 2.7 lb/hr into the liquid injection port 264.
  • the zone temperature ⁇ (Z1-Z5, °F) were set at
  • the screw temperature (SI) was set at 66°F.
  • the mixture temperature ⁇ (T1-T6, °F) were mea ⁇ ured as 359, 278, 185, 105, 100 and 109, respectively.
  • the screw rotation was ⁇ et at 70 rpm.
  • the product wa ⁇ very ⁇ oft while warm and fell apart during chewing. However, this was not atypical for this product. After aging for two months, the product was again chewed and found to have excellent texture and flavor. No rubber lumps were vi ⁇ ible.
  • Thi ⁇ example illustrates the preparation of a spearmint flavored sugarless gum.
  • a mixture of 42.1% fine ground calcium carbonate, 18.9% glycerol ester of wood rosin, 16.7% glycerol ester of partially hydrogenated wood rosin, 17.0% ground butyl rubber, and 5.3% dusted ground (25:75) styrene butadiene rubber (75% rubber, 25% calcium carbonate) was added into port 212 (Fig. 23) at 38.4 lb/hr.
  • the fat mixture included 35.7% hydrogenated cottonseed oil, 30.7% hydrogenated soybean oil, 20.6% partially hydrogenated soybean oil, 12.8% glycerol monostearate and 0.2% BHT.
  • glycerin was injected at 25.5 lb/hr into the fourth mixing zone 250 (Fig. 23) through a liquid injection port (not shown) .
  • a coevaporated blend of hydrogenated starch hydrolysate and glycerin (at 40°C) was injected further downstream in the fourth mixing zone 250 through another liquid injection port (not shown).
  • the coevaporated blend included 67.5% hydrogenated starch hydrolysate ⁇ olid ⁇ , 25% glycerin and 7.5% water.
  • the zone temperatures (Z1-Z5, °F) were set at 400, 400, 150, 62 and 62, respectively.
  • the screw temperature (SI) was set at 66°F.
  • the mixture temperatures (T1-T6, °F) were measured a ⁇ 307, 271, 202, 118, 103 and 116.
  • the gum had good appearance with no sorbitol spot ⁇ or rubber lump ⁇ .
  • the gum was slightly wet to the touch, sticky and fluffy (low den ⁇ ity) , but was acceptable.
  • the gum was con ⁇ idered soft initially but firmed up with continued chewing.
  • This example illustrates the preparation of a sugarles ⁇ spearmint gum for use in coated pellets.
  • a mixture of 28.6% dusted ground butyl rubber (75% rubber, 25% calcium carbonate), 27.4% high molecular weight terpene re ⁇ in, 26.9% low molecular weight terpene resin and 17.1% calcium carbonate was added into port 212 (Fig. 23) at 41.9 lb/hr.
  • a fat composition (82°C ) was injected 50/50 into ports 241 and 243 at a total rate of 21.7 lb/hr.
  • the fat composition included 22.6% hydrogenated cotton ⁇ eed oil, 21.0% hydrogenated ⁇ oybean oil, 21.0% partially hydrogenated soybean oil, 19.9% glycerol monostearate, 15.4% glycerin and 0.2% BHT.
  • a 70% sorbitol ⁇ olution wa ⁇ injected into the fourth mixing zone 250 (Fig. 23) at 17.4 lb/hr, using a hollow barrel pin liquid injection port (not shown) .
  • the zone temperature ⁇ (Z1-Z5, °F) were set at 400, 400, 150, 61 and 61, respectively.
  • the screw temperature (SI) was ⁇ et at 65°F.
  • the mixture temperature ⁇ (T1-T6, °F) were mea ⁇ ured as 315, 280, 183, 104, 109 and 116, respectively.
  • the screw rotation was set at 61 rpm.
  • Thi ⁇ example illustrates the preparation of a peppermint flavored sugar chewing gum.
  • a fat mixture preheated to 83°C, was injected into the liquid injection ports in the third mixing zone (ports 241 and 243 in Fig. 23), at a total rate of 14.5 lb/hr, with 50% of the mixture being fed through each port.
  • the fat mixture included 0.2% BHT, 2.5% cocoa powder, 31.9% hydrogenated cotton ⁇ eed oil, 19.8% glycerol mono ⁇ tearate, 18.7% hydrogenated soybean oil, 13.7% lecithin, and 13.2% partially hydrogenated cottonseed oil.
  • a mixture of 84.6% sugar and 15.4% dextrose monohydrate was injected at 203.1 lb/hr into the large feed port 262 in the fifth mixing zone.
  • the mixing screw temperature SI was set at 101°F.
  • the mixer temperatures T1-T6 were measured at steady state (in °F) a ⁇ 320, 280,
  • the peppermint sugar gum product wa ⁇ de ⁇ irably soft, and acceptable in quality.
  • This example illu ⁇ trate ⁇ the preparation of a sugarless stick bubble gum.
  • the ⁇ crew configuration shown in Fig. 24, and u ⁇ ed for the previous examples was varied as follows.
  • the conveying section 210 and mixing sections 220, 250 and 260 were configured substantially as before.
  • the three low shear elements 80 (Fig. 20) were also not changed.
  • a fat/wax mixture (at 82°C) was fed 50/50 into the liquid injection ports 241 and 243 in the third mixing zone 240, at a total rate of 13.9 lb/hr.
  • Diluted glycerin was injected into the fourth mixing zone 250 at 28.2 lb/hr using a liquid injection port (not shown) .
  • the dilution was 87% glycerin and 13% water.
  • the zone temperatures (Z1-Z5, °F) were set at 350, 350, 100, 64 and 64, re ⁇ pectively.
  • the screw temperature (SI) was set at 100°F.
  • the mixture temperatures (T1-T6, °F) were recorded as 286, 260, 163, 107, 104 and 112, respectively.
  • the screw rotation was 75 rpm.
  • the finished product looked good and contained no base lumps.
  • the flavor and texture were very good during chewing, as were the bubble blowing characteri ⁇ tics.
  • Examples 22-36 also disclose the use of a blade-and-pin mixer to make a complete chewing gum.
  • Example 22 70/30% Split of Terpene Resin and 12/88% Split of PVAC. This example illustrates the preparation of a gum base to be used for a peppermint flavored sugar gum.
  • a blend of 25.545% ground isobutylene-isoprene copolymer, 13.183% low molecular weight terpene resin, 13.343% high molecular weight terpene resin, 0.731% high molecular weight polyvinyl acetate, 5.844% low molecular weight polyvinyl acetate, and 41.354% fine ground calcium carbonate was added to the fir ⁇ t large feed port 212 at 26.88 lb/hr.
  • a blend of 70.270% low molecular weight polyvinyl acetate, 8.786% high molecular weight polyvinyl acetate, 9.273% low molecular weight terpene re ⁇ in, 9.423% low molecular weight terpene re ⁇ in, 9.423% high molecular weight terpene resin, and 2.24 color was added into the ⁇ econd large feed port 232 at 16.01 lb/hr. Polyi ⁇ obutylene was also added into the second large feed port at 3.51 lb/hr. A fat mixture (225°F.) was injected into zone
  • This fat mixture included 37% hydrogenated cotton ⁇ eed oil, 22% hydrogenated ⁇ oybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
  • Glycerin was injected into zone 260 at 3.5 lb/hr. A mixture of 85% sucrose and 15% dextrose monohydrate was added to the large feed port 262 at 103.1 lb/hr. Corn syrup (100°F.) was injected into zone 260 at 30.0 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55, and 55 respectively, and the screw temperature (SI) was set at 100°F.
  • the mixture temperature ⁇ (T1-T6, °F.) were measured as 319, 291, 170, 118, 112 and 89, re ⁇ pectively.
  • the ⁇ crew rotation wa ⁇ set at 60 rpm.
  • the finished product had good chew characteristic and there wa ⁇ no evidence of rubber lump ⁇ .
  • This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated ⁇ oybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
  • Glycerin was injected into zone 260 at 3.5 lb/hr.
  • Corn syrup (100°F.) was injected into zone 260 at 30.50 lb/hr.
  • Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F.) were ⁇ et at
  • the screw temperature (SI) was set at 100°F.
  • the mixture temperature ⁇ (T1-T6, °F.) were measured as 316, 289, 154, 116, 110 and 90, re ⁇ pectively.
  • the ⁇ crew rotation wa ⁇ set at 60 rpm.
  • the finished product had good chew characteri ⁇ tic and there was no evidence of rubber lump ⁇ .
  • the example illustrates the preparation of a gum base to be used for a peppermint flavored sugar gum.
  • a blend of 71.664% low molecular weight polyvinyl acetate, 8.960% high molecular weight polyvinyl acetate, 8.579% low molecular weight terpene resin, 8.718% high molecular weight terpene re ⁇ in, and 2.08% color was added into the second large feed port 232 at 17.31 lb/hr.
  • Polyisobutylene was also added into the second large feed port at 3.51 lb/hr.
  • a fat mixture (225°F.) was injected into zone 240 at a total rate of 14.16 lb/hr.
  • This fat mixture included 37% hydrogenated cotton ⁇ eed oil, 22% hydrogenated soybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
  • Glycerin was injected into zone 260 at 3.5 lb/hr.
  • a mixture of 85% sucrose and 15% dextrose monohydrate was added to the large feed port 262 at 203.1 lb/hr.
  • Corn syrup (100°F.) was injected into zone 260 at 30.0 lb/hr.
  • Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F.
  • the mixture temperatures (T1-T6, °F.) were measured as 322, 291, 155, 116, 109 and 89, respectively.
  • the screw rotation was set at 60 rpm.
  • the finished product had good chew characteristic ⁇ and there was no evidence of rubber lumps.
  • a blend of 67.688% low molecular weight polyvinyl acetate, 8.514% high molecular weight polyvinyl acetate, 10.536% low molecular weight terpene re ⁇ in, 10.707% high molecular weight terpene resin, and 2.559% color was added into the second large feed port 232 at 14.13 lb/hr.
  • Polyisobutylene was also added into the second large feed port 232 at 3.51 lb/hr.
  • a fat mixture (225°F.) was injected in to zone 240, at a total rate of 14.16 lb/hr.
  • This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated soybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
  • Glycerin was injected into zone 260 at 3.9 lb/hr.
  • a mixture of 85% sucrose and 15% dextrose monohydrate was added to the large feed port 262 at 203.1 lb/hr.
  • Corn syrup (100°F.) was injected into zone 260 at 30.0 lb/hr.
  • Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F.
  • the mixture temperatures (T1-T6, °F.) were measured as 311, 289, 158, 114, 109, and 89 respectively.
  • the fini ⁇ hed product had good chew characteristic and there was no evidence of rubber lumps.
  • This example illustrates the preparation of a gum base to be used for a non-tack peppermint flavored ⁇ ugar gum.
  • a blend of 46.302% ground i ⁇ obutylene- i ⁇ oprene copolymer, 18.980% low molecular weight polyvinyl acetate and 34.718% fine ground calcium carbonate was added to the first large feed port 212 at
  • Polyisobutylene was also added into the second large feed port at 3.5 lb/hr.
  • a fat mixture (225°F.) was injected into zone
  • This fat mixture included 34% hydrogenated cotton ⁇ eed oil, 34% hydrogenated ⁇ oybean oil, 25% partially hydrogenated ⁇ oybean oil, 6.8% glycerol mono ⁇ tearate and 0.10% BHT.
  • Glycerin was injected into zone 260 at 2.1 lb/hr.
  • a mixture of 98.62% ⁇ ucro ⁇ e and 1.38% sorbitol was added into the large feed port 262 at 194.7 lb/hr.
  • Corn syrup (100°F.) was injected into zone 260 at 39.9 lb/hr.
  • Peppermint flavor was injected into zone 260 at 2.1 lb/hr.
  • the zone temperature ⁇ (Z1-Z5, °F.) were set at 350, 350, 300, 55, and 55, respectively, and the screw temperature (SI) was set at 150°F.
  • the mixture temperatures (T1-T6, °F.) were measured as 326, 304, 264, 129, 101 and 85, respectively.
  • the screw rotation was set at 69 rpm.
  • Thi ⁇ fat mixture included 34% hydrogenated cottonseed oil, 34% hydrogenated soybean oil, 25.1% partially hydrogenated cottonseed oil, 6.8% glycerol monostearate and 0.10% BHT.
  • Glycerin was injected into zone 260 at 2.1 lb/hr.
  • a mixture of 98.62% sucrose and 1.38% sorbitol was added into the large feed port 262 at 194.7 lb/hr.
  • Corn syrup (100°F.) was injected into zone 260 at 39.9 lb/hr.
  • Peppermint flavor was injected into zone 260 at 2.1 lb/hr.
  • the zone temperatures (Z1-Z5, °F.) were set at 350, 350, 300, 55, and 55, re ⁇ pectively, and the ⁇ crew temperature (SI) wa ⁇ ⁇ et at 150°F.
  • the mixture temperature ⁇ (T1-T6, °F.) were measured as 338, 300, 260, 125, 101 and 86 respectively.
  • the screw rotation was set at 69 rpm.
  • the finished product had good chew characteristics and there was no evidence of rubber lumps.
  • a blend of 9.271% medium molecular weight polyvinyl acetate, 74.152% low molecular weight polyvinyl acetate, 7.306% high molecular weight terpene resin, 7.184% low molecular weight terpene resin and 2.087% color was added at 25.08 lb/hr into the second large feed port 232.
  • Polyisobutylene preheated to 250°F was also added into the second large feed port at 3.51 lb/hr.
  • a fat mixture (225°F) was injected into zone 240 at a total rate of 14.16 lb/hr.
  • This fat mixture included 37% hydrogenated cotton ⁇ eed oil, 22% hydrogenated ⁇ oybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
  • Glycerin was injected into zone 260 at 3.9 lb/hr.
  • a mixture of 85% ⁇ ucro ⁇ e and 15% dextro ⁇ e monohydrate wa ⁇ added into the large feed port 262 at 203.1 lb/hr.
  • Corn ⁇ yrup (100°F) was injected into zone 260 at 30.0 lb/hr.
  • a peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F.
  • the mixture temperatures (T1-T6, °F.) were measured as 324, 291, 154, 117, 110 and 89 respectively.
  • the screw rotation was set at 60 rpm.
  • the finished product had good chew characteristic and there was no evidence of rubber lumps.
  • a blend of 8.099% high molecular weight polyvinyl acetate, 64.777% low molecular weight polyvinyl acetate, 12.749% high molecular weight terpene resin, 12.551% low molecular weight terpene re ⁇ in and 1.823% color was added at 19.74 lb/hr. into the second large feed point 232.
  • Polyisobutylene preheated to 250°F was also added into the ⁇ econd large feed port at 3.51 lb/hr.
  • a fat mixture (225°F) was injected into zone
  • This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated ⁇ oybean oil, 15% partially hydrogenated cotton ⁇ eed oil, 23% glycerol mono ⁇ tearate, 2.4% ⁇ oy lecithin and 0.12% BHT.
  • Glycerin was injected into zone 260 at 3.9 lb/hr.
  • a mixture of 85% sucrose and 15% dextrose monohydrate wa ⁇ added into the large feed port 262 at 203.1 lb/hr.
  • Corn ⁇ yrup 100°F was injected into zone 260 at 30.0 lb/hr.
  • Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperature ⁇ (Z1-Z5, °F) were ⁇ et at
  • the screw temperature (SI) was set at 100°F.
  • the mixture temperatures (T1-T6, °F) were measured at 339, 289, 155, 112, 107 and 90, respectively.
  • the screw rotation was set at 60 rpm.
  • the finished product had good chew characteristic and there was no evidence of rubber lumps.
  • a blend of 7.189% high molecular weight polyvinyl acetate, 57.499% low molecular weight polyvinyl acetate, 16.981% high molecular weight terpene resin, 16.712% low molecular weight terpene re ⁇ in and 1.619% color was added at 22.24 lb/hr. into the second large feed port 232.
  • Polyisobutylene preheated to 250°F was added into the second large feed port at 3.51 lb/hr.
  • a fat mixture (225°F) was injected into zone 240 at a total rate of 14.16 lb/hr.
  • This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated soybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
  • Glycerin wa ⁇ injected into zone 260 at 3.87 lb/hr.
  • a mixture of 85% ⁇ ucrose and 15% dextrose monohydrate was added into the large feed port 262 at 203.1 lb/hr.
  • Corn syrup (100°F) was injected into zone 260 at 30.0 lb/hr.
  • Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
  • the zone temperatures (Z1-Z5, °F) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F.
  • the mixture temperature ⁇ (T1-T6, °F) were measured at 346, 250, 156, 115, 108 and 88, respectively.
  • the screw rotation was set at 60 rpm.
  • the finished product had good chew characteristics and there was no evidence of rubber lumps.
  • examples 31-33 the same formulation and procedures were used to make three additional base and gum products using a blade-and-pin mixer. The differences were that the formula amount of butyl rubber (isobutylene-isoprene copolymer) was dry blended at room temperature with hydrogenated soybean oil at a level of 1% (Ex. 31) , 2.5% (Ex. 32) and 5% (Ex. 33) of the butyl rubber. This provided an early addition of liquid oil in zone 220. The remaining hydrogenated soybean oil was added with the other fat ⁇ /oil ⁇ into the liquid injection port .
  • butyl rubber isobutylene-isoprene copolymer
  • Addition rate ⁇ of the rubber/filler/re ⁇ in were about 24.5 to 24.6 lb/hr.
  • Rates for the PVAC resin were about 17.9 to 18.2 lb/hr.
  • Rate ⁇ for the fat/oil composition were 13.8 to 19.1 lb/hr., and the rate for polyisobutylene was 3.5 lb/hr.
  • Examples 34-36 the ⁇ ame formulation and procedure ⁇ were u ⁇ ed to make three additional base and gum products using a blade-and-pin mixer. Differences of the ⁇ e three example ⁇ were that glycerol monostearate wa ⁇ blended with the butyl rubber. The level of glycerol mono ⁇ tearate used was 1% (Ex. 34), 2.5% (Ex. 35), and 5% (Ex. 36) of the butyl rubber. The remaining glycerol mono ⁇ tearate was added with the other fats/oils into the liquid injection ports.
  • the best mode of the invention may therefore exclude ingredients, proce ⁇ ⁇ tep ⁇ , material ⁇ or component ⁇ other than those listed above for inclusion or use in the invention.
  • the described embodiments are to be considered in all respects only as illustrative and not restrictive, and the ⁇ cope of the invention i ⁇ , therefore, indicated by the appended claim ⁇ rather than by the foregoing de ⁇ cription. All change ⁇ which come within the meaning and range of equivalency of the claims are to be embraced within their scope.

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Abstract

A process for continuously producing a chewing gum base comprises the steps of continuously adding a hard elastomer, a filler and lubricating agents into a continuous mixer, subjecting the elastomer, filler and lubricating agents to a dispersive mixing operation followed by a distributive mixing operation and continuously discharging the resulting chewing gum base from the mixer while the adding and mixing steps are in progress. The lubricating agents are introduced into the continuous mixer at a plurality of spatially separated feed inlets. Preferably part of the lubricating agents are introduced into the mixer with the hard elastomer and the filler prior to the dispersive mixing zone, and a portion of the lubricating agents are introduced into the mixer downstream of the dispersive mixing zone but prior to the distributive mixing zone. The lubricating agents may include elastomer solvents, soft elastomers, plastic polymers and softening agents such as fats, oils and waxes.

Description

CONTINUOUS CHEWING GUM BASE MANUFACTURING PROCESS USING ADDITION OF LUBRICATING AGENTS AT A PLURALITY OF FEED INLET LOCATIONS
CROSS REFERENCE TO RELATED APPLICATIONS
The present application is a continuation-in- part of the following U.S. Patent Applications: 1) Serial No. 08/126,319, filed September 24, 1993, now entitled "Continuous Chewing Gum Base Manufacturing
Process Using Highly Distributive Mixing"; 2) Serial No. 08/136,589, filed October 14, 1993, now entitled "Continuous Chewing Gum Base Manufacturing Process Using A Mixing Restriction Element", which is a continuation- in-part of Serial No. 08/126,319; 3) Serial No.
08/141,281, filed October 22, 1993, entitled "Continuous Gum Base Manufacturing Using Paddle Mixing"; 4) Serial No. 08/361,759, filed December 22, 1994, entitled "Continuous Chewing Gum Manufacture From Base Concentrate", which is a continuation-in-part of Serial
No. 08/305,363, filed September 13, 1994, entitled "Total Chewing Gum Manufacturing Using High Efficiency Continuous Mixing"; and 5) Serial No. 08/362,254, filed December 22, 1994, entitled "Total Chewing Gum Manufacture Using High Efficiency Continuous Mixing", which is also a continuation-in-part of Serial No. 08/305,363. The disclosure of each of the foregoing documents is hereby incorporated by reference.
FIELD OF THE INVENTION
This invention is directed to a continuous process for the manufacture of chewing gum bases. BACKGROUND OF THE INVENTION
A typical chewing gum base includes one or more elastomers, one or more fillers, one or more elastomer solvents, softening agents and optional plastic polymers and miscellaneous colors, flavors and antioxidants. Due primarily to the difficulty in melting and dispersing the elastomers homogeneously among the other gum base ingredients, gum base manufacture has typically been a tedious and time-consuming batch process. For example, one such conventional process uses a sigma blade batch mixer having a front to rear blade speed ratio of 2:1, and a mixing temperature of about 80-125°C.
In this conventional proceεε, initial portions of elastomer, elastomer solvent and filler are added to the heated sigma blade mixer and blended until the elastomer is melted or smeared and thoroughly mixed with he elastomer solvent and fillers. Then the remaining portions of elastomer, elastomer solvent, softening agents, fillers and other ingredients are added sequenti- ally, in a stepwise fashion, often with sufficient time for each stepwise addition to become completely mixed before adding more ingredients. Depending on the composition of the particular chewing gum bases and, in particular, the amount and type of elastomer, consider- able patience may be required to insure that each ingredient becomes thoroughly mixed. Overall, anywhere from one to four hours of mixing time can be required to make one batch of chewing gum base using a conventional sigma blade mixer. After mixing, the molten gum base batch must be emptied from the mixer into coated or lined pans, or pumped to other equipments such as a holding tank or a filtering device, then extruded or cast into shapes, and allowed to cool and solidify, before being ready for use in chewing gum. This additional processing and cooling requires even more time. Various efforts have been undertaken to try to simplify and reduce the time required for gum base manufacture. European Patent Publication No. 0 273 809, in the name of General Foods France, discloses a process for making nonadhesive chewing gum base by blending elastomer and filler components together in an industrial mill type mixer to form a nonadhesive premix, dividing the premix into fragments, and blending the premix fragments and at least one other nonadhesive gum base component together in a powder mixer. Alternatively, the premix fragments and other base components can be added to an extruder along with other chewing gum components to accomplish direct manufacture of chewing gum.
French Patent Publication No. 2 635 441, also in the name of General Foods France, discloses a process for making a gum base concentrate using a twin screw extruder. The concentrate is prepared by mixing high molecular weight elastomers and plasticizers in desired proportions and feeding them into the extruder. Mineral fillers are added to the extruder downstream of the feed inlet of the elastomer/plasticizer blend. The resulting gum base concentrate has a high level of elastomers. The concentrate can then be mixed with the other gum base ingredients to provide a complete gum base. U.S. Patent No. 3,995,064, issued to Ehrgott et al., discloses the continuous manufacture of gum base using a sequence of mixers or a single variable mixer. U.S. Patent No. 4,187,320, issued to Koch et al., discloses a two stage process for preparing a chewing gum base. In the first stage, a solid elastomer, an elastomer solvent, and an oleaginous plasticizer are combined and mixed together under high shear. In the second stage, a hydrophobic plasticizer, a non-toxic vinyl polymer, and an emulsifier are added to the mixture and mixed using high shear.
U.S. Patent No. 4,305,962, issued to Del Angel, discloses an elastomer/resin masterbatch formed by mixing a finely ground ester gum resin with a latex elastomer to form an emulsion, coagulating the emulsion using sodium chloride and sulfuric acid, separating the coagulated solid crumbs from the liquid phase, washing the solid crumbs, and removing the excess water.
U.S. Patent No. 4,459,311, issued to DeTora et al., discloses making gum base using two separate mixers - a high intensity mixer for pre-plasticizing the elastomer in the presence of a filler, followed by a medium intensity mixer for ultimately blending all the gum base components together.
U.S. Patent No. 4,968,511, issued to D'Amelia et al., discloses that chewing gum can be made directly in a one-step compounding process (without making an intermediate gum base) if certain vinyl polymers are used as the elastomer portion.
Several publications disclose that a continuous extruder can be used to make the ultimate chewing gum product after a separate process has previously been used to make the chewing gum base. These publications include U.S. Patent No. 5,135,760, issued to Degady et al.; U.S. Patent No. 5,045,325, issued to Lesko et al., and U.S. Patent No. 4,555,407, issued to Kramer et al.
Notwithstanding the prior efforts described above, there is a need and desire in the chewing gum industry for a continuous process which can effectively and efficiently be used to make a variety of complete chewing gum bases without limiting the type or quantity of elastomer employed, and without requiring preblending or other pretreatment of the elastomer.
Continuous gum base manufacturing processes, while desirable, present a number of difficulties. One of these is that continuous equipment has a given processing length once set up for operation. This length is limited in practice by what is commercially available, and is often less than what may be desired from the gum base manufacture's standpoint. As a result, continuous mixing operations have less degrees of freedom than traditional batch processes. For example, in a batch process, if longer mixing times are needed, it is a simple matter to continue mixing. However, the residence time in a continuous mixer is a function of the operating speed and feed rates. Therefore, to change the mixing time, some other factor must be adjusted and accommodated. Further, in a batch process, additional ingredients can be added at any time. Commercial continuous mixers have a limited number of feed inlets at fixed positions. Therefore the additional ingredients can be added at only preset points in the mixing process.
Also, in a batch mixer, dispersive and distributive mixing can be independently varied and controlled. On a continuous mixer, changes to one type of mixing will often also affect the other type of mixing. If the amount of the machine used for high shear mixing is increased, there is less machine available for distributive mixing. Also, if the speed is increased, heat may be generated beyond the ability of the cooling capabilities of the equipment.
One of the particular problems that has been encountered during development of continuous gum base manufacturing processes is that the properties of the chewing gum base, particularly the softness of the chew, is a function of the gum base ingredients and the mixing conditions that are applied to those ingredients. However, the mixing conditions are also a function of the gum base ingredients, as well as the type of mixing elements being used, the temperature and viscosity of the ingredients and the fullness of the mixer barrel. For example, if there is a high content of elastomer solvent in the base, less aggressive mixing occurs in the mixer because the elastomer solvent acts as a lubricant. Conversely, if the filler level in the gum base is high, the mixing is very aggressive, and may cause excessive breakup of the elastomer. SUMMARY OF THE INVENTION
It has been discovered that one way to control the mixing process, particularly during dispersive mixing where hard elastomers are masticated, yet at the same time provide all of the ingredients desired in the chewing gum base, is to add gum base ingredients that act as lubricating agents at a plurality of feed inlet locations in the continuous mixing process.
In one aspect, the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having at least one dispersive mixing zone and at least one distributive mixing zone and a plurality of spatially separated feed inlets, at least a portion of the hard elastomer and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located before the end of the dispersive mixing zone and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located downstream of the dispersive mixing zone and before the end of the distributive mixing zone; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
In a second aspect, the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer comprising a plurality of spatially separated feed inlets and a barrel having a predetermined length, at least a portion of the hard elastomer and a portion of the lubricating agents being introduced into one or more feed inletε located within the first 40% of the barrel length and a portion of the lubricating agents being introduced through one or more feed inlets located within the last 60% of the barrel length; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer. In a third aspect, the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having a plurality of spatially separated feed inlets, high shear mixing elements and low shear mixing elements downstream from the high shear mixing elements, at least a portion of the hard elastomer and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located at or before the high shear mixing elements and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located downstream of the high shear mixing elements and at or before the low shear mixing elements; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
In a fourth aspect, the invention is a process for continuously producing a chewing gum base comprising the steps of continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having at least one dispersive mixing zone and at least one distributive mixing zone and a plurality of spatially separated feed inlets, at least a portion of the hard elastomer, a portion of the lubricating agents and at least a portion of the filler being introduced into the mixer through one or more feed inlets located before the end of the dispersive mixing zone and a portion of the lubricating agents being introduced into the mixer through one or more feed inlets located downstream of the dispersive mixing zone and before the end of the distributive mixing zone, the ratio of the amount of lubricating agents added before the end of the dispersive mixing zone to the amount of lubricating agents added downstream of the dispersive mixing zone being optimized so that the gum base contains a desired amount of lubricating agents and the dispersive mixing is effective to properly masticate the hard elastomer; subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and continuously discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
The invention has numerous advantages. First, chewing gum base is produced in a continuous process. If desired, the output can be used to supply a continuous chewing gum production line or, if sufficient mixing can be accomplished in the first part of the mixer, the complete chewing gum can be produced in one mixer. Second, the average residence time for gum base ingredients is reduced from hours to minutes. Third, all of the necessary addition and gum base compounding steps can be performed in sequence, preferably using a single continuous mixing apparatus. Fourth, the preferred embodiment provides improved metering and mixing of intermediate and low viscosity gum base ingredients by adding these ingredients in the liquid state under pressure. Fifth, the invention is effective for a wide range of gum base compositions, including different gum base elastomers and elastomer percentages, without requiring preblending or other pretreatment of the elastomers. Sixth, the gum base can be produced on demand, eliminating finished base inventory. This allows maximum flexibility to react to market demands and formula changes. Seventh, high quality gum bases, including those containing high levels of fats, oil and/or low melting point waxes, can be made on a continuous basis.
The foregoing and other features and advantages of the invention will become further apparent from the following detailed description of the presently preferred embodiments, read in conjunction with the accompanying examples and drawings. BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 depicts a schematic representation of a twin screw extruder set up for use in practicing the present invention.
FIG. 2 depicts a set of shearing disks used in the extruder of FIG. 1.
FIG. 3 depicts a set of toothed elements used in the extruder of FIG. 1.
FIG. 4 depicts a set of kneading disks used in the extruder of FIG. 1. FIG. 5 depicts a plurality of kneading disks, set up in a helical fashion, to form kneading blocks.
FIGS. 6a-e depict schematic sequential representations of gum base ingredients during the mixing process. FIG. 7 is a perspective view of a single flat mixing paddle as used in practicing another embodiment of the invention.
FIG. 8 is a side view of the mixing paddle of FIG. 1. FIG. 9a is a front view of the mixing paddle of
FIG. 7, shown at zero degrees rotation (referred to as the no. 1 position) . FIG. 9b is a front view of the mixing paddle of FIG. 7, shown at 45 degrees counter-clockwise rotation (referred to as the no. 2 position) .
FIG. 9c is a front view of the mixing paddle of FIG. 7, shown at 90 degrees counter-clockwise rotation (referred to as the no. 3 position) .
FIG. 9d is a front view of the mixing paddle of FIG. 1, shown at 135 degrees counter-clockwise rotation (referred to as the no. 4 position) . FIG. 10a is a perspective view of a feeding element (not a paddle element) used in the feed areas of a paddle mixer.
FIG. 10b is a front view of the feed element of FIG. 10a. FIG. 11a is a perspective view of a forward helical mixing paddle which can be used in a paddle mixer.
FIG. lib is a front view of the forward helical mixing paddle of FIG. 11a. FIG. lie is based on a top view of the forward helical mixing paddle of 11a, showing only the top intersection line 92 superimposed over the bottom intersection line 90, and a reference line 91.
FIG. 12a is a perspective view of a reverse helical mixing paddle which can be used in a paddle mixer.
FIG. 12b is a front view of the reverse helical mixing paddle of FIG. 12a.
FIG. 12c is based on a top view of the reverse helical mixing paddle of FIG. 12a, showing only the top intersection line 92 superimposed over the bottom intersection line 90, and a reference line 91.
FIG. 13 is a perspective view of an overall paddle mixing configuration of a paddle mixer. FIG. 14 is a schematic illustration of a barrel and feeder arrangement which can be used in conjunction with the paddle mixer configuration shown in FIG. 13. FIG. 15 is a cross-sectional view taken along line 15-15 of FIG. 14, showing the relationship between the rotating paddles and the barrel wall.
FIG. 16 is a schematic illustration of two paddle mixers arranged in series.
FIG. 17 is a partial exploded perspective view of a Buss high efficiency, blade-and-pin mixer used to practice another embodiment of the invention, illustrating a mixing barrel and mixing screw arrangement.
FIG. 18a is a perspective view of an on-screw element used on the upstream side of a restriction ring assembly in the high efficiency mixer of FIG. 17.
FIG. 18b is a perspective view of an on-screw element used on the downstream side of the restriction ring assembly in the high efficiency mixer of FIG. 17.
FIG. 18c is a perspective view of a restriction ring assembly used in the high efficiency mixer of FIG. 17. FIG. 19 is a perspective view showing the relative positioning of the elements of FIGS. 18a, 18b and 18c in the high efficiency mixer of FIG. 17.
FIG. 20 is a perspective view of a low-shear mixing screw element used in the high efficiency mixer of FIG. 17.
FIG. 21 is a perspective view of a high-shear mixing screw element used in the high efficiency mixer of FIG. 17.
FIG. 22 is a perspective view of a barrel pin element used in the high efficiency mixer of FIG. 17.
FIG. 23 is a schematic diagram of an arrangement of mixing barrel pins and ingredient feed ports used with the high efficiency mixer of FIG. 17.
FIG. 24 is a schematic diagram of a presently preferred mixing screw configuration used with the high efficiency mixer of FIG. 17. DETAILED DESCRIPTION OF THE DRAWINGS AND PREFERRED EMBODIMENTS OF THE INVENTION
As noted earlier, gum base ingredients play a functional role during both mixing of the gum base and in the final chew characteristics of the chewing gum made from the base. During high shear, dispersive mixing, the filler acts to increase the shear. Some of the other gum base ingredients act as lubricating agents, reducing the shear. Most elastomer solvents, soft elastomers, plastic polymers and softening agents generally act as lubricating agents in continuous gum base manufacturing processes. Some lubricating agents such as polyisobutylene and the elastomer solvents cause the elastomer to disentangle, while others are not miscible with the elastomer and act only to lubricate the mixing and shearing operations.
To get an optimized shear in a limited amount of mixing space inside of continuous mixers, the amount of lubricating agents introduced into the mixer prior to the distributive mixing zone may therefore often be less than the amount of the lubricating agents desired in the final gum base. Thus, the methods of the present invention introduce the lubricating agents at a plurality of feed inlets so that a desired amount of shear can be achieved in a limited portion of the mixer, yet the final gum base can include all of the elastomer, filler and lubricating agents desired from a εensory and cost standpoint. Preferably, the portion of the lubricating agent added before the dispersive mixing will be one that acts as a solvent for the hard elastomer.
In one embodiment of the invention, it is preferable if the dispersive mixing can be accomplished in the first 40% of the barrel length of a continuous mixer. Therefore, in one embodiment of the invention, the first portion of lubricating agents will be introduced within the first 40% of the barrel length, and the second portion is added in the last 60% of the barrel length. The split of lubricating agents between one feed inlet and another can be split between types of lubricating agents, such as elastomer solvents and soft elastomers, or more preferably a split of one particular lubricating agent. For example, the terpene resin used in the gum base may preferably be split and added at two or more feed inlets.
The invention also contemplates a method of optimizing the process for making chewing gum base in a continuous process by adjusting the ratio of lubricating agents being introduced at the different feed inlets until the proper mixing is achieved. For instance, in one set of experiments, the same gum base ingredients were added at the same places in the mixer for each run, except that the elastomer solvent was split at various ratios between 85:15 and 55:45 as it was added at two different points to the mixer. The desired ratio that will result in optimum processing, and the range of ratios that will be experimented with, will of course depend on the gum base formulation, the type of mixer being used, and the arrangement of mixing elements in the mixer.
The chewing gum base made by the process of the present invention will be the same as bases made by conventional processes, and can thereafter be made into conventional chewing gums, including bubble gum, by conventional methods. The methods of production are well known and therefore not repeated here. Of course, specialized chewing gum, such as nonadhesive chewing gum and bubble gum, will use specialized gum base ingredients. However, those gum base ingredients can be combined using the processes herein described.
In general, a chewing gum composition typically comprises a water-soluble bulk portion, a water-insoluble chewable gum base portion and typically water-insoluble flavoring agents. The water-soluble portion dissipates with a portion of the flavoring agent over a period of time during chewing. The gum base portion is retained in the mouth throughout the chew.
The insoluble gum base generally comprises elastomers, elastomer solvents, softening agents and inorganic fillers. Plastic polymers, such as polyvinyl acetate, which behave somewhat as plasticizers, are also often included. Other plastic polymers that may be used include polyvinyl laurate, polyvinyl alcohol and polyvinyl pyrrolidone. Elastomers may constitute about 5 to about 95 percent by weight of the gum base, preferably between 10 and 70 percent by weight and most preferably between 15 and 45 percent by weight. Elastomers may include polyisobutylene, butyl rubber (isobutylene-isoprene copolymer) , styrene butadiene rubber, polyisoprene and butadiene rubber, as well as natural rubbers such as smoked or liquid latex and guayule, as well as natural gums such as jelutong, lechi caspi, perillo, massaranduba balata, massaranduba chocolate, nispero, rosindinha, chicle, gutta hang kang or mixtures thereof.
Elastomer used in chewing gum base can generally be categorized as hard elastomers or soft elastomers. Hard elastomers, which are most commonly butyl rubber and styrene butadiene rubber, generally have a high molecular weight, typically a Flory molecular weight over 200,000. A typical butyl rubber used in chewing gum base has a Flory molecular weight of about 400,000. Hard elastomers are those which require high shear, dispersive mixing to be utilized in chewing gum base. Hard elastomers generally do not flow at room temperature, even over an extended period of time, and are not pumpable even when heated to temperatures just below which substantial degradation occurs.
Soft elastomers have a lower molecular weight, typically a Flory molecular weight under 100,000.
Polyisobutylene and polybutadiene are typically soft elastomers. A typical polyisobutylene used in chewing gum base has a Flory molecular weight of about 53,000. Soft elastomers are generally pumpable at temperatures normally used to make chewing gum base, and will flow at room temperature, though often very slowly. In addition to Flory molecular weight, sometimes a Stodinger molecular weight is specified. Stodinger molecular weights are generally 1/3 to 1/5 of Flory molecular weights. For example, the polyisobutylene having a Flory molecular weight of 53,000 has a Stodinger molecular weight of about 12,000.
Sometimes number average or weight average molecular weights are reported, or the measurement method is not reported. In such instances, the above recitation of the functionality of the elastomer and how they are mixed in producing the chewing gum base can generally be used to classify the elastomer as hard or soft.
Elastomer solvents may constitute from about 0 to about 75 percent by weight of the gum base, preferably 5 to 45 percent by weight and most preferably 10 to 30 percent by weight. Elastomer solvents include natural rosin esters such as glycerol ester of wood rosin, glycerol ester of partially hydrogenated rosin, glycerol ester of polymerized rosin, glycerol ester of partially dimerized rosin, glycerol ester of rosin, pentaerythritol esters of partially hydrogenated rosin, methyl and partially hydrogenated methyl esters of rosin, pentaerythritol ester of rosin, resin ester of glycerol abietate or mixtures thereof. Elastomer solvents also include synthetics such as terpene resins derived from alpha-pinene, beta-pinene and/or d-limonene.
Softening agents include oils, fats, waxes and emulsifiers. Oils and fats, sometimes referred to as plasticizers, include tallow, lard, hydrogenated and partially hydrogenated vegetable oils, such as soybean oil, cotton seed oil, palm oil, palm kernel oil, coconut oil, sunflower oil and corn oil, cocoa butter, and lipids made from triglycerides of fatty acids. Commonly employed waxes include polywax, paraffin, microcrystalline and natural waxes such as candelilla, beeswax and carnauba. Paraffin waxes may be considered to be plasticizers. Microcrystalline waxes, especially those with a high degree of crystallinity, may be considered as bodying agents or textural modifiers.
Emulsifiers, which also sometimes have plasticizing properties, include glycerol monostearate, lecithin, mono and diglycerides of fatty acids, glycerol mono and distearate, triacetin, acetylated monoglyceride, and glycerol triacetate.
The gum base typically also includes a filler component. The filler component may be calcium carbonate, magnesium carbonate, talc, dicalcium phosphate or the like. The filler may constitute between about 5 and about 60 percent by weight of the gum base. Preferably, the filler comprises about 5 to about 50 percent by weight of the gum base.
Further, gum bases may also contain optional ingredients such as antioxidants, colors and flavors.
The temperature attained in the mixer often varies over the length of the mixer. The peak temperature in the dispersive mixing zone where high shear mixing elements are located, will preferably be over 175°F, more preferably over 250°F and most preferably over 300°F, and even 350°F for some gum base manufacturing processes.
The insoluble gum base may constitute between about 5 to about 80 percent by weight of the gum. More typically the insoluble gum base comprises between 10 and 50 percent by weight of the gum and most often about 20 to about 35 percent by weight of the gum.
The water soluble portion of the chewing gum may include softeners, bulk sweeteners, high intensity sweeteners, flavoring agents and combinations thereof. Softeners are added to the chewing gum in order to optimize the chewability and mouth feel of the gum. The softeners, which are also known as plasticizers or plasticizing agents, generally constitute between about 0.5-15% by weight of the chewing gum. The softeners may include glycerin, lecithin, and combinations thereof. Aqueous sweetener solutions such as those containing sorbitol, hydrogenated starch hydrolysates, corn syrup and combinations thereof, may also be used as softeners and binding agents in chewing gum.
Bulk sweeteners constitute between 5-95% by weight of the chewing gum, more typically 20-80% by weight of the chewing gum and most commonly 30-60% by weight of the chewing gum. Bulk sweeteners may include both sugar and sugarless sweeteners and components. Sugar sweeteners may include saccharide containing components including but not limited to sucrose, dextrose, maltose, dextrin, dried invert sugar, fructose, levulose, galactose, corn syrup solids, and the like, alone or in combination. Sugarless sweeteners include components with sweetening characteristics but are devoid of the commonly known sugars. Sugarless sweeteners include but are not limited to sugar alcohols such as sorbitol, mannitol, xylitol, hydrogenated starch hydrolysates, maltitol, and the like, alone or in combination. High intensity sweeteners may also be present and are commonly used with sugarless sweeteners. When used, high intensity sweeteners typically constitute between 0.001-5% by weight of the chewing gum, preferably between 0.01-1% by weight of the chewing gum. Typically, high intensity sweeteners are at least 20 times sweeter than sucrose. These may include but are not limited to sucralose, aspartame, salts of acesulfame, alitame, saccharin and its salts, cyclamic acid and its salts, glycyrrhizin, dihydrochalcones, thaumatin, monellin, and the like, alone or in combination.
Combinations of sugar and/or sugarless sweeteners may be used in chewing gum. The sweetener may also function in the chewing gum in whole or in part as a water soluble bulking agent. Additionally, the softener may provide additional sweetness such as with aqueous sugar or alditol solutions. Flavor should generally be present in the chewing gum in an amount within the range of about 0.l- 15% by weight of the chewing gum, preferably between about 0.2-5% by weight of the chewing gum, most preferably between about 0.5-3% by weight of the chewing gum. Flavoring agents may include essential oils, synthetic flavors or mixtures thereof including but not limited to oils derived from plants and fruits such as citrus oils, fruit essences, peppermint oil, spearmint oil, other mint oils, clove oil, oil of wintergreen, anise and the like. Artificial flavoring agents and components may also be used in the flavor ingredient of the invention. Natural and artificial flavoring agents may be combined in any sensorially acceptable fashion. Optional ingredients such as colors, emulsifiers, pharmaceutical agents and additional flavoring agents may also be included in chewing gum.
The preferred process of the present invention may be carried out with a variety of continuous mixing equipment. In some embodiments of the invention, more than one piece of continuous mixing equipment will be coupled in series. As used in the claims, the term "a continuous mixer" means one mixer or a plurality of mixers in series. Three specific types of continuous mixing equipment are described in detail below and are shown in the attached drawings: twin screw extruders, paddle mixers and blade-and-pin mixers, which are specialized single screw extruders. Extruders are preferred for use in the present invention, particularly the blade-and-pin mixer. A. Twin Screw Extruders
In one embodiment, the invention may be carried out on a twin screw extruder such as depicted schematically in FIG. 1. The twin screw extruder used to practice the preferred embodiment of the invention will be set up with several different feed inlet locations where chewing gum base ingredients can be added. The screws inside the barrel of the extruder are equipped with different types of elements along the length of the screws. The different mixing zones are sometimes referred to as processing zones, and described by the type of elements employed in the zones. The barrel is typically made up of different sections. These sections may be heated or cooled independent of other sections. Heating and cooling is thus typically done by region of the extruder barrel, which generally coincides with the barrel sections. These regions of heating or cooling may or may not coincide with processing zones, depending on the lengths of the barrel sections and the elements in the processing zones.
While different equipment manufacturers make different types of elements, the most common types of elements include conveying elements, compression elements, reverse conveyance elements, homogenizing elements such as shearing disks and toothed elements, and kneading disks and blocks. Conveying elements generally have flights spiraling along the elements with wide gaps between the flights. These elements are used at feed inlet zones to quickly move material into the body of the extruder. Compression elements have flights with a pitch that narrows as the material moves along the flights. This results in compression and high pressure in the forward direction, which is required to force material downstream and through the other elements. Reverse conveyance elements have flights that are angled opposite those of the conveying elements. The flights rotate in a direction that would force material upstream. These elements provide a high back pressure and slow down movement of the material through the extruder. Of course, the extruded material still works its way opposite the flights to move downstream through the reverse elements. A reverse helical arrangement of kneading blocks can accomplish a similar result.
Shearing disks, as their name implies, impart high shearing forces on the material in the extruder, resulting in highly dispersive mixing. In a twin screw extruder, the shearing disks opposite one another on the two different screws have close fitting disk/slot elements, as depicted in FIG. 2. Toothed elements, as depicted in FIG. 3, have gear-like teeth that oppose a cylindrical spacer shaft on the other screw. Toothed elements impart highly distributive mixing. Often the toothed elements are made in matched sets, with a cylindrical shaft portion and a toothed portion as one unit. Kneading disks, as shown in FIG. 4, have an elliptical shape, and produce a kneading action in the material passing through the extruder. Often a plurality of kneading disks will be placed next to each other in a helical arrangement, as shown in FIG. 5, referred to as kneading blocks.
Highly distributive mixing can also be accomplished using reverse conveyance elements that have portions missing from the flights to allow flow counter to the direction of compression. These missing portions may be arranged as a groove through the flights cut parallel to the length of the element. Also, kneading blocks followed by reverse conveyance elements, to build up high back pressure, also produce highly distributive mixing.
Mixing-restriction elements produce a high back pressure and some mixing without overly restricting throughput. For this reason, nozzles or orifices are not suitable as mixing-restriction elements. As noted above, reverse conveyance elements provide back pressure, and are thus mixing-restriction elements. Shearing disks, like those shown in FIG. 2, also produce a high back pressure and are thus another example of a mixing- restriction element. The high back pressure is important so that other elements, such as those that produce highly distributive or highly dispersive mixing, will be able to function properly. Thus in the preferred embodiment of the invention, mixing-restriction elements are used after each mixing zone. It is most preferable to use a mixing- restriction element just prior to the gum base exiting the extruder.
These various types of elements, and other elements useful in twin screw extruders, are well known in the art and are commercially available. The elements are often specifically designed for the different types of commonly available twin screw extruders, which include co-rotation, counter rotation, intermeshing and tangential twin screw extruders. Elements intended for similar functions will vary in design depending on the type of extruder for which they are intended.
One specific type of element for a specific brand of extruder is a non-intermeshing polygon element sold by the Farrel Corporation, 25 Main Street, Ansonia, Conn. 06401, for the Farrel-Rockstedt co-rotating twin screw extruder. It is believed that the non-intermeshing polygons produce dispersive mixing.
In preferred embodiments of the invention, the dispersive mixing disentangles the elastomers with a minimum amount of degradation of the polymer chains.
Thus, while dispersive mixing will inevitably reduce the molecular weight of the polymer, it is preferable to control the dispersive mixing operation to minimize this molecular weight reduction. Preferably, the average molecular weight will not be reduced below the average molecular weight of the same polymers mixed into gum base using conventional processes. An adequate dispersive mixing will produce a smooth, rubbery fluid, with no detectable lumps of rubber. If only a few lumps of rubber are present they may be screened out or dispersed during subsequent mixing steps. However, if the number or size of lumps is excessive, or the processed elastomers and fillers are in the form of an agglomeration or grainy mass, the dispersive mixing applied is inadequate.
The distributive mixing should be sufficient to produce a homogeneous gum base, rather than a material that appears to be "sweating", or that has a marbled or swiss cheese texture. In the preferred embodiment of the invention, the highly distributive mixing is sufficient to incorporate softening agents, particularly fats, oils and waxes, to the same degree these softening agents are incorporated in conventional chewing gum base manufacturing processes.
As shown in FIG. 1, for practicing a preferred embodiment of the invention, a twin screw extruder 10 is set up with a first feed inlet location 12 adjacent a first processing zone 21 fitted with conveying elements 31, conveying and compresεion elements 32 and compression elements 35. The second processing zone 23 is equipped with a combination of toothed elements 33, as depicted in FIG. 3, and several sets of shearing disks 34, as depicted in FIG. 2. At the end of the second processing zone 23 the extruder 10 is equipped with a port 16 which is connected to a vacuum source (not shown) . The third processing zone 24 contains additional conveying elements 31, conveying and compression elements 32 and compression elements 35. A second feed inlet 13 is provided in the extruder adjacent this second set of conveying elements 31, for feeding additional gum base ingredients into the third processing zone 24. Feed inlet 13 allows for the addition of powdered ingredients as well as liquid ingredients from pump 41. The fourth processing zone 25 is fitted with kneading disks 36. At the beginning of the fifth processing zone 26, the twin screw extruder 10 has another inlet 15 connected to a pump 43 and a feed inlet 14 in the form of a port connected to a side feeder 42, which may be a single or twin screw extruder, or even a gear pump which can generate high pressure. The fifth processing zone 26 is fitted with conveying elements 31, conveying and compression elements 32 and compression elements 35, which force the gum base ingredients into the sixth and final processing zone 28. Zone 28 contains two sets of toothed elements 33, followed by reverse elements 39 and shearing disks 34. After passing through the shearing disks 34, the gum base ingredients exit the extruder 10.
It may be preferable to heat some of the ingredients, either to melt them or to lower their viscosity. As shown in FIG. 1, the extruder 10 may be set up with heated tanks 44 and 45, connected respectively to pumps 41 and 43, for this purpose. Other commonly used equipment, such as equipment to monitor the temperature and heat or cool the extruder, is not shown in FIG. 1. The equipment will also include conventional weighing and feeding devices for continuously adding granulated or powdered ingredients. All of the ingredients are preferably fed into the extruder by equipment that is controlled to operate at a steady state; although during startup it may be preferable to start feeding some ingredients before others, and to feed the ingredients in at different rates than those desired for steady-state operation. It will be understood that FIG. 1, as a schematic representation, shows the various components in their respective order from the standpoint of flow through the extruder 10. Typically the screws are mounted in a horizontal side-to-side position and feed inlets, especially those open to the atmosphere like the inlet 12 and 13, are placed vertically above the screws. While the arrangement of FIG. 1 is preferred for particular gum bases outlined in the examples below, other arrangements may be preferred for other gum bases. FIG. l depicts an extruder with three general areas of ingredient addition and six processing zones. For some gum bases, two, four or more ingredient feeding zones may be used, with different numbers of processing zones. FIG. 1 also depicts the use of one set each of long conveying elements 31, conveying and compression elements 32 and compression elements 35 in the first processing zone 21, a short set of conveying and compression elements 32 in zones 24 and 26, and a short set of conveying elements 31 and compression elements 35 in zone 26. In reality, one, two or more elements of different types and length may be used in these zones. FIG. 1 also depicts one set of toothed elements 33 and three sets of shearing disks 34 in zone 23, but different numbers of these elements, or different elements all together, may be used. Likewise in zones 25 and 28, different types of elements that produce distributive mixing may be used, dependent on the gum ingredients being mixed in those zones and the type of extruder being used.
FIGS. 6a-e represent the state of various gum base ingredients as they are compounded into chewing gum base. At the beginning, as shown in FIG. 6a, the high molecular weight (hard) elastomer 51 and medium molecular weight elastomer 52 are both in the form of granules or particles in which the elastomer molecules are tightly bound together. The filler 53 is in particulate form, but may not be homogeneously mixed with the elastomers 51 and 52. The elastomer solvent 54 may be present in the form of droplets. As mixing begins, depicted in FIG. 6b, the elastomer solvent 54 becomes associated with the elastomers 51 and 52. With the presence of the filler 53, elastomer solvent 54 and heat, the granules begin to come apart into individual elastomer molecules. Also, the filler 53 becomes more evenly distributed, and may have its particle size reduced. As the process continues, the elastomers 51 and 52 become disentangled, as shown in FIG. 6c. This disentangling is the result of subjecting the elastomers 51 and 52 to highly dispersive mixing.
After this step, the lower viscosity ingredients, such as polyvinyl acetate 55, may be added, as shown in FIG. 6d. Initially, this material will also be in discrete particles, or droplets as it melts. Further mixing and further ingredient additions, such as waxes 56 and emulsifiers 57, are subjected to distrib¬ utive mixing, as depicted in FIG. 6e. Continued highly distributive mixing produces a homogeneous chewing gum base, wherein discrete particles or droplets are not detectible by sensory perception.
The elastomer may be added at the first feed inlet 12 along with elastomer solvent such as resins and the filler. However, especially lower weight elastomers may be added at least partially at the second feed inlet 13. Portions of the filler may also be added at the second feed inlet 13. Polyvinyl acetate may be added via a powder feeder or the single screw extruder 42, or a twin screw extruder or gear pump, at the feed inlet port 14, while melted fats and waxes and oils are added at the last feed inlet 15. This will result in the filler, elastomer and some lubricating agents being subjected to highly dispersive mixing first before lower viscosity ingredients are added. The toothed elements 38, reverse elements 39 and shearing disk 40 after feed inlet 15 result in highly distributive mixing of all of the low viscosity gum base ingredients with the other gum base ingredients.
A preferred small scale extruder is a model LSM 30.34 counter-rotational, intermeshing and tangential twin screw extruder from Leistritz, Nϋrenberg, Germany. Other acceptable twin screw extruders include the Japan Steel Works Model TEX30HSS32.5PW-2V intermeshing co- and counter-rotating twin screw extruder, also known as the Davis Standard D-Tex Model, distributed by Crompton & Knowles Corporation, #1 Extrusion Dr. , Pawcatuck, CT 06379, and either the co-rotating or counter-rotating intermeshing twin screw extruders from Werner &
Pfleiderer Corporation, 663 E. Crescent Ave. , Ramsey N.J. 07446. It is preferred to have a long barrel length. A Werner & Pfleiderer co-rotational twin screw extruder can go up to a length to diameter (L/D) ratio of 48. The Japan Steel Works Model TEX30HSS32.5PW-2V extruder may be equipped to have an L/D of 58.
B. Paddle Mixers
Another type of continuous mixer that may be used to practice the present invention is a paddle mixer. A mixing paddle 85 having a flat (non-helical) configuration is shown in FIGS. 7-9. The term "mixing paddle" is defined herein as a four-sided mixing element having two flat surfaces 86 and 87, and two concave surfaces 88 and 89. The flat surfaces are parallel to each other and intersect only the concave surfaces. The concave surfaces oppose each other and intersect each other at two lines 90 and 91. A non-circular (preferably square) opening 94 passes through the center of each mixing paddle 85, in a direction perpendicular to the flat surfaces 86 and 87, and intersects both flat surfaces. The openings 94 are used for mounting a plurality of paddles on rotating shafts, in a predetermined sequence (FIG. 13) . Referring to FIGS. 9a-d, the mixing paddles 85 can be positioned on a shaft at the same or different rotational angles relative to each other. For purposes of the following description, the "No. 1 position" is defined pursuant to FIG. 9a, wherein a straight line drawn on the flat surface 87 and intersecting the lines
90 and 92 coincides with a reference line (for example, a vertical line) . The "No. 2 position" is defined pursuant to FIG. 9b, wherein a straight line drawn on the flat surface 87 and intersecting the lines 90 and 92 is 45 degrees counter-clockwise from the reference line. The "No. 3 position" is defined pursuant to FIG. 9c, wherein a straight line drawn on the flat surface 87 and intersecting the lines 90 and 92 is 90 degrees counter¬ clockwise from the reference line. The "No. 4 position" is defined pursuant to FIG. 9d, wherein a straight line drawn on the flat surface 87 and intersecting the lines 90 and 92 is 135 degrees counter-clockwise from the reference line.
Because the paddles 85 in FIGS. 9a-d are symmetrical, there is no need to further define the relative rotational positions of the paddles for angles of 180, 225, 270 and 315 degrees from the reference line. For example, a paddle having a rotational position of 180 degrees coincides exactly with a paddle having a rotational angle of zero (FIG. 9a) . Similarly, a paddle having a rotational angle of 225 degrees coincides exactly with a paddle having a rotation angle of 45 degrees (FIG. 9b) ; a paddle having a rotational angle of 270 degrees coincides exactly with a paddle having a rotational angle of 90 degrees (FIG. 9c) , and a paddle having a rotational angle of 315 degrees coincides exactly with a paddle having a rotational angle of 135 degrees (FIG. 9d) .
It is also understood that each mixing paddle 85 will be in constant rotation during operation of the paddle mixer, due to the rotation of the shafts supporting the paddles (FIG. 13) . For purposes of describing the mixing paddles in terms of relative rotational positions (i.e. relative to each other) as explained above, the reference line should be deemed to rotate as the paddles rotate. For example, if the mixing paddles shown in FIGS. 9a-d are positioned sequentially on a single shaft, and if the shaft is rotated 90 degrees, then the chosen reference line, initially vertical, would rotate to a horizontal position. In other words, the relative rotational positions of the mixing paddles in FIGS. 9a-d, defined respectively as 1-2-3-4, will not change during operation of the paddle mixer.
Referring to FIGS. 10a and 10b, the method of the invention also provides for the use of a minor portion of non-paddle elements known as forward conveying or feed elements 50. Each feed element 50 has a flat front surface 48, a flat back surface 49 parallel to the front surface, and a non-circular (preferably square) opening 46 perpendicular to and intersecting the front and back surfaces. However, unlike the mixing paddles described above, the feed elements do not have two concave surfaces intersecting at two lines. Instead, each feed element 50 includes portions of two alternating helical channels 47 and 59. The helical channels are more apparent in FIG. 13 wherein a plurality of feed elements 50 are combined in sequence on the rotating shafts 110 to form feed zones in the mixer. The primary purpose of the feed elements 50 is to convey chewing gum base ingredients forward to the regions of the mixer where paddle mixing takes place.
Referring to FIGS. 11a and lib, a type of mixing paddle known as a forward helical paddle 95 can also be used with the method of the invention. When used, the forward helical paddle 95 imparts a slight forward conveying action while mixing the gum base ingredients. Like the flat mixing paddles 85, each forward helical paddle 95 has two flat surfaces and two concave surfaces 88 and 89. The flat surfaces are parallel to each other and intersect only the concave surfaces. The concave surfaces oppose each other and intersect at two lines 90 and 92. Again, a non-circular (preferably square) opening 94 passes through the center of each mixing paddle 95 and intersects both flat surfaces. The difference between the forward helical paddle 95 and the flat mixing paddle 85 is that, in the flat mixing paddle 85, the lines 90 and 92 (defining the intersections of concave surfaces 88 and 89) are parallel to each other as shown in FIG. 8. In the forward helical paddle, the line 90 has been rotated counter-clockwise with respect to the line 92 so that the lines are no longer parallel, aε shown in FIG. lib. Similarly, the line 92 has been rotated clockwise with respect to the line 90. The effect of this rotation is to bend the concave surfaces 88 and 89 so that these surfaces have a mildly helical configuration.
Referring to FIGS. 12a and 12b, a type of mixing paddle known as a reverse helical paddle 96 can also be used with the method of the invention. When used, the reverse helical paddle 96 imparts a slight resistance to forward conveying of the gum base ingredients while mixing the ingredients. This causes a locally higher degree of mixer fill and slight elevation in pressure, in the vicinity of the reverse helical paddle 96.
The reverse helical paddle 96 is configured in the same fashion as the forward helical pattern 95 discussed above, except that the lines 90 and 92 (defining the intersections of concave surfaces 88 and
89) are rotated in the opposite directions. Referring to FIG. 12a, the line 90 has been rotated clockwise with respect to the line 92, and the line 92 has been rotated counter-clockwise with respect to the line 90. The effect of this rotation is to bend the concave surfaces 88 and 89 so that these surfaces have a mild reverse helical configuration.
The degree of rotation of lines 90 and 92 for the forward and reverse helical paddles 95 and 96 can be explained with reference to FIGS, lie and 12c. In
FIGS, lie and 12c, the helical paddles have been viewed from above and only the lines 90 and 92 of the paddles are shown, superimposed one on top of the other. A reference line 91 is also shown, indicating the positions of lines 90 and 92 if there were no rotation, as in a flat paddle 85. Referring to FIG. lie, the angle "a" is the amount of counter-clockwise rotation of line 90 present in a forward helical paddle 95. The angle "a" should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds. The angle "b" is the amount of clockwise rotation of line 92 present in a forward helical paddle 95. The angle "b" should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds.
Referring to FIG. 12c, the angle "a" is the amount of clockwise rotation of line 90 present in a reverse helical paddle 96. The angle "a" should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds. The angle "b" is the amount of counter-clockwise rotation of line 92 present in a reverse helical paddle 96. The angle "b" should be between about 5 and about 30 degrees, preferably between about 10 and about 18 degrees, most preferably about 13 degrees, 53 minutes, 50 seconds.
Referring to FIG. 13, the mixing paddles and feed elements are assembled on two parallel shafts 110 in a predetermined configuration. In the embodiment shown, for a 5-inch paddle mixer, each of the shafts 110 has an active length of 36 inches and a square cross-sectional area of 1.375 inches x 1.375 inches (1.891 square inches) . The parallel shafts 110 are spaced apart at a distance of 3.5 inches (center to center) . The shafts 110 are adapted for co-rotation (rotation in the same direction) inside a mixing barrel. Each of the shafts 110 supports an identical arrangement of mixing paddles and feed elements. The mixing paddles and feed elements on the adjacent shafts may intermesh, as shown in FIG. 13, but do not touch each other, as the shafts rotate. Each of the shafts 110 is long enough to accommodate thirty-six inches of elements, each having a length of 1 inch, a maximum diameter of 4.874 inches and a minimum diameter of 2 inches. Two or more 1-inch segments may be combined to make longer elements without affecting the operation. For instance, the feed elements 50 often have a length of 2 inches. For purposes of the invention, a large portion of each shaft should be covered with mixing paddles. Generally, at least about 40 percent of each shaft should be covered with mixing paddles. Preferably at least about 50 percent of each shaft is covered with mixing paddles, most preferably at least about 60 percent. Of the mixing paddles, a majority should be flat mixing paddles as opposed to forward helical or reverse helical paddles. In the embodiment shown in FIG. 13, 67 percent of the shaft length is covered with mixing paddles (24 one-inch elements) and 33 percent of the shaft length is covered with feed elements (6 two-inch elements) .
The mixer configuration 102 in FIG. 13 includes two feed zones 125 and 135, and two paddle mixing zones 130 and 150. The specific mixer configuration is indicated in Table 1 below. In Table 1 and other tables, the following abbreviations are used:
FC - feed conveying element (each occupying two 1-inch positions) FP - flat mixing paddle (each occupying one 1-inch position) FH - forward helical mixing paddle (each occupying one 1-inch position) RH - reverse helical mixing paddle (each occupying one 1-inch position) Table 1 : Mixer Confiαuration (Per Shaft I - FIG. 13
Longitudin Rotational Longitudina Rotational al Position Element Position I Position Element Position
1 FC 4 19 FP 3
2 FC 4 20 FC 3
3 FC 4 21 FC 3
4 FC 4 22 FC 3
5 FC 4 23 FC 3
6 FC 4 24 FP 3
7 FC 4 25 FP 3
8 FC 4 26 FP 3
9 FP 4 27 FP 1
10 FP 4 28 FP 1
11 FP 4 29 FP 1
12 FP 2 30 FP 3
13 FP 2 31 FP 3
14 FP 2 32 FP 3
15 FP 3 33 FP 4
16 FP 4 34 FP 1
17 FP 1 35 FP 2
18 FP 2 36 RH 1
The use of two or more feed zones and two or more mixing zones in the mixer configuration 102, permits sequential addition and mixing of different gum base ingredients. For example, a high viscosity portion including elastomer, filler, and some resin or polyvinyl acetate can be continuously fed to the first feed zone 125 in FIG. 13. These ingredients can then be thoroughly mixed in the first paddle mixing zone 130 before being combined with additional ingredients. A lower viscosity portion including waxes (when used) , fats, oils, colorants and additional resin or polyvinyl acetate can be continuously fed to the second feed zone 135. All gum base ingredients can then be thoroughly mixed in the second paddle mixing zone 150.
The mixer configuration 102 shown in FIG. 13 is, in practice, surrounded by one or more barrel seg¬ ments extending the length of the mixer configuration 102. FIG. 14 illustrates, schematically, a typical barrel 105 surrounding the mixer configuration 102. A motor 101 drives the shafts 110 which support the mixer elements. The gum base ingredients are fed through feed ports 103 and 123 in the barrel 105. The gum base remains in the mixer for a sufficient time to ensure homogeneity, ' for example, a time on the order of about 20-30 minutes, and exits through an exit nozzle 155. The barrel 105 may be heated or cooled. Heating may be accomplished using hot water or a steam jacket surrounding the barrel (not shown) . Cooling may be accomplished by supplying cooling water to a jacket surrounding the barrel 105. Alternative methods of heating and cooling may also be employed. Generally, heating is applied at the start up, but cooling iε applied in the latter stages to prevent overheating and base degradation.
The heating and cooling of the barrel should be supplied, as necessary, to maintain the product exit temperatures at about 90°C-150°C, preferably at about 100-135°C, during mixing of the gum base ingredients.
FIG. 15 is a sectional view of the barrel 105 which indicates how the paddle mixer is able to operate with longer residence times, compared to a conventional twin screw extruder. As shown in FIG. 15, the barrel wall 116 has the shape of two intersecting cylinders, each cylinder having a diameter larger than the largest diameter of the mixing paddle 85 contained therein. This barrel configuration resembles that of a standard twin screw extruder. However, unlike the screws of a twin screw extruder, the paddles 85 do not mostly fill the space defined by the barrel wall 116.
The mixing paddles 85 have a typically close tolerance with the barrel wall 116, and with each other, in the vicinity of the lines 90 and 92 where the concave surfaces intersect. For paddles 85 having a long diameter of 4.874 inches, the closeεt tolerance between each paddle and the barrel wall 116 may be on the order of about 0.048 inch to about 0.078 inch, and the closest tolerance between the two paddles may be on the order of about 0.060 inch to about 0.090 inch. However, away from the lines 90 and 92, the distance between each paddle 85 and the barrel wall 116 is much greater. Due to the unique design of the paddles 85, the percentage of barrel space occupied by the paddles 85 is much smaller than for a conventional twin screw extruder. Also, the pressure in the paddle mixer should remain below about 50 psig, preferably below about 20 psig, when there is a large percentage of paddles compared to other elements. Each paddle 85, when viewed from the front aε in FIG. 15, has a smaller width than height. Preferably, the ratio of height to width of each mixing paddle is more than 1.5:1. Most preferably, the ratio of height to width for each mixing paddle is more than 2:1.
The large amount of available barrel space also allows the method of the invention to be practiced at high residence times in paddle mixers. The high proportion of mixing paddles, especially flat paddles, also contributes to the longer residence times and lower pressure. The average residence time in the paddle mixer should be at least about 10 minutes, preferably more than 15 minutes, moεt preferably more than 20 minuteε.
The remaining operating parameters, e.g., mixer rpm, feed rates, production rates, etc. vary depending on the size of the mixer and on the specific gum base composition. A commercially available paddle mixer suitable for practicing the invention is a Teledyne Readco Continuous Processor, available from Teledyne Readco in York, Pennsylvania. These paddle mixers are available in a wide variety of sizes. Paddle diameters for the different size mixers range from 2 to 24 inches, and the ratios of mixer length to diameter (L/D) range from 4:1 to 14:1. For purpoεeε of the present invention, the maximum paddle diameter is preferably between 2 incheε and 5 inches, and the L/D is preferably about 7:1. The paddle mixer configuration and process conditions should be selected so that a homogeneous gum base product is achieved. In a particularly useful embodiment, two or more paddle mixers may be used in series, in the manner illustrated in FIG. 16. The use of two mixers in series allows greater flexibility for feeding different gum base ingredients at different locations. A combination of elastomer, filler and resin can be continuously fed via feed port 103 to the feed barrel 105 of the first mixer. These materials are mixed in the first mixer, after which additional resin can be added to the first mixer via feed port 123. The combined ingredients are blended in the first mixer, and leave the first mixer at the exit 155, whereupon they are immediately fed into the barrel 205 of the second mixer 208 (powered by motor 201) via the feed port 203. Polyvinyl acetate can also be continuously fed to the barrel 205 from hopper 207, via feed conveyor 209 and feed port 203.
Further ingredients, such as waxes or oils, can be injected into the second mixer from feed tanks 211 and 231, via pumps 213 and 233. Optionally, a portion of ingredients can be added into a downstream feed port 204. After all the components are mixed, the gum base leaves the second mixer via exit 255. A wide variety of different feeding and mixing arrangementε can also be employed using two or more paddle mixers in series, in order to achieve good dispersion of ingredients and a wide variety of gum base products.
In addition to the paddles described above, a wide variety of mixing paddles, available from various extruder companies, can be used. Paddles, often called kneading elements, must have the effect of mixing in an extruder. Paddles can be two-sided, three-sided, or multiple sided. The paddle mixer, which may be referred to as a compounder, has different characteristics than a typical extruder even though the same equipment may be used. The difference between an extruder and a compounder is the ratio of paddles or kneading elements to the conveying elements. Conveying elements and compression elements cause an extruder to build up pressure. Paddles or kneading elements do not build as much pressure in the extruder, thus there is more mixing with low pressure. If the extruder contains at least 40% kneading elements, then the pressure can be about one-fifth to one-tenth that of a typical extruder which uses more conveying and compression elements.
Nearly all extruders can be used as compounders. However, compounders which have a low L/D ratio of about 3:1 to 20:1 cannot generally be used as high pressure extruders. Also, compounders with this low L/D ratio have less effective shaft length and may require more paddle or kneading elements compared to conveying elements. For this type of compounder, mixing paddles should cover at least 50%, and preferably at least 60% of the shaft. Conversely, for an extruder having an L/D of about 20/1 to about 40/1, only about 40% of the shaft needs to be covered with mixing paddles or kneading elements. For extruders with high L/D ratios greater than 40/1, only about 30% of the shaft may need to be covered with mixing paddles or kneading elements.
One of the key advantages to the preferred embodiment of the paddle mixer disclosed above is that the residence time is much higher than in typical extruders. Many extruders provide a residence time of less than 2 minutes or even less than 1 minute. However, in the preferred paddle mixer described above, a residence time of at leaεt 10 minutes, and preferably at least 15-20 minutes, can be provided. C. Blade-and-Pin Mixers
The method of the present invention may also be advantageously performed using a continuous mixer whose mixing screw is composed primarily of precisely arranged mixing elements with only a minor fraction of simple conveying elements. A presently preferred mixer is a blade-and-pin mixer exemplified in Fig. 17. This mixer may be used to produce not only gum base, but an entire chewing gum composition. A blade-and-pin mixer uses a combination of selectively configured rotating mixer blades and stationary barrel pins to provide efficient mixing over a relatively short distance. A commercially available blade-and-pin mixer is the Buss kneader, manufactured by Buss AG in Switzerland, and available from Buss America, located in Bloomingdale, Illinois.
Referring to FIG. 17, a presently preferred blade-and-pin mixer 100 includes a single mixing screw 120 turning inside a barrel 140 which, during use, is generally closed and completely εurrounds the mixing εcrew 120. The mixing screw 120 includes a generally cylindrical shaft 122 and three rows of mixing blades 124 arranged at evenly spaced locations around the screw shaft 122 (with only two of the rows being visible in FIG. 1) . The mixing blades 124 protrude radially outward from the shaft 122, with each one resembling the blade of an axe.
The mixing barrel 140 includes an inner barrel housing 142 which is generally cylindrical when the barrel 140 iε cloεed around the εcrew 120 during operation of the mixer 100. Three rowε of εtationary pins 144 are arranged at evenly spaced locations around the εcrew εhaft 142, and protrude radially inward from the barrel housing 142. The pins 144 are generally cylindrical in shape, and may have rounded or bevelled ends 146.
The mixing screw 120 with blades 124 rotates inεide the barrel 140 and is driven by a variable speed motor (not εhown) . During rotation, the mixing εcrew 120 also moves back and forth in an axial direction, creating a combination of rotational and axial mixing which is highly efficient. During mixing, the mixing blades 124 continually pass between the stationary pins 144, yet the blades and the pins never touch each other. Also, the radial edges- 126 of the bladeε 124 never touch the barrel inner εurface 142, and the ends 146 of the pins 144 never touch the mixing screw shaft 122. FIGS. 18-22 illustrate various screw elements which can be used to configure the mixing screw 120 for optimum use. Figs. 18a and 18b illustrate on-screw elements 60 and 61 which are used in conjunction with a restriction ring assembly. The on-screw elements 60 and 61 each include a cylindrical outer εurface 62, a plurality of blades 64 projecting outward from the surface 62, and an inner opening 66 with a keyway 68 for receiving and engaging a mixing screw shaft (not shown) . The εecond on-screw element 61 is about twice as long as the first on-screw element 60.
FIG. 18c illustrates a restriction ring assembly 70 used to build back preεsure at selected locations along the mixing screw 120. The restriction ring assembly 70 includes two halves 77 and 79 mounted to the barrel housing 142, which halves engage during use to form a cloεed ring. The restriction ring assembly 70 includes a circular outer rim 72, an inner ring 74 angled as shown, and an opening 76 in the inner ring which receives, but does not touch, the on-screw elements 60 and 61 mounted to the screw shaft. Mounting openings 75 in the surface 72 of both halveε of the restriction ring assembly 70 are used to mount the halves to the barrel housing 142.
FIG. 19 illustrates the relationship between the restriction ring asεembly 70 and the on-screw elements 60 and 61 during operation. When the mixing screw 120 is turning inside the barrel 140, and reciprocating axially, the clearances between the on- screw elementε 60 and 61 and the inner ring 74 provide the primary means of passage of material from one side of the reεtriction ring aεsembly 70 to the other. The on- screw element 60 on the upstream side of the restriction ring assembly includes a modified blade 67 permitting clearance of the inner ring 74. The other on-screw element 61 is placed generally downstream of the restriction ring assembly 70, and has an end blade (not visible) which moveε close to and wipes the oppoεite surface of the inner ring 74.
The clearances between outer εurfaces 62 of the on-screw elements 60 and 61 and the inner ring 74 of the restriction ring assembly 70, which can vary and preferably are on the order of 1-5 mm, determine to a large extent how much pressure build-up will occur in the upstream region of the restriction ring asεembly 70 during operation of the mixer 100. It εhould be noted that the upεtream on-εcrew element 60 has an L/D of about 1/3, and the downstream on-screw element 61 has an L/D of about 2/3, reεulting in a total L/D of about 1.0 for the on-screw elements. The restriction ring aεεembly 70 has a smaller L/D of about 0.45 which coincideε with the L/D of the on-screw elements 60 and 61, which engage each other but do not touch the restriction ring asεembly.
Figε. 20 and 21 illuεtrate the mixing or "kneading" elementε which perform moεt of the mixing work. The primary difference between the lower εhear mixing element 80 of FIG. 20 and the higher εhear mixing element 78 of FIG. 21 iε the εize of the mixing bladeε which project outward on the mixing elements. In FIG. 21, the higher shear mixing blades 83 which project outward from the surface 81 are larger and thicker than the lower shear mixing blades 84 projecting outward from the surface 82 in FIG. 20. For each of the mixing elements 80 and 78, the mixing blades are arranged in three circumferentially-spaced rows, as explained above with respect to FIG. 17. The use of thicker mixing blades 83 in FIG. 21 means that there is less axial distance between the blades and also less clearance between the blades 83 and the stationary pinε 144 aε the screw 120 rotates and reciprocates axially (FIG. 17) . This reduction in clearance causes inherently higher shear in the vicinity of the mixing elementε 78. FIG. 22 illuεtrateε a εingle stationary pin 144 detached from the barrel 140. The pin 144 includes a threaded base 145 which permits attachment at selected locations along the inner barrel shaft 142. It is also possible to configure some of the pins 144 as liquid injection ports by providing them with hollow center openings.
FIG. 23 is a schematic view showing the preεently preferred barrel configuration, including the presently preferred arrangement of barrel pins 144. FIG. 24 is a corresponding schematic view illustrating the presently preferred mixing screw configuration. The mixer 200 whose preferred configuration is illuεtrated in FIGS. 23 and 24 has an overall active mixing L/D of about 19.
The mixer 200 includes an initial feed zone 210 and five mixing zones 220, 230, 240, 250 and 260. The zones 210, 230, 240, 250 and 260 include five possible large feed ports 212, 232, 242, 252 and 262, respectively, which can be used to add major (e.g. solid) ingredients to the mixer 200. The zones 240 and 260 are also configured with five εmaller liquid injection portε 241, 243, 261, 263 and 264 which are uεed to add liquid ingredients. The liquid injection ports 241, 243, 261, 263 and 264 include special barrel pins 144 formed with hollow centers, as explained above.
Referring to FIG. 23, barrel pins 144 are preferably present in most or all of the available locations, in all three rows as shown.
Referring to FIG. 24, the presently preferred configuration of the mixing εcrew 120 for moεt chewing gum products iε schematically illustrated as follows. Zone 210, which iε the initial feed zone, is configured with about 1-1/3 L/D of low shear elements, such as the element 40 shown in FIG. 4. The L/D of the initial feed zone 210 is not counted as part of the overall active mixing L/D of 19, discussed above, because its purpose iε merely to convey ingredientε into the mixing zoneε.
The first mixing zone 220 is configured, from left to right (FIG. 24) , with two low shear mixing elements 80 (FIG. 20) followed by two high shear elementε 78 (FIG. 21) . The two low εhear mixing elementε contribute about 1-1/3 L/D of mixing, and the two high εhear mixing elementε contribute about 1-1/3 L/D of mixing. Zone 220 haε a total mixing L/D of about 3.0, including the end part covered by a 57mm reεtriction ring asεembly 70 with cooperating on-screw elements 60 and 61 (not separately designated in FIG. 24) .
The reεtriction ring aεεembly 70 with cooperating on-εcrew elementε 60 and 61, εtraddling the end of the first mixing zone 220 and the start of the εecond mixing zone 230, have a combined L/D of about 1.0, part of which is in the second mixing zone 230. Then, zone 230 is configured, from left to right, with three low shear mixing elements 80 and 1.5 high shear mixing elements 78. The three low shear mixing elements contribute about 2.0 L/D of mixing, and the 1.5 high shear mixing elements contribute about 1.0 L/D of mixing. Zone 230 has a total mixing L/D of about 4.0.
Straddling the end of the second mixing zone 230 and the start of the third mixing zone 240 is a 60mm restriction ring assembly 70 with cooperating on-screw elements 60 and 61 having an L/D of about l.o. Then, zone 240 iε configured, from left to right, with 4.5 high shear mixing elements 78 contributing a mixing L/D of about 3.0. Zone 240 also has a total mixing L/D of about 4.0. Straddling the end of the third mixing zone 240 and the start of the fourth mixing zone 250 is another 60mm reεtriction ring aεεembly 70 with cooperating on- εcrew elementε having an L/D of about 1.0. Then, the remainder of the fourth mixing zone 250 and the fifth mixing zone 260 are configured with eleven low shear mixing elements 80 contributing a mixing L/D of about 7%. Zone 250 has a total mixing L/D of about 4.0, and zone 260 has a total mixing L/D of about 4.0.
Example 1
Gum base was made on a continuous basis using a Leistritz model LSM 30.34 counter-rotational, intermeshing and tangential extruder in intermeshing mode with a barrel diameter of 30.3 mm set up with the following elements (given in order proceeding from first feed inlet to the output end of the extruder and using the Leistritz part designation for each element) : FF-1-30-120 (conveying element)
KFD-1-30/20-120 (conveying and compression element)
FD-3-30-120 (compresεion element)
ZSS-2-R4 (toothed element)
ZSS-2-R4 KS (εhearing diεk)
KS
FF-1-30-120
KFD-1-30/20-120
FD-3-30-120 ZSS-2-R4
ZSS-2-R4
ZSS-2-R4
KS
The die at the end of the extruder had a 1mm hole. The extruder had two feeding zoneε, each one adjacent the FF-1-30-120 conveying elementε. A powder blend of ground butyl rubber, calcium carbonate and terpene resin at a ratio of 6:23:17 was fed at a rate of 3 kg/hr in the first feed zone. Polyiεobutylene at 50- 80°C waε alεo fed at the firεt feed zone at a rate of 0.39 kg/hr. A powder blend of 5 partε glycerol monostearate, 8 parts hydrogenated cottonseed oil, 5 partε hydrogenated εoybean oil, 3 partε high molecular weight polyvinyl acetate and 21 partε low molecular weight polyvinyl acetate was fed into the second feeding zone at a rate of 2.74 kg/hr, along with a blend of 3 parts partially hydrogenated εoybean oil and 3 parts lecithin heated to 30°C and fed at a rate of 0.4 kg/hr. The ratio of elastomers to fats and oils was 0.75:1. The set temperature (except for the die, which did not have a temperature control) and actual temperature of the extruder housing during operation were as followε:
Zone 1 2 3 5 6 7 Die
Set 90°C. 90°C. 95°C. 130-C. 130°C. 130°C. 110°C.
Tempera¬ ture
Actual 90°C. 990C. 95-C. 130°C. 130-C. 130-C. 110-C. 115-C. Tempera¬ (est.) (est.) ture
The extruder was operated at a speed of 100 rpm and drew 9 amps. A chewing gum base was produced which had no rubber particles or segregated oil. However, some of the polyvinyl acetate was not fully incorporated. This would be incorporated as the base was used to make chewing gum, or if desired, could be eliminated by using a single screw extruder as a side feeder/pre-melter for the polyvinyl acetate.
Example 2
The same extruder set up and temperatureε aε uεed in Example 1 were uεed to continuously make another chewing gum base. A powder blend of ground butyl rubber and calcium carbonate at a ratio of 15:31 was fed into the first zone at a rate of 3 kg/hr, along with polyisobutylene heated to 50-80°C and fed at a rate of 2.08 kg/hr. A powder blend of 22 parts low molecular weight polyvinyl acetate, 13 parts hydrogenated cottonseed oil, 3 partε glycerol monostearate and 13 partε hydrogenated soybean oil was fed into the second feed inlet at a rate of 6.63 kg/hr, along with partially hydrogenated soybean oil heated to 30-60°C and fed at a rate of 1.3 kg/hr. The ratio of elastomer to fats and oils was 0.65:1. The extruder was operated at lOOrpm, and drew 7-8 amps. A complete chewing gum base was prepared, although it was not as well mixed as the base of Example 1 and there were difficulties in material accumulating at the second feed zone.
Example 3
An Leistritz Model 30.34 twin εcrew extruder iε εetup as shown in FIG. 1, with the following elementε (the numberε to the left in parentheεiε repreεent reference numbers from FIG. 1) :
(31) FF-1-30-120
(32) KFD-1-30/20-120
(35) FD-3-30-120
(33) ZSS-2-R4
(34) KS
(34) KS
(34) KS
(31) FF-1-30-120
(32) KFD-1-30/20-60
(35) FD-3-30-120
(36) 18 kneading diεks, stacked in 2 sets of 2 and 4 εetε of 3, with a 90° εet off between each set.
(31) FF-1-30-60
(32) KFD-1-30/20-60
(35) FD-3-30-30
(33) ZSS-2-R4
(33) ZSS-2-R4
(39) FF-1-30-30 (set up for reverse operation)
(34) KS
The overall length of these elements is 1060 mm, giving a
L/D for a 30.3 mm barrel of about 35.
As specified in Table 2, gum base ingredients are added at the specified rates to the extruder 10 at the locations specified. The rateε liεted are for steady state operation. Table 2
Figure imgf000047_0001
The total feed rate iε 25 lb/hr. The temperature iε controlled so that the mixture is at about 115°C. - 125°C. The ratio of elastomerε to fatε and oils is 0.92:1.
While the examples have been given for relatively small scale operations, the procesε is readily scaled up. When using twin screw extruders, scale up is accomplished by using a larger barrel diameter, such as 6 inches, and a longer length, but maintaining the same L/D ratio. For an L/D of 45, a 6 inch barrel would be 22.5 feet in length. If larger machines generate more heat than can eaεily be removed, the rpm of the extruder may need to be reduced, or cooled εhaftε and mixing elementε could be used. Also, by putting in some of the resin at the firεt feed zone, the heat generated during mixing should be reduced.
When conducting the experiment relating to Example l, the polyisobutylene was originally added at the second feed inlet. This was possible during startup, but when the blend of fats and polyvinyl acetate were also added, the fatε melted and lubricated the screws so that they no longer drew in the polyisobutylene. This iε why the polyisobutylene is introduced at the first feed zone in Example 1.
In Exampleε l and 2, εince the butyl rubber was ground before it was used, a portion of the filler and the ground butyl rubber were premixed (at a ratio of filler to butyl rubber of 1:3) to help keep the ground butyl rubber in a form that allowed it to be fed into the extruder as a powder blend. This filler was included in the overall ratios cited in the examples.
It has been found that high quality chewing gum bases, with high levels of fats and oils such as those in Examples 1-3, can be successfully produced on a continuous basis using the present invention. It is noted that the highly distributive mixing operation followed by the mixing-reεtriction elements used in the examples is particularly uεeful for incorporating the fatε and oilε in with the elaεtomers and fillers.
Example 4
Using a 5-inch paddle diameter Teledyne Readco Continuous Mixer, having the mixer configuration illustrated in FIG. 13 and described in Table 1 above, chewing gum baεe waε made aε followε. A mixture of ground isobutylene-iεoprene copolymer (2-7 mm. particle size) , calcium carbonate (<12 micron particle size) , and terpene resin at a ratio of 8:21:17 was fed at a rate of 0.383 lb/min. at the first feed inlet. In the second feed inlet, three mixtures were added: 1) a powder blend of polyvinyl acetate, glycerol monostearate, and hydrogenated soybean and vegetable oils at a ratio of 24:5:13 fed at a rate of 0.35 lb/min., 2) 6 parts molten polyisobutylene at 130°C, fed at a rate of 0.05 lb/min., and 3) 6 partε of a 1:1 ratio of hydrogenated cottonseed oil and lecithin at 70°C fed at a rate of 0.05 lb/min.
Overall, the production rate for the gum base was 50 pounds per hour. The gum base was manufactured using an extruder rpm of 400, initial barrel temperatures of 270-275°F, and a product exit temperature of about 128°C. The average residence time in the paddle mixer waε about 30-40 minuteε.
Example 5
This example was performed using a 2-inch paddle diameter Teledyne Readco Continuous Mixer and a 5-inch paddle diameter Teledyne Readco Continuous Mixer in series, similar to the arrangement shown in FIG. 16, with the 2-inch paddle diameter mixer being first. The mixers were configured with the objective of accomplishing disperεive mixing of rubber using the 2-inch compounder, and distributive mixing of oil using the 5-inch compounder. Specifically, the 2-inch and 5-inch compounders were configured as described in Tables 3 and 4.
The 2-inch compounder included 4 inches of conveying elements, and a balance of reverse helical and flat paddles, each 0.53 inch long. Overall, twenty-five reverse helical and flat paddleε (total) were used, for a total paddle length of 13.25 inches. The total active length of each of the shafts carrying the paddles was 17.25 inches. The 5-inch compounder used paddles and conveying elementε with the dimensions described above.
Table 3: Mixer Configuration (Per Shaft) For 2-Inch Teledvne Readco Mixer
Longitudin Rotational Longitudina Rotational al Position "Element Position I Position Element Position
1 FC 4 16 FP 2
2 FC 4 17 FP 4
3 FC 4 18 FP 4
4 FC 4 19 FP 4
5 FP 4 20 FP 2
6 FP 4 21 FP 2
7 FP 4 22 FP 2
8 FP 2 23 FP 3
9 FP 2 24 FP 4
10 FP 2 25 FP 1
11 FP 4 26 FP 2
12 FP 4 27 FP 4
13 FP 4 28 FP 4
14 FP 2 29 RH 2
15 FP 2
Table 4: Mixer Configuration (Per Shaft) For 5-Inch Teledvne Readco Mixer
Longitudin Rotational Longitudina Rotational al Position Element Position I Position Element Position
1 FC 4 19 FP 2
2 FC 4 20 FP 2
3 FC 4 21 FP 4
4 FC 4 22 FP 4
5 FC 4 23 FP 4
6 FC 4 24 FP 2
7 FC 4 25 FP 2
8 FC 4 26 FP 2
9 FP 4 27 FP 4
10 FP 4 28 FP 4
1 1 FP 4 29 FP 4
12 FP 2 30 FP 1
13 FP 2 31 FP 2
14 FP 2 32 FP 3
15 FP 4 33 FP 4
16 FP 4 34 FP 2
17 FP 4 35 FP 2
18 FP 2 36 RH 4
The feed ports were arranged as follows Feed Port No. 1 - above longitudinal posi¬ tions 1 - 4 on 2-inch mixer
Feed Port No. 2 - above longitudinal posi- tionε 1 - 4 on 5-inch mixer
Feed Port No. 3
(oil injection) - at longitudinal poεition 9 on 5-inch mixer
Uεing the above mixer arrangement, chewing gum baεe was made as follows.
A mixture of ground iεobutylene-isoprene copolymer (2-7 mm particle size) and calcium carbonate at a ratio of 10:13 was fed at a rate of 0.192 lb/min. to feed port No. 1. Also added at feed port No. 1 was 16 parts polyisobutylene at 130°C at a rate of 0.133 lb/min. At feed port No. 2, 22 parts polyvinyl acetate and 29 parts of a powder blend of hydrogenated vegetable oil, glyorol monostearate, and hydrogenated soybean oil at a ratio of 13:3:13 were added at a rate of 0.425 lb/min. Also added at feed port No. 2 waε a liquid blend at 70°C of 5 partε hydrogenated cottonεeed oil and 5 partε lecithin at a rate of 0.083 lb/min. Feed port No. 3 waε not used.
Overall, the production rate for the gum base was 50 pounds per hour. The gum base waε manufactured uεing the following process conditions:
2-Inch Mixer 5-Inch Mixer RPM 314 450
Initial Barrel Temp., °F 265-270 225-230 Product Exit Temp., °C 164 133
Average Residence Time 5-10 min. 30-40 min.
About 60 pounds of gum base product was made at these conditions. The gum base had normal color, a smooth texture, and a homogeneous conεistency, except for an occasional wood sliver resulting from a previous use of the equipment.
Example 6 This example was performed using the same two- mixer arrangement described in Example 5. The 2-inch and 5-inch Teledyne Readco Continuous Mixers were configured as described in Tables 3 and 4, above. The feed ports were arranged as described in Example 5. Uεing the above mixer arrangement, bubble gum base was made as follows.
A mixture of styrene-butadiene rubber, calcium carbonate (<12 micron particle size) , and glycerol ester of wood rosin at a ratio of 9:46:18 was added at feed port No. l at a rate of 0.608 lb/min. At feed port No. 2, a mixture of glycerol ester of wood rosin, glycerol monostearate, and microcryεtalline wax (m.p. = 180°F) at a ratio of 20:1:6 was added at a rate of 0.175 lb/min. Feed port No. 3 was not used.
Overall, the production rate for the bubble gum base was 47 pounds per hour. The gum base was manufactured using the following process conditions:
2-Inch Mixer 5-Inch Mixer RPM 314 450
Initial Barrel Temp., °F not recorded 225-230 Product Exit Temp., °C 140 not recorded
Average Residence Time 2-6 min. 30-40 min.
About 40 pounds of bubble gum base was made at these conditions. The gum baεe had normal color, a εmooth texture, and a homogeneous consiεtency.
Example 7
Thiε example was performed using a two-mixer arrangement described in Example 5, except for the following changes. Again, the 2-inch Teledyne Readco Continuous Mixer was configured as described in Table 3 of Example 5. However, the 5-inch Teledyne Readco
Continuous Mixer was configured as described in Table 1 (Example 4) except that a reverse helical paddle was placed in position 19. The feed ports were arranged aε followε:
Feed Port No. 1 - above longitudinal positions 1
4 on 2-inch mixer
Feed Port No. 2 - above longitudinal positions 1 - 4 on 5-inch mixer
Feed Port No. 3 - above longitudinal positionε 20-
23 on 5-inch mixer
Using the above mixer arrangement, chewing gum base waε made as follows. A mixture of ground isobutylene-isoprene copolymer (2-7 mm particle size) , calcium carbonate (<12 micron particle size) , and terpene resin at a ratio of 8:21:17 was fed at a rate of 0.383 lb/min. at the first feed inlet. In the second feed inlet, a powder blend of polyvinyl acetate, glycerol monostearate, and hydrogenated εoybean and vegetable oil at a ratio of 24:5:13 were fed at a rate of 0.35 lb/min. In the third feed port, 6 partε of polyiεobutylene at 130°C at a feed rate of 0.05 lb/min. and 6 parts of a 50/50 mixture of hydrogenated cottonseed oil/lecithin at 70°C at a feed rate of 0.05 lb/min. were added.
Overall, the production rate for the gum base was 50 pounds per hour. The gum base was manufactured using the following proceεε conditionε:
2-Inch Mixer 5-Inch Mixer RPM 310 387
Initial Barrel Temp., °F 275-280 235-240 Product Exit Temp. , °C 162 120
Average Residence Time 2-6 min. 30-40 min.
About 40 pounds of gum base product was made at these conditionε. The gum base had normal color, a smooth texture, and a homogeneous conεistency, except for an occasional isolated undispersed particle.
Based on these and other runs, it was concluded that paddle mixing is an effective technique for manufacturing gum base on a continuous basis. The optimum process conditions, and the use of one or two mixers, vary depending on the specific gum base composition and the desired output rate.
Example 8 Gum base waε made on a continuouε basis using a
Japan Steel Works Incorporated model TEX30HSS32.5PW-2V twin screw extruder set up in a co-rotating mode with extremely aggressive kneading elements and two feed inlets.
"Extremely aggressive kneading elements" means that most of the extruder shaftε were covered with kneading elementε as paddleε. The arrangement was: 1/6 conveying elements at the first feed inlet, 1/3 kneading elements, then 1/6 conveying elements at the second feed inlet and 1/3 kneading elements. This results in paddles covering 67% of the shafts.
A mixture of ground styrene - butadiene rubber (2-7 mm particle size) , calcium carbonate (<12 micron particle size) and resin ester of glycerol abietate at a ratio of 9:46:18 was fed at a rate of 5.4 kg/hr at the first feed inlet. A mixture of resin ester of glycerol abietate, glycerol monoεtearate and microcryεtalline wax at a ratio of 20:1:6 was fed at a rate of 2 kg/hr at the second feed inlet. The extruder waε operated with temperature controls for seven heating zones and the die. The set point and actual temperatures were as follows:
Zone 1 2 3 4 5 6 7 Die
Set 130°C 130°C 130°C 130°C 100°C 100°C 100°C 80°C Temperature
Actual 129°C 131 °C 122°C 130°C 100°C ιoo°c 100°C 139°C Temperature
The first feed inlet waε between zones 1 and 2 and the second feed inlet was between zones 3 and 4. The extrudate exited at 118°C. The machine was run at 200 rpm, drawing 21 ampε. The extrudate was a finished gum base that had no lumps.
Example 9
Thiε example waε performed uεing a two-mixer arrangement with two 5-inch Teledyne Readco Continuous Mixer Compounders. The first compounder was configured the same as in Table 4 of Example 5. The second compounder was configured based on Table 1, shown previously. This configuration is also shown in Figure
13.
The feed portε were arranged as follows:
Feed Port No. 1 - above longitudinal positions 1 - 4 on first 5-inch mixer
Feed Port No. 2 - above longitudinal positions 1 -
4 on second 5-inch mixer Feed Port No. 3 - above longitudinal positions 20-
23 on εecond 5-inch mixer.
Uεing the above mixer arrangement, chewing gum base was made as follows:
A mixture of ground isobutylene-iεoprene copolymer (2-7 mm particle size) , calcium carbonate (<12 micron particle size) , terpene resin, and powder color at a ratio of 11:18:17:1 was fed at a rate of 1.435 lb/min. in the first feed inlet. In the εecond feed inlet, a powder blend of polyvinyl acetate, glycerol monoεtearate, and hydrogenated εoybean and vegetable oil at a ratio of 24:5:12 was fed at a rate of 1.264 lb/min. In the third feed port, 6 parts of polyisobutylene at 95°C at a feed rate of 0.181 lb/min. and 6 parts of a 50/50 mixture of hydrogenated cottonseed oil/lecithin at 80°C at a feed rate of 0.203 lb/min. were added.
Overall, the production rate for the gum base waε about 185 pounds per hour. The gum base waε manufactured using the following process conditions:
First 5-Inch Second 5-Inch Mixer Mixer RPM 250 400
Initial Barrel Temp. , °C 135 115 Product Exit Temp. , °C 190 115 Average Residence Time 20 min. 10 min.
About 200 pounds of gum base product was made.
The gum base had normal color, no lumps, no unincorporate oil, but had a burnt off taste and odor. Example 10
Thiε example waε performed uεing a two-mixer arrangement with two 5-inch Teledyne Readco Continuous Mixer Compounderε. Both compounders were configured with the same paddle configuration that waε shown in Table 1. Four feed ports were arranged as follows:
Feed Port No. 1 - above longitudinal positions 1 -
4 on first 5-inch mixer
Feed Port No. 2 - above longitudinal positions
20 - 23 on first 5-inch mixer
Feed Port No. 3 - above longitudinal positions 1 - 4 on second 5-inch mixer
Feed Port No. 4 - above longitudinal poεitionε 20-
23 on second 5-inch mixer.
Using the above mixer arrangement, chewing gum baεe waε made as follows:
A mixture of ground isobutylene-iεoprene copolymer (2-7 mm particle εize) , calcium carbonate (<12 micron particle size) , and polyvinyl acetate at a ratio of 13:10:7 was fed at a rate of 0.75 lb/min. in the first feed inlet. In the second feed inlet, 15 parts of polyvinyl acetate was added at 0.375 lb/min. In the third feed port, hydrogenated vegetable oil, hydrogenated soybean oil, and glycerol monostearate at a ratio of 13:13:3 were added at a rate of 0.725 lb/min. In the fourth feed port, 10 parts of partially hydrogenated vegetable oil at 0.25 lb/min., and 16 parts of polyisobutylene at 130°C at a rate of 0.40 lb/min. were added.
Overall, the production rate for the gum base was 150 pounds per hour. The gum base was manufactured using the following procesε conditions: Firεt 5-Inch Second 5-Inch
Mixer Mixer
RPM 373 374
Initial Barrel Temp. , °C 150-180 110 Product Exit Temp, , °C 165-191 111 Average Reεidence Time 20-30 min. 12-15 min.
About 400 pounds of gum base product was made. The gum base had normal color, no lumpε, no unincorporated oil, and clean taεte and odor.
Example 11
This example was made uεing the εame equipment, mixer arrangement, εcrew configuration, and feed portε as Example 10, except feed port No. 2 was closed off. The gum base was made as follows:
A mixture of ground isobutylene-iεoprene copolymer (2-7 mm particle εize) , calcium carbonate (<12 micron particle εize) , terpene resin, and polyvinyl acetate at a ratio of 11:18:17:6 was fed at a rate of 1.30 lb/min. in the first feed inlet. In the third feed inlet, a powder blend of polyvinyl acetate, glycerol monostearate, hydrogenated soybean oil and vegetable oil, and powdered color at a ratio of 18:5:12:1 was fed at a rate of 0.90 lb/min. In the fourth feed inlet, 6 parts of polyisobutylene at 130°C was added at a rate of 0.15 lb/min., and 6 parts at a 50/50 blend of lecithin and hydrogenated cottonseed oil at 90°C was added at a rate of 0.15 lb/min.
Overall, the production rate for the gum base waε 150 pounds per hour. The gum base waε manufactured using the following process conditions. First 5-Inch Second 5-Inch
Mixer Mixer
RPM 300 373
Initial Barrel Temp., °C 150-180 110 Product Exit Temp., °C 172 113 Average Residence Time 20-30 min. 12-15 min.
About 400 pounds of gum base product was made. The gum base had normal color, no lumps, no unincorporated oil, and clean taεte and odor.
Gum baεes of Examples 10 and 11 were analyzed by Gel Permeation chromatography (GPC) and compared to the same formulation of base made by conventional batch processeε. Analyεeε εhowed that the iεobutylene-isoprene copolymer of Examples 10 and 11 was over-sheared and degraded. Sugar gum formulations were made to compare sensory attributeε of baεes from Examples 10 and 11 to base made by the conventional batch procesε. Tests showed that bases of Examples 10 and 11 gave a much softer texture than the baseε from conventional batch proceεs.
Example 12
This example was performed using a two-mixer arrangement with two 5-inch Teledyne Readco Continuous Mixer Compounderε. Both compounders were configured according to the following Table 5. The feed ports were the same as Example 11.
Table 5: Mixer Configuration .Per Shaft)
Longitudin Rotational Longitudina Rotational al Position Element Position I Position Element Position
1 FC 4 19 FP 3
2 FC 4 20 FC 3
3 FC 4 21 FC 3
4 FC 4 22 FC 3
5 FC 4 23 FC 3
6 FC 4 24 FC 3
7 FC 4 25 FC 3
8 FC 4 26 FC 3
9 FP 4 27 FC 3
10 FP 4 28 FP 2
11 FP 4 29 FP 2
12 FP 2 30 FP 4
13 FP 2 31 FP 4
14 FP 2 32 FP 4
15 FP 4 33 FP 2
16 FP 4 34 FP 2
17 FP 1 35 FP 4
18 FP 2 36 RH 4
Using the above mixer arrangement, chewing gum base was made as follows.
A mixture of ground isobutylene-isoprene copolymer (2-7 mm particle size) , and calcium carbonate, terpene resins, and polyvinyl acetate at a ratio of 11:18:17:1 was added at a rate of 1.175 lb/min. to feed inlet No. 1. To feed inlet No. 3 a powder blend of polyvinyl acetate, glycerol monostearate, hydrogenated soybean and vegetable oils, and powdered color at a ratio of 23:5:12:1 was fed at a rate of 1.025 lb/min. To feed inlet No. 4, 6 parts of polyisobutylene at 130°C was added at a rate of 0.15 lb/min., and 6 parts of a 50/50 blend of lecithin and hydrogenated cottonseed oil at 90°C was added at a rate of 0.15 lb/min. Overall, the production rate for the gum base waε 150 poundε per hour. The gum baεe waε manufactured uεing the following proceεε conditions:
First 5-] [nch Second 5-Inch
Mixer Mixer
RPM 250 376
Initial Barrel Temp. , °C 150-180 110
Product Exit Temp. , °C 175 120
Average Residence Time 20-30 min. 12-15 min.
About 350 pounds of gum base was made. The gum base had normal color, no lumpε, no unincorporated oil, and clean taste and odor. Analysiε of the gum baεe by GPC indicated it is very similar to the same base formula made by a conventional batch procesε. Also, gum made from base of this example had sensory properties virtually the same as gum made with base made by conventional batch procesε.
Examples 13-21 - Continuous Chewing Gum Manufacture
In Examples 13-21, the chewing gum base is made in a blade-and-pin mixer, which is then also uεed to complete the making of the chewing gum composition. In order to accomplish the total chewing gum manufacture using the preferred blade-and-pin mixer 200 (Fig. 17) , it is advantageous to maintain the rpm of the mixing screw 120 at less than about 150, preferably less than about 100. Also, the mixer temperature iε preferably optimized so that the gum base is at about 130°F or lower when it initially meets the other chewing gum ingredientε, and the chewing gum product iε at about 130°F or lower (preferably 125°F or lower) when it exits the mixer. This temperature optimization can be accomplished, in part, by selectively heating and/or water cooling the barrel sections surrounding the mixing zones 220, 230, 240, 250 and 260 (Fig. 23). In order to manufacture the gum base, the following preferred procedure can be followed. The elastomer, filler, and at least some of the elastomer solvent are added to the firεt large feed port 212 in the feed zone 210 of the mixer 200, and are εubjected to highly diεperεive mixing in the firεt mixing zone 220 while being conveyed in the direction of the arrow 122. The remaining elastomer solvent (if any) and polyvinyl acetate are added to the second large feed port 232 in the second mixing zone 230, and the ingredients are subjected to a more distributive mixing in the remainder of the mixing zone 230.
Fats, oils, waxes (if used) , emulsifiers and, optionally, colors and antioxidants, are added to the liquid injection ports 241 and 243 in the third mixing zone 240, and the ingredientε are εubjected to distributive mixing in the mixing zone 240 while being conveyed in the direction of the arrow 122. At this point, the gum base manufacture εhould be complete, and the gum baεe εhould leave the third mixing zone 240 as a substantially homogeneous, lump-free compound with a uniform color.
The fourth mixing zone 250 is used primarily to cool the gum base, although minor ingredient addition may be accomplished. Then, to manufacture the final chewing gum product, glycerin, corn syrup, other bulk sugar sweeteners, high intensity sweetenerε, and flavors can be added to the fifth mixing zone 260, and the ingredients are subjected to diεtributive mixing. If the gum product is to be sugarless, hydrogenated starch hydrolyzate or sorbitol solution can be substituted for the corn syrup and powdered alditolε can be εubεtituted for the εugarε.
Preferably, glycerin iε added to the firεt liquid injection port 261 in the fifth mixing zone 260. Solid ingredients (bulk sweetenerε, encapεulated high intensity sweeteners, etc.) are added to the large feed port 262. Syrups (corn syrup, hydrogenated starch hydrolyzate, sorbitol solution, etc.) are added to the next liquid injection port 263, and flavors are added to the final liquid injection port 264. Flavors can alternatively be added at ports 261 and 263 in order to help plasticize the gum base, thereby reducing the temperature and torque on the screw. This may permit running of the mixer at higher rpm and throughput. The gum ingredients are compounded to a homogeneous mass which is discharged from the mixer as a continuouε stream or "rope". The continuous stream or rope can be deposited onto a moving conveyor and carried to a forming station, where the gum iε εhaped into the desired form such as by preεεing it into εheetε, εcoring, and cutting into εtickε. Because the entire gum manufacturing proceεs is integrated into a single continuous mixer, there is less variation in the product, and the product is cleaner and more stable due to its εimplified mechanical and thermal hiεtorieε.
The following Examples 13-22 were run uεing a Buss kneader with a 100mm mixer screw diameter, configured in the preferred manner described above (unless indicated otherwise) , with five mixing zones, a total mixing L/D of 19, and an initial conveying L/D of 1-1/3. No die was used at the end of the mixer, unless indicated otherwise, and the product mixture exited as a continuouε rope. Each example waε deεigned with feed rateε to yield chewing gum product at the rate of 300 poundε per hour.
Liquid ingredients were fed using volumetric pumps into the large feed ports and/or smaller liquid injection ports generally positioned as described above, unlesε otherwiεe indicated. The pumpε were appropriately εized and adjuεted to achieve the deεired feed rateε. Dry ingredientε were added uεing gravimetric εcrew feeders into the large addition ports positioned aε deεcribed above. Again, the feeders were appropriately sized and adjuεted to achieve the deεired feed rateε. Temperature control waε accomplished by circulating fluids through jackets surrounding each mixing barrel zone and inside the mixing screw. Water cooling was used where temperatures did not exceed 200°F, and oil cooling waε used at higher temperatures. Where water cooling waε desired, tap water (typically at about 57°F) was used without additional chilling.
Temperatures were recorded for both the fluid and the ingredient mixture. Fluid temperatures were set for each barrel mixing zone (corresponding to zones 220, 230, 240, 250 and 260 in Figs. 23 and 24) , and are reported below as Zl, Z2, Z3, Z4 and Z5, respectively. Fluid temperatures were alεo εet for the mixing εcrew 120, and are reported below aε SI. Actual mixture temperatureε were recorded near the downstream end of mixing zones 220, 230, 240 and 250; near the middle of mixing zone 260; and near the end of mixing zone 260. Theεe mixture temperatureε are reported below aε TI, T2, T3, T4, T5 and T6, reεpectively. Actual mixture temperatures are influenced by the temperatures of the circulating fluid, the heat exchange properties of the mixture and εurrounding barrel, and the mechanical heating from the mixing proceεε, and often differ from the set temperatures due to the additional factors. All ingredients were added to the continuous mixer at ambient temperature (about 77°F) unleεε otherwise noted.
Example 13 This example illustrates the preparation of a spearmint flavored non-tack εugar chewing gum. A mixture of 24.2% terpene reεin, 29.7% dusted ground butyl rubber (75% rubber with 25% fine ground calcium carbonate as an anti-blocking aid) and 46.1% fine ground calcium carbonate was fed at 25 lb/hr into the first large feed port (port 212 in Figs. 23 and 24) . Low molecular weight polyisobutylene (mol. wt. = 12,000) , preheated to 100°C, was alεo added at 6.3 lb/hr into thiε port.
Ground low molecular weight polyvinyl acetate was added at 13.3 lb/hr into the second large feed port (por 232 in Figs. 23 and 24) .
A fat mixture, preheated to 83°C, was injected into the liquid injection portε in the third mixing zone (portε 241 and 243 in Fig. 23) , at a total rate of 18.4 lb/hr, with 50% of the mixture being fed through each port. The fat mixture included 30.4% hydrogenated εoybean oil, 35.4% hydrogenated cottonεeed oil, 13.6% partially hydrogenated εoybean oil, 18.6% glycerol monoεtearate, 1.7% cocoa powder, and 0.2% BHT.
Glycerin was injected into the first liquid injection port in the fifth mixing zone (port 261 in Fig. 23) at 3.9 lb/hr. A mixture of 1.1% sorbitol and 98.9% sugar was added into the large feed port in the fifth mixing zone (port 262 in Fig. 23) at 185.7 lb/hr. Corn syrup, preheated to 44°C, was added into the second liquid injection port in the fifth mixing zone (port 263 in Fig. 23) at 44.4 lb/hr. Spearmint flavor was added into the third liquid injection port in the fifth mixing zone (port 264 in Fig. 23) at 3.0 lb/hr.
The zone temperatures Z1-Z5 were set (in °F) at 350, 350, 150, 57 and 57, reεpectively. The mixing εcrew temperature SI was set at 120°F. The mixture temperatures T1-T6 were meaεured at εteady εtate (in °F) aε 235, 209, 177, 101 and 100, and fluctuated εlightly during the trial. The screw rotation was 80 rpm. The chewing gum product exited the mixer at
120°F. The product was comparable to that produced by conventional pilot scale batch procesεing. The chew waε εlightly rubbery but no baεe lumps were visible.
Example 14
This example illustrateε the preparation of a peppermint flavored non-tack sugar chewing gum. A dry mixture of 57% dusted ground butyl rubber (75% rubber, 25% calcium carbonate) and 43% fine ground calcium carbonate waε added at the firεt large feed port 212 (Fig. 23), at 13.9 lb/hr. Molten polyiεobutylene (preheated to 100°C) waε also added to port 212 at 9.5 lb/hr.
Ground low molecular weight polyvinyl acetate was added to port 232 at 13.0 lb/hr.
A fat mixture (preheated to 82°C) was pumped 50/50 into portε 241 and 243 at a total rate of 23.6 lb/hr. The fat mixture included 33.6% hydrogenated cottonseed oil, 33.6% hydrogenated soybean oil, 24.9% partially hydrogenated εoybean oil, 6.6% glycerol monostearate, 1.3% cocoa powder and 0.1% BHT. Glycerin was added to port 261 at 2.1 lb/hr. A mixture of 98.6% sugar and 1.4% sorbitol was added to port 262 at 196 lb/hr. Corn syrup (preheated to 40°C) was added to port 263 at 39.9 lb/hr. Peppermint flavor waε added to port 264 at 2.1 lb/hr. The zone temperatures (Z1-Z5, °F) were set at
350, 350, 300, 60 and 60, reεpectively. The εcrew temperature (SI) was set at 200°F. The mixture temperatures (T1-T6, °F) were measured as 297, 228, 258, 122, 98 and 106, respectively. The screw rotation was 85 rpm.
The chewing gum product exited the mixer at 119°F. The finished product was free of lumps but was dry and lacked tensile strength. These defects were attributed to the formula rather than the proceεεing.
Example 15
Thiε example illuεtrates the preparation of a εpearmint flavored gum for pellet coating. A blend of 27.4% high molecular weight terpene resin, 26.9% low molecular weight terpene resin, 28.6% dusted ground butyl rubber (75% rubber, 25% calcium carbonate) and 17.1% fine ground calcium carbonate was fed into the first large port 212 (Fig. 23), at 33.5 lb/hr. Molten polyisobutylene (100°C) was pumped into the same port at 1.3 lb/hr.
Low molecular weight polyvinyl acetate was fed to port 232 at 19.8 lb/hr.
A fat mixture (82°C) was added 50/50 into ports 241 and 243, at a total rate of 17.4 lb/hr. The fat mixture included 22.6% hydrogenated cottonseed oil, 21.0% partially hydrogenated soybean oil, 21.0% hydrogenated soybean oil, 19.9% glycerol monoεtearate, 15.4% lecithin and 0.2% BHT.
Sugar was fed into port 262 at 157.8 lb/hr. Corn syrup (40°C) was added to port 263 at 68.4 lb/hr. Spearmint flavor was added to port 264 at 1.8 lb/hr. The zone temperatures (Z1-Z5, °F) were set at
160, 160, 110, 60 and 60, respectively. The screw temperature (SI) was set at 68°F. The mixture temperatureε (T1-T6, °F) were meaεured aε 230, 215, 166, 105, 109 and 111, respectively. The screw rotation was 80 rpm.
The chewing gum product exited the mixer at 121°F. The product was firm and cohesive when chewed (normal for a pellet center) . No base lumps were visible.
Example 16
This example illuεtrateε the preparation of a peppermint flavored sugar chewing gum. A blend of 24.4% dusted ground butyl rubber (75% rubber, 25% calcium carbonate), 18.0% low molecular weight terpene resin,
18.3% high molecular weight terpene reεin and 39.4% fine ground calcium carbonate was added to the first large port 212 (Fig. 23) at 27.6 lb/hr.
A blend of 11.1% high molecular weight polyvinyl acetate and 88.9% low molecular weight polyvinyl acetate was added into the second large feed port 232 at 14.4 lb/hr. Polyiεobutylene (preheated to 100°C) waε alεo added to thiε port at 3.5 lb/hr.
A fat mixture (83°C) waε added 50/50 into portε 241 and 243, at a total rate of 14.5 lb/hr. This fat mixture included 31.9% hydrogenated cottonseed oil, 18.7% hydrogenated soybean oil, 13.2% partially hydrogenated cottonseed oil, 19.8% glycerol monostearate, 13.7% soy lecithin, 2.5% cocoa powder and 0.2% BHT.
Glycerin waε injected into port 261 at 3.9 lb/hr. A mixture of 84.6% sucrose and 15.4% dextrose monohydrate was added to port 262 at 203.1 lb/hr. Corn syrup (40°C) was injected into port 263 at 30.0 lb/hr. A mixture of 90% peppermint flavor and 10% soy lecithin was injected into port 264 at 3.0 lb/hr. The zone temperatures (Z1-Z5, °F) were set at
350, 350, 100, 60 and 60, respectively, and the εcrew temperature (SI) was εet at 100°F. The mixture temperatureε (T1-T6, °F) were measured as 308, 261, 154, 95, 94 and 105, respectively. The screw rotation was set at 55 rpm.
The product exited the mixer at 127°F. The finished product had good chew characteriεticε and there waε no evidence of rubber lumpε.
Example 17
This example illustrateε the preparation of a fruit-flavored sugar gum. A mixture of 39.3% duεted ground butyl rubber (75% rubber, 25% calcium carbonate) , 39.1% low molecular weight terpene reεin and 21.6% fine ground calcium carbonate was added to the first large feed port 212 (Fig. 23) at 20.6 lb/hr.
A mixture of 33.0% low molecular weight terpene reεin and 67.0% low molecular weight polyvinyl acetate waε added at 24.4 lb/hr into the εecond large feed port 232. Polyisobutylene (preheated to 100°C) was also added at 1.0 lb/hr into the port 232. A fat/wax composition (82°C) was injected 50/50 into the liquid injection ports 241 and 243, at a total rate of 14.0 lb/hr. The composition included 29.7% paraffin wax, 21.7% microcrystalline wax (m.p. = 170°F) , 5.7% microcrystalline wax (m.p. = 180°F) , 20.5% glycerol monostearate, 8.6% hydrogenated cottonseed oil, 11.4% soy lecithin, 2.1% cocoa powder, and 0.3% BHT.
Glycerin was injected into the liquid injection port 261 at 3.3 lb/hr. A mixture of 88.5% sucrose and 11.5% dextrose monohydrate was added at 201.0 lb/hr into the large port 262. Corn syrup (40°C) waε injected at 3.0 lb/hr into the liquid injection port 263, and a mixture of 88.9% fruit flavor and 11.1% soy lecithin was injected at 2.7 lb/hr into the liquid injection port 264. The zone temperatureε (Z1-Z5, °F) were set at
425, 425, 200, 61 and 61, respectively. The screw temperature (SI) was set at 66°F. The mixture temperatureε (T1-T6, °F) were meaεured as 359, 278, 185, 105, 100 and 109, respectively. The screw rotation was εet at 70 rpm.
The chewing gum product exited the mixer at 122°F. The product waε very εoft while warm and fell apart during chewing. However, this was not atypical for this product. After aging for two months, the product was again chewed and found to have excellent texture and flavor. No rubber lumps were viεible.
Example 18
Thiε example illustrates the preparation of a spearmint flavored sugarless gum. A mixture of 42.1% fine ground calcium carbonate, 18.9% glycerol ester of wood rosin, 16.7% glycerol ester of partially hydrogenated wood rosin, 17.0% ground butyl rubber, and 5.3% dusted ground (25:75) styrene butadiene rubber (75% rubber, 25% calcium carbonate) was added into port 212 (Fig. 23) at 38.4 lb/hr. Low molecular weight polyvinyl acetate at 12.7 lb/hr, and polyiεobutylene (preheated to 100°C) at 7.6 lb/hr, were added into port 232.
A fat mixture (82°C) waε injected 50/50 into ports 241 and 243, at a total rate of 20.9 lb/hr. The fat mixture included 35.7% hydrogenated cottonseed oil, 30.7% hydrogenated soybean oil, 20.6% partially hydrogenated soybean oil, 12.8% glycerol monostearate and 0.2% BHT. Unlike the previous examples, glycerin was injected at 25.5 lb/hr into the fourth mixing zone 250 (Fig. 23) through a liquid injection port (not shown) . A coevaporated blend of hydrogenated starch hydrolysate and glycerin (at 40°C) was injected further downstream in the fourth mixing zone 250 through another liquid injection port (not shown). The coevaporated blend included 67.5% hydrogenated starch hydrolysate εolidε, 25% glycerin and 7.5% water.
A mixture of 84.8% sorbitol, 14.8% mannitol and 0.4% encapsulated aspartame waε added into port 262 in the fifth mixing zone 260, at 162.3 lb/hr. A mixture of 94.1% spearmint flavor and 5.9% lecithin was injected at 5.1 lb/hr into the port 264 located further downstream. The zone temperatures (Z1-Z5, °F) were set at 400, 400, 150, 62 and 62, respectively. The screw temperature (SI) was set at 66°F. The mixture temperatures (T1-T6, °F) were measured aε 307, 271, 202, 118, 103 and 116. The mixing εcrew rotation waε 69 rpm. The chewing gum product exited the mixer at 117°F. The gum had good appearance with no sorbitol spotε or rubber lumpε. The gum was slightly wet to the touch, sticky and fluffy (low denεity) , but was acceptable. During chewing, the gum was conεidered soft initially but firmed up with continued chewing. Example 19
This example illustrates the preparation of a sugarlesε spearmint gum for use in coated pellets. A mixture of 28.6% dusted ground butyl rubber (75% rubber, 25% calcium carbonate), 27.4% high molecular weight terpene reεin, 26.9% low molecular weight terpene resin and 17.1% calcium carbonate was added into port 212 (Fig. 23) at 41.9 lb/hr.
Low molecular weight polyvinyl acetate at 24.7 lb/hr, and polyisobutylene (preheated to 100°C) at 1.7 lb/hr, were added into port 232.
A fat composition (82°C ) was injected 50/50 into ports 241 and 243 at a total rate of 21.7 lb/hr. The fat composition included 22.6% hydrogenated cottonεeed oil, 21.0% hydrogenated εoybean oil, 21.0% partially hydrogenated soybean oil, 19.9% glycerol monostearate, 15.4% glycerin and 0.2% BHT.
A 70% sorbitol εolution waε injected into the fourth mixing zone 250 (Fig. 23) at 17.4 lb/hr, using a hollow barrel pin liquid injection port (not shown) .
A mixture of 65.8% sorbitol, 17.9% precipitated calcium carbonate and 16.3% mannitol waε added at 184.2 lb/hr into the final large port 262. A mixture of 71.4% εpearmint flavor and 28.6% εoy lecithin waε added at 8.4 lb/hr into the final liquid injection port 264.
The zone temperatureε (Z1-Z5, °F) were set at 400, 400, 150, 61 and 61, respectively. The screw temperature (SI) was εet at 65°F. The mixture temperatureε (T1-T6, °F) were meaεured as 315, 280, 183, 104, 109 and 116, respectively. The screw rotation was set at 61 rpm.
The chewing gum exited the mixer at 127°F. The product appearance waε good with no εorbitol spotε or rubber lumpε. However, the initial chew waε reported aε being rough and grainy. Example 20
Thiε example illustrates the preparation of a peppermint flavored sugar chewing gum. A mixture of 27.4% duεted ground butyl rubber (75% butyl rubber dusted with 25% calcium carbonate), 14.1% lower softening terpene resin (softening point = 85°C) , 14.4% higher softening terpene resin (softening point = 125°C) and 44.1% calcium carbonate was fed at 24.6 lb/hr into the first large feed port (port 212 in Figs. 23 and 24) . A mixture of 73.5% low molecular weight polyvinyl acetate, 9.2% high molecular weight polyvinyl acetate, 8.6 lower softening terpene resin and 8.7% higher softening terpene resin was fed at 17.4 lb/hr into the second large feed port 232. Polyisobutylene was also added at 3.5 lb/hr into this port.
A fat mixture, preheated to 83°C, was injected into the liquid injection ports in the third mixing zone (ports 241 and 243 in Fig. 23), at a total rate of 14.5 lb/hr, with 50% of the mixture being fed through each port. The fat mixture included 0.2% BHT, 2.5% cocoa powder, 31.9% hydrogenated cottonεeed oil, 19.8% glycerol monoεtearate, 18.7% hydrogenated soybean oil, 13.7% lecithin, and 13.2% partially hydrogenated cottonseed oil. A mixture of 84.6% sugar and 15.4% dextrose monohydrate was injected at 203.1 lb/hr into the large feed port 262 in the fifth mixing zone. Glycerin waε added at 3.9 lb/hr into the firεt liquid injection port 261 in the fifth mixing zone. Corn εyrup, preheated to 44°C, was added at 30.0 lb/hr into the second liquid injection port 263 in the fifth mixing zone. A mixture of 90.0% peppermint flavor and 10.0% lecithin waε injected into the third liquid injection port 264 in the fifth mixing zone at 3.0 lb/hr. The zone temperatureε Z1-Z5 were set (in °F) at
350, 350, 110, 25 and 25, respectively. The mixing screw temperature SI was set at 101°F. The mixer temperatures T1-T6 were measured at steady state (in °F) aε 320, 280,
164, 122, 105 and 103, respectively. The screw rotation was 63 rpm, and the product exited the mixer at 52-53°C.
The peppermint sugar gum product waε deεirably soft, and acceptable in quality.
Example 21
This example illuεtrateε the preparation of a sugarless stick bubble gum. For this example, the εcrew configuration shown in Fig. 24, and uεed for the previous examples, was varied as follows. The conveying section 210 and mixing sections 220, 250 and 260 were configured substantially as before. In the second mixing zone 230, the three low shear elements 80 (Fig. 20) were also not changed.
Thereafter, the 1-1/2 high εhear elementε 78 (Fig. 21) in zone 230, the reεtriction element 70 overlapping zoneε 230 and 240, all of zone 240, and the restriction element 70 overlapping zones 240 and 250 were removed. Three high shear elements 78 (combined L/D =
2.0) were placed in zone 230 and extended into zone 240. Two and one-half low shear elements 80 (combined L/D = 1- 2/3) followed in zone 240. Then, three and one-half high shear elements 78 (combined L/D = 2-1/3) followed in zone 240 and extended into zone 250. The eleven low-shear elements 80 in zones 250 and 260 were not changed.
To make the product, a mixture of 53.3% high molecular weight polyvinyl acetate, 31.0% talc, 12.2% glycerol ester of wood rosin and 3.5% duεted ground (25:75) εtyrene-butadiene rubber (75% rubber, 25% calcium carbonate) were fed into the large port 212 (Fig. 23) at 54.9 lb/hr. Polyisobutylene (preheated to 100°C) was pumped into the εame port at 9.0 lb/hr.
Glycerol ester of partially hydrogenated wood rosin at 15.3 lb/hr, and triacetin at 4.4 lb/hr, were added into the large port 232 in the second mixing zone 230. A fat/wax mixture (at 82°C) was fed 50/50 into the liquid injection ports 241 and 243 in the third mixing zone 240, at a total rate of 13.9 lb/hr. The mixture included 50.3% glycerol monostearate, 49.4% paraffin (m.p. = 135°F) and 0.3% BHT.
Diluted glycerin was injected into the fourth mixing zone 250 at 28.2 lb/hr using a liquid injection port (not shown) . The dilution was 87% glycerin and 13% water. A mixture of 84.0% sorbitol, 12.7% mannitol,
1.1% fumaric acid, 0.2% aspartame, 0.4% encapsulated aεpartame, 0.7% adipic acid and 0.9% citric acid was fed into port 262 in the fifth mixing zone 260 at 165.0 lb/hr. A mixture of 51.6% bubble gum flavor and 48.4% soy lecithin was injected into port 264 in zone 260 at 9.3 lb/hr.
The zone temperatures (Z1-Z5, °F) were set at 350, 350, 100, 64 and 64, reεpectively. The screw temperature (SI) was set at 100°F. The mixture temperatures (T1-T6, °F) were recorded as 286, 260, 163, 107, 104 and 112, respectively. The screw rotation was 75 rpm.
The chewing gum exited the mixer at 118°F. The finished product looked good and contained no base lumps. The flavor and texture were very good during chewing, as were the bubble blowing characteriεtics.
Examples 22-36
Examples 22-36 also disclose the use of a blade-and-pin mixer to make a complete chewing gum.
These examples, like some of the previous examples, have a specific lubricating agent, such aε terpen resin and/or polyvinyl acetate, added at two different feed inlets. Example 22 70/30% Split of Terpene Resin and 12/88% Split of PVAC. This example illustrates the preparation of a gum base to be used for a peppermint flavored sugar gum. A blend of 25.545% ground isobutylene-isoprene copolymer, 13.183% low molecular weight terpene resin, 13.343% high molecular weight terpene resin, 0.731% high molecular weight polyvinyl acetate, 5.844% low molecular weight polyvinyl acetate, and 41.354% fine ground calcium carbonate was added to the firεt large feed port 212 at 26.88 lb/hr.
A blend of 70.270% low molecular weight polyvinyl acetate, 8.786% high molecular weight polyvinyl acetate, 9.273% low molecular weight terpene reεin, 9.423% low molecular weight terpene reεin, 9.423% high molecular weight terpene resin, and 2.24 color was added into the εecond large feed port 232 at 16.01 lb/hr. Polyiεobutylene was also added into the second large feed port at 3.51 lb/hr. A fat mixture (225°F.) was injected into zone
240 at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonεeed oil, 22% hydrogenated εoybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
Glycerin was injected into zone 260 at 3.5 lb/hr. A mixture of 85% sucrose and 15% dextrose monohydrate was added to the large feed port 262 at 103.1 lb/hr. Corn syrup (100°F.) was injected into zone 260 at 30.0 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
The zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55, and 55 respectively, and the screw temperature (SI) was set at 100°F. The mixture temperatureε (T1-T6, °F.) were measured as 319, 291, 170, 118, 112 and 89, reεpectively. The εcrew rotation waε set at 60 rpm. The product exited the mixer at 121°F. The finished product had good chew characteristic and there waε no evidence of rubber lumpε.
Example 23
70/30% Split of Terpene Resin and 6/94% Split of PVAC This example illustrates the preparation of a gum base to be used for a peppermint flavored sugar gum. A blend of 26.413% ground isobutylene-isoprene copolymer, 13.632% low molecular weight terpene resin, 13.797% high molecular weight terpene resin, 0.378% high molecular weight polyvinyl acetate, 3.021% low molecular weight polyvinyl acetate, and 42.759% fine ground calcium carbonate was added to the first large feed port 212 at 25.41 lb/hr.
A blend of 71.223% low molecular weight polyvinyl acetate, 8.905% high molecular weight polyvinyl acetate, 8.798% low molecular weight terpene resin, 8.941 high molecular weight terpene resin, and 2.133 color waε added into the second large feed port 232 at 16.88 lb/hr. Polyisobutylene was also added into the εecond large feed port at 3.51 lb/hr.
A fat mixture (225°F.) waε injected into zone 240 at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated εoybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
Glycerin was injected into zone 260 at 3.5 lb/hr. A mixture of 85% sucroεe and 15% dextroεe monohydrate waε added to the large feed port 262 at 203.1 lb/hr. Corn syrup (100°F.) was injected into zone 260 at 30.50 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr. The zone temperatures (Z1-Z5, °F.) were εet at
350, 350, 100, 55 and 55 reεpectively, and the screw temperature (SI) was set at 100°F. The mixture temperatureε (T1-T6, °F.) were measured as 316, 289, 154, 116, 110 and 90, reεpectively. The εcrew rotation waε set at 60 rpm.
The product exited the mixer at 121°F. The finished product had good chew characteriεtic and there was no evidence of rubber lumpε.
Example 24
70/30% Split of Terpene Resin and 3/97% Split of PVAC The example illustrates the preparation of a gum base to be used for a peppermint flavored sugar gum. A blend of 26.870% ground isobutylene-iεoprene copolymer, 13.867% low molecular weight terpene reεin, 14.035% high molecular weight terpene reεin, 0.192% high molecular weight polyvinyl acetate, 1.537% low molecular weight polyvinyl acetate, and 43.499% fine ground calcium carbonate was added to the first large feed port 212 at 24.99 lb/hr.
A blend of 71.664% low molecular weight polyvinyl acetate, 8.960% high molecular weight polyvinyl acetate, 8.579% low molecular weight terpene resin, 8.718% high molecular weight terpene reεin, and 2.08% color was added into the second large feed port 232 at 17.31 lb/hr. Polyisobutylene was also added into the second large feed port at 3.51 lb/hr.
A fat mixture (225°F.) was injected into zone 240 at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonεeed oil, 22% hydrogenated soybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
Glycerin was injected into zone 260 at 3.5 lb/hr. A mixture of 85% sucrose and 15% dextrose monohydrate was added to the large feed port 262 at 203.1 lb/hr. Corn syrup (100°F.) was injected into zone 260 at 30.0 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr. The zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F. The mixture temperatures (T1-T6, °F.) were measured as 322, 291, 155, 116, 109 and 89, respectively. The screw rotation was set at 60 rpm.
The produce exited the mixer at 121°F. The finished product had good chew characteristicε and there was no evidence of rubber lumps.
Example 25
70/30% Split of Terpene Resin and 25/75% Split of PVAC This example illustrates the preparation of a gum base to be used for a peppermint flavored sugar gum. A blend of 23.864% ground isobutylene-isoprene copolymer, 12.316% low molecular weight terpene resin, 12.465% high molecular weight terpene resin, 1.418% high molecular weight polyvinyl acetate, 11.303% low molecular weight polyvinyl acetate, and 38.633% fine ground calcium carbonate was added to the firεt large feed port 212 at 28.13 lb/hr.
A blend of 67.688% low molecular weight polyvinyl acetate, 8.514% high molecular weight polyvinyl acetate, 10.536% low molecular weight terpene reεin, 10.707% high molecular weight terpene resin, and 2.559% color was added into the second large feed port 232 at 14.13 lb/hr. Polyisobutylene was also added into the second large feed port 232 at 3.51 lb/hr.
A fat mixture (225°F.) was injected in to zone 240, at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated soybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT. Glycerin was injected into zone 260 at 3.9 lb/hr. A mixture of 85% sucrose and 15% dextrose monohydrate was added to the large feed port 262 at 203.1 lb/hr. Corn syrup (100°F.) was injected into zone 260 at 30.0 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
The zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F. The mixture temperatures (T1-T6, °F.) were measured as 311, 289, 158, 114, 109, and 89 respectively. The screw rotating waε εet at 60 rpm. The product exited the mixer at 121°F. The finiεhed product had good chew characteristic and there was no evidence of rubber lumps.
Example 26 25/75% Split of PVAC
This example illustrates the preparation of a gum base to be used for a non-tack peppermint flavored εugar gum. A blend of 46.302% ground iεobutylene- iεoprene copolymer, 18.980% low molecular weight polyvinyl acetate and 34.718% fine ground calcium carbonate was added to the first large feed port 212 at
17.12 lb/hr.
A blend of 97.015% low molecular weight polyvinyl acetate, and 2.9% color was added into the second large feed port 232 at 10.05 lb/hr.
Polyisobutylene was also added into the second large feed port at 3.5 lb/hr.
A fat mixture (225°F.) was injected into zone
240 at a total rate of 23.33 lb/hr. This fat mixture included 34% hydrogenated cottonεeed oil, 34% hydrogenated εoybean oil, 25% partially hydrogenated εoybean oil, 6.8% glycerol monoεtearate and 0.10% BHT. Glycerin was injected into zone 260 at 2.1 lb/hr. A mixture of 98.62% εucroεe and 1.38% sorbitol was added into the large feed port 262 at 194.7 lb/hr.
Corn syrup (100°F.) was injected into zone 260 at 39.9 lb/hr. Peppermint flavor was injected into zone 260 at 2.1 lb/hr.
The zone temperatureε (Z1-Z5, °F.) were set at 350, 350, 300, 55, and 55, respectively, and the screw temperature (SI) was set at 150°F. The mixture temperatures (T1-T6, °F.) were measured as 326, 304, 264, 129, 101 and 85, respectively. The screw rotation was set at 69 rpm.
The product exited the mixer at 121°F. The finiεhed product had good chew characteristic and there was no evidence of rubber lumps.
Example 27
3/97% Split of PVAC This example illuεtrateε the preparation of a gum baεe to be used for a non-tack peppermint flavored sugar gum. A blend of 55.586% ground isobutylene- isoprene copolymer, 2.735% low molecular weight polyvinyl acetate and 41.679% fine ground calcium carbonate was added to the first large feed port 212 at 14.26 lb/hr.
A blend of 97.674% low molecular weight polyvinyl acetate and 2.325% color was added into the second large feed port 232 at 12.9 lb/hr. Polyisobutylene waε alεo added to the εecond large feed port at 3.5 lb/hr.
A fat mixture (225°F) waε injected into zone 240 at a total rate of 23.33 lb/hr. Thiε fat mixture included 34% hydrogenated cottonseed oil, 34% hydrogenated soybean oil, 25.1% partially hydrogenated cottonseed oil, 6.8% glycerol monostearate and 0.10% BHT.
Glycerin was injected into zone 260 at 2.1 lb/hr. A mixture of 98.62% sucrose and 1.38% sorbitol was added into the large feed port 262 at 194.7 lb/hr. Corn syrup (100°F.) was injected into zone 260 at 39.9 lb/hr. Peppermint flavor was injected into zone 260 at 2.1 lb/hr. The zone temperatures (Z1-Z5, °F.) were set at 350, 350, 300, 55, and 55, reεpectively, and the εcrew temperature (SI) waε εet at 150°F. The mixture temperatureε (T1-T6, °F.) were measured as 338, 300, 260, 125, 101 and 86 respectively. The screw rotation was set at 69 rpm.
The product exited the mixer at 117°F. The finished product had good chew characteristics and there was no evidence of rubber lumps.
Example 28
75/25% Split of Terpene Resin This example illustrates the preparation of a gum base to be uεed to make a peppermint flavored εugar chewing gum. A blend of 26.774% dusted ground isobutylene-iεoprene copolymer, 14.822% low molecular weight terpene resin, 15.062% high molecular weight terpene resin, and 43.343% fine ground calcium carbonate was added to the firεt large feed port 212 at 25.08 lb/hr.
A blend of 9.271% medium molecular weight polyvinyl acetate, 74.152% low molecular weight polyvinyl acetate, 7.306% high molecular weight terpene resin, 7.184% low molecular weight terpene resin and 2.087% color was added at 25.08 lb/hr into the second large feed port 232. Polyisobutylene (preheated to 250°F) was also added into the second large feed port at 3.51 lb/hr.
A fat mixture (225°F) was injected into zone 240 at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonεeed oil, 22% hydrogenated εoybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT.
Glycerin was injected into zone 260 at 3.9 lb/hr. A mixture of 85% εucroεe and 15% dextroεe monohydrate waε added into the large feed port 262 at 203.1 lb/hr. Corn εyrup (100°F) was injected into zone 260 at 30.0 lb/hr. A peppermint flavor was injected into zone 260 at 3.0 lb/hr.
The zone temperatures (Z1-Z5, °F.) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F. The mixture temperatures (T1-T6, °F.) were measured as 324, 291, 154, 117, 110 and 89 respectively. The screw rotation was set at 60 rpm.
The product exited the mixer at 124°F. The finished product had good chew characteristic and there was no evidence of rubber lumps.
Example 29
50/50% Split of Terpene Resin Thiε example illustrates the preparation of a gum base to be used to make a peppermint flavored sugar chewing gum. A blend of 29.737% dusted ground isobutylene-iεoprene copolymer, 10.975% low molecular weight terpene resin, 11.148% high molecular weight terpene resin and 48.140% fine ground calcium carbonate was added to the first large feed port 212 at 22.58 lb/hr.
A blend of 8.099% high molecular weight polyvinyl acetate, 64.777% low molecular weight polyvinyl acetate, 12.749% high molecular weight terpene resin, 12.551% low molecular weight terpene reεin and 1.823% color was added at 19.74 lb/hr. into the second large feed point 232. Polyisobutylene (preheated to 250°F) was also added into the εecond large feed port at 3.51 lb/hr. A fat mixture (225°F) was injected into zone
240 at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated εoybean oil, 15% partially hydrogenated cottonεeed oil, 23% glycerol monoεtearate, 2.4% εoy lecithin and 0.12% BHT.
Glycerin was injected into zone 260 at 3.9 lb/hr. A mixture of 85% sucrose and 15% dextrose monohydrate waε added into the large feed port 262 at 203.1 lb/hr. Corn εyrup (100°F) was injected into zone 260 at 30.0 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr. The zone temperatureε (Z1-Z5, °F) were εet at
350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F. The mixture temperatures (T1-T6, °F) were measured at 339, 289, 155, 112, 107 and 90, respectively. The screw rotation was set at 60 rpm.
The product exited the mixer at 121°F. The finished product had good chew characteristic and there was no evidence of rubber lumps.
Example 30
25/75% Split of Terpene Resin This example illustrates the preparation of a gum base to be used to make a peppermint flavored εugar chewing gum. A blend of 33.433% duεted ground isobutylene-isoprene copolymer, 6.170% low molecular weight terpene resin, 6.274% high molecular weight terpene resin, and 54.123% fine ground calcium carbonate was added to the first large feed port 212 at 20.09 lb/hr. A blend of 7.189% high molecular weight polyvinyl acetate, 57.499% low molecular weight polyvinyl acetate, 16.981% high molecular weight terpene resin, 16.712% low molecular weight terpene reεin and 1.619% color was added at 22.24 lb/hr. into the second large feed port 232. Polyisobutylene (preheated to 250°F) was added into the second large feed port at 3.51 lb/hr.
A fat mixture (225°F) was injected into zone 240 at a total rate of 14.16 lb/hr. This fat mixture included 37% hydrogenated cottonseed oil, 22% hydrogenated soybean oil, 15% partially hydrogenated cottonseed oil, 23% glycerol monostearate, 2.4% soy lecithin and 0.12% BHT. Glycerin waε injected into zone 260 at 3.87 lb/hr. A mixture of 85% εucrose and 15% dextrose monohydrate was added into the large feed port 262 at 203.1 lb/hr. Corn syrup (100°F) was injected into zone 260 at 30.0 lb/hr. Peppermint flavor was injected into zone 260 at 3.0 lb/hr.
The zone temperatures (Z1-Z5, °F) were set at 350, 350, 100, 55 and 55, respectively, and the screw temperature (SI) was set at 100°F. The mixture temperatureε (T1-T6, °F) were measured at 346, 250, 156, 115, 108 and 88, respectively. The screw rotation was set at 60 rpm.
The product exited the mixer at 121°F. The finished product had good chew characteristics and there was no evidence of rubber lumps.
Examples 31-33
For examples 31-33, the same formulation and procedures were used to make three additional base and gum products using a blade-and-pin mixer. The differences were that the formula amount of butyl rubber (isobutylene-isoprene copolymer) was dry blended at room temperature with hydrogenated soybean oil at a level of 1% (Ex. 31) , 2.5% (Ex. 32) and 5% (Ex. 33) of the butyl rubber. This provided an early addition of liquid oil in zone 220. The remaining hydrogenated soybean oil was added with the other fatε/oilε into the liquid injection port .
Addition rateε of the rubber/filler/reεin were about 24.5 to 24.6 lb/hr. Rates for the PVAC resin were about 17.9 to 18.2 lb/hr. Rateε for the fat/oil composition were 13.8 to 19.1 lb/hr., and the rate for polyisobutylene was 3.5 lb/hr. Examples 34-36
For Examples 34-36, the εame formulation and procedureε were uεed to make three additional base and gum products using a blade-and-pin mixer. Differences of theεe three exampleε were that glycerol monostearate waε blended with the butyl rubber. The level of glycerol monoεtearate used was 1% (Ex. 34), 2.5% (Ex. 35), and 5% (Ex. 36) of the butyl rubber. The remaining glycerol monoεtearate was added with the other fats/oils into the liquid injection ports.
Sensory results of Examples 31-36 εhowed that softening agents may be added very early in the base manufacture and be εucceεεfully added to make a chewing gum product. It εhould be appreciated that the methodε of the preεent invention are capable of being incorporated in the form of a variety of embodimentε, only a few of which have been illuεtrated and described above. The invention may be embodied in other forms without departing from its spirit or eεεential characteriεticε. It will be appreciated that the addition of some other ingredients, procesε εteps, materials or components not εpecifically included will have an adverεe impact on the present invention. The best mode of the invention may therefore exclude ingredients, proceεε εtepε, materialε or componentε other than those listed above for inclusion or use in the invention. However, the described embodiments are to be considered in all respects only as illustrative and not restrictive, and the εcope of the invention iε, therefore, indicated by the appended claimε rather than by the foregoing deεcription. All changeε which come within the meaning and range of equivalency of the claims are to be embraced within their scope.

Claims

WE CLAIM :
1. A procesε for continuously producing a chewing gum base comprising the steps of: a) continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having at least one dispersive mixing zone and at least one distributive mixing zone and a plurality of spatially separated feed inlets, at least a portion of said hard elastomer and a portion of said lubricating agents being introduced into εaid mixer through one or more feed inlets located before the end of εaid dispersive mixing zone and a portion of said lubricating agents being introduced into said mixer through one or more feed inlets located downstream of said dispersive mixing zone and before the end of said distributive mixing zone; b) subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and c) continuouεly discharging the chewing gum base from the mixer while chewing gum base ingredientε continue to be introduced and mixed within the mixer.
2. The process of claim 1 wherein the continuous mixer comprises one piece of equipment.
3. The process of claim 1 wherein the mixer comprises a blade-and-pin mixer.
4. The process of claim 1 wherein the hard elastomer is brought into contact with the filler prior to any subεtantial mastication of the hard elastomer.
5. The procesε of claim 1 wherein the lubricating agentε comprise one or more elastomer solvents and the one or more elastomer solvents are introduced into the continuous mixer at two or more of said spatially separated feed inlet locations.
6. The procesε of claim 5 wherein the elaεtomer εolvent is selected from the group consisting of terpene resins, natural rosin eεterε and mixtures thereof.
7. The proceεs of claim 1 wherein the mixer is selected from the group consisting of a counter- rotating twin screw extruder, a co-rotating twin screw extruder, a Japan Steel Works twin screw extruder, a Werner & Pfleiderer twin εcrew extruder, a Leiεtritz twin εcrew extruder, a blade-and-pin mixer and a paddle mixer.
8. The proceεε of claim 6 wherein the natural roεin eεter is selected from the group consisting of glycerol ester of wood roεin, glycerol ester of partially hydrogenated rosin, glycerol eεter of polymerized rosin, glycerol ester of partially dimerized roεin, glycerol eεter of rosin, pentaerythritol esters of partially hydrogenated rosin, methyl eεters of rosin, partially hydrogenated methyl esters of rosin, pentaerythritol esters of rosin, resin ester of glycerol abietate and mixtures thereof.
9. The process of claim 5 wherein the elastomer solvent is added at first and second feed inlets and the ratio of the amount of elastomer εolvent added at the firεt feed inlet compared to the amount of elaεtomer solvent added at the second feed inlet is between about 85:15 and about 55:45.
10. The proceεε of claim 1 wherein the dispersive mixing zone functions as such due to a combination of the use of high shear mixing elements in the mixer, the gum baεe ingredientε being mixed therein, and the temperature and fullneεε conditionε of the mixer.
11. The proceεε of claim 1 wherein the mixer is operated at a peak temperature greater than 250°F in said dispersing mixing zone.
12. The procesε of claim 1 wherein at leaεt a portion of the filler is introduced into the mixer through one or more feed inletε located before the end of the dispersive mixing zone.
13. The procesε of claim 1 wherein the gum base is discharged from the mixer as part of a chewing gum composition.
14. The procesε of claim 1 wherein the hard elaεtomer iε all added at a firεt feed inlet.
15. The proceεε of claim 1 wherein the elaεtomer comprises styrene-butadiene rubber and the filler comprises calcium carbonate.
16. The process of claim 1 wherein the chewing gum base ingredients further comprise polyvinyl acetate and the lubricating agents comprise an elastomer solvent.
17. The process of claim 16 wherein the polyvinyl acetate is preblended with a portion of the elastomer solvent and added to the mixer therewith.
18. A procesε for continuouεly producing a chewing gum baεe compriεing the steps of: a) continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer comprising a plurality of spatially separated feed inlets and a barrel having a predetermined length, at leaεt a portion of εaid hard elaεtomer and a portion of said lubricating agents being introduced into one or more feed inlets located within the first 40% of the barrel length and a portion of said lubricating agentε being introduced through one or more feed inletε located within the last 60% of the barrel length; b) subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum baεe; and c) continuouεly diεcharging the chewing gum baεe from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
19. The procesε of claim 18 wherein the lubricating agents are selected from the group conεiεting of elaεtomer εolventε, εoftening agentε, εoft elaεtomerε, plastic polymers and mixtures thereof.
20. The process of claim 19 wherein the plastic polymers comprises polyvinyl acetate.
21. The process of claim 19 wherein the elastomer solvents are selected from the group consiεting of terpene resins, natural rosin esters and mixtures thereof.
22. The process of claim 19 wherein the softening agents are selected from the group consisting of fats, oils, waxeε emulsifiers and mixtures thereof.
23. The process of claim 19 wherein the hard elastomers have a Flory molecular weight of over about 200,000 and the soft elastomerε have a Flory molecular weight of below about 100,000.
24. The proceεε of claim 23 wherein the εoft elaεtomers are selected from the group consisting of polyisobutylene, polybutadiene and mixtures thereof.
25. The procesε of claim 23 wherein the hard elaεtomer is selected from the group consisting of isobutylene-isoprene copolymer, styrene-butadiene rubber, natural rubbers, natural gums and mixtures thereof.
26. A proceεε for continuously producing a chewing gum base comprising the steps of: a) continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having a plurality of εpatially separated feed inlets, high shear mixing elements and low shear mixing elements downεtream from said high shear mixing elementε, at least a portion of said hard elaεtomer and a portion of said lubricating agents being introduced into said mixer through one or more feed inlets located at or before the high shear mixing elements and a portion of said lubricating agents being introduced into said mixer through one or more feed inletε located downεtream of εaid high εhear mixing elementε and at or before said low shear mixing elements; b) subjecting the chewing gum base ingredients to continuous mixing operations within the mixer, thereby producing a chewing gum base; and c) continuouεly discharging the chewing gum base from the mixer while chewing gum base ingredients continue to be introduced and mixed within the mixer.
27. The procesε of claim 26 wherein the mixer is operated at a peak temperature greater than 175°F. at the high shear mixing elements.
28. The procesε of claim 26 wherein the mixer iε operated at a peak temperature greater than 250°F. at the high εhear mixing elementε.
29. The process of claim 26 wherein the mixer is operated at a peak temperature greater than 300°F. at the high shear mixing elements.
30. The process of claim 26 wherein the lubricating agents comprise one or more softening agents and the one or more softening agents are introduced into the continuous mixer at two or more of said spatially separated feed inlet locationε.
31. The proceεs of claim 26 wherein the lubricating agents comprise one or more soft elastomers and the one or more εoft elastomers are introduced into the continuous mixer at two or more of said spatially separated feed inlet locations.
32. The process of claim 26 wherein the lubricating agents comprise one or more plastic polymers and the one or more plaεtic polymers are introduced into the continuouε mixer at two or more of εaid spatially separated feed inlet locationε.
33. The proceεε of claim 26 wherein the filler is introduced into the continuous mixer at two or more of said εpatially εeparated feed inlet locationε.
34. A proceεε for continuouεly producing a chewing gum baεe compriεing the steps of: a) continuously adding chewing gum base ingredients, including a hard elastomer, filler and one or more lubricating agents, into a continuous mixer having at least one disperεive mixing zone and at least one distributive mixing zone and a plurality of spatially separated feed inlets, at leaεt a portion of εaid hard elaεtomer, a portion of εaid lubricating agentε and at least a portion of said filler being introduced into εaid mixer through one or more feed inlets located before the end of said dispersive mixing zone and a portion of said lubricating agents being introduced into said mixer through one or more feed inlets located downεtream of εaid diεperεive mixing zone and before the end of εaid diεtributive mixing zone, the ratio of the amount of lubricating agents added before the end of the dispersive mixing zone to the amount of lubricating agents added downstream of the dispersive mixing zone being optimized so that the gum base contains a desired amount of lubricating agentε and the diεperεive mixing iε effective to properly masticate the hard elastomer; b) subjecting the chewing gum base ingredientε to continuouε mixing operations within the mixer, thereby producing a chewing gum base; and c) continuously discharging the chewing gum baεe from the mixer while chewing gum baεe ingredientε continue to be introduced and mixed within the mixer.
35. A chewing gum base produced by the process of claim 1.
36. A chewing gum base produced by the procesε of claim 18.
37. A chewing gum baεe produced by the process of claim 26.
38. A chewing gum base produced by the procesε of claim 34.
39. A chewing gum product compriεing a chewing gum baεe made by the proceεs of claim 1.
40. A chewing gum product comprising a chewing gum base made by the process of claim 18.
41. A chewing gum product comprising a chewing gum baεe made by the process of claim 26.
42. A chewing gum product comprising a chewing gum base made by the process of claim 34.
43. A procesε for making a chewing gum composition wherein a gum base is made according to the process of claim 1 and mixed with flavoring agents and bulking and sweetening agents to make said chewing gum composition.
44. A process for making a chewing gum composition wherein a gum base is made according to the process of claim 18 and mixed with flavoring agents and bulking and εweetening agents to make εaid chewing gum compoεition.
45. A proceεs for making a chewing gum composition wherein a gum base is made according to the process of claim 26 and mixed with flavoring agents and bulking and sweetening agents to make said chewing gum composition.
46. A procesε for making a chewing gum composition wherein a gum base is made according to the process of claim 34 and mixed with flavoring agents and bulking and sweetening agents to make said chewing gum composition.
PCT/US1995/003172 1995-03-13 1995-03-13 Continuous chewing gum base manufacturing process using addition of lubricating agents at a plurality of feed inlet locations WO1996028043A1 (en)

Priority Applications (2)

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EP95913684A EP0759700A4 (en) 1995-03-13 1995-03-13 Continuous chewing gum base manufacturing process using addition of lubricating agents at a plurality of feed inlet locations
PCT/US1995/003172 WO1996028043A1 (en) 1995-03-13 1995-03-13 Continuous chewing gum base manufacturing process using addition of lubricating agents at a plurality of feed inlet locations

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US7111372B2 (en) * 2001-11-26 2006-09-26 Opti-Clip Ltd. Computer-controlled milling machine for producing lenses for clip-on accessory

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EP0759700A4 (en) 1999-01-13

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