AU4058702A - Reduced antioxidant gum base and method of preparation - Google Patents

Reduced antioxidant gum base and method of preparation Download PDF

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Publication number
AU4058702A
AU4058702A AU40587/02A AU4058702A AU4058702A AU 4058702 A AU4058702 A AU 4058702A AU 40587/02 A AU40587/02 A AU 40587/02A AU 4058702 A AU4058702 A AU 4058702A AU 4058702 A AU4058702 A AU 4058702A
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Australia
Prior art keywords
antioxidant
chewing gum
gum base
gum
base
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Application number
AU40587/02A
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AU775609B2 (en
Inventor
Kevin B. Broderick
David W. Record
Joo H. Song
Donald J. Townsend
Henry T. Tyrpin
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WM Wrigley Jr Co
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WM Wrigley Jr Co
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Description

S&FRef: 370635D2
AUSTRALIA
PATENTS ACT 1990 COMPLETE SPECIFICATION FOR A STANDARD PATENT
ORIGINAL
Name and Address of Applicant: Actual Inventor(s): Address for Service: Invention Title: Wm. Wrigley Jr. Company 410 North Michigan Avenue Chicago Illinois 60611 United States of America Henry T. Tyrpin, David W. Record, Donald J.
Townsend, Kevin B. Broderick, Joo H. Song Spruson Ferguson St Martins Tower,Level 31 Market Street Sydney NSW 2000 (CCN 3710000177) Reduced Antioxidant Gum Base and Method of Preparation The following statement is a full description of this invention, including the best method of performing it known to me/us:- 5845c REDUCED ANTIOXIDANT GUM BASE AND METHOD OF PREPARATION FIELD OF Th-E INVENTION This invention is directed to a gum base hlaying reduced initial antioxidant levels, a method of making gum base which requires less in~tia antic-xidn: :ra c~v~-:ioal ezhods, and a f-4 e unzsecnewn-gum which havenormal ant ioxidan-- levels but reoucedlevels of: dezrad~ed antioxidant b'ooccs BA~:~RTW7O T--iE 7NVE'NTLION ci 2un ba-ses, f-or Use~ in wizun r e U s act2rn I :xda as.
a :':zan U ns t be added a t s UffIIc Ient Ie~ :ne gum bas e to iorovide stability of" a) the aurn a :nrra~etsAuring manufacture o' -n un c ase; C gun, base and othe-r chewing gun ingredienits, durl-ncmnanufacture of the chewing gum; and c) thefnst cn-e%%'nz- gu-n oroduct, during shelf storage.
The most severe conditions rea uirjng antioxidant generally occur during manufacture of the gum base, as a result of the relatively high snear, high temperature and long mixing times required to 2 disperse the elastomer, filler, and other gum base ingredients. For instance, a two hour total mixing time at 280 0 F is common for a conventional batch process used to make gum base. Even though the Santioxidant is often added late, along with fats and oils, a half hour or more is often required to incorporate the stabilized fats and oils into the base.
During this time, much of the antioxidant initially added is often lost due to degradation and volatilization from the heat. This loss may exceed o the initial antioxidant.
Co-ared to te gum, -ase manufacturine cess, e crecarai or cew--n cum procuc: f case ano ndch=- cn cw na, reaien t is s cn D re o nalc c C f ave icx ni= i e, ccared :c the e 7anu f: ac f c'-wi~ cum SCe v muil. S S1~llCc_- eve-?" C~3~e tc 7cc: aniox:an: during the ini:ial manufacture of c-ewIng aulm -ase he synthetic anticxdants butvated nyr'xyol ee (BHT) an' but latei hydroxyanisol 'Et effecive stabilizers for finished chewin c-um crocucts at levels of about 10-100 carts Der mi- 1cr ecause thec gun- base cenerally constitutes S about 10-50% by weight of the chewing gum product, these antioxidants are added at higher concentrations curing manufacture of the gut base. During the mixing of the gum base ingredients, these antioxidants partially volatilize or degrade into complex furans, biphenyl compounds, and other unwanted chemicals. The initial addition of antioxidant into the gum base must be sufficiently high to permit these losses as well as the dilution of antioxidant occurring when the gum base is combined with other chewing gum ingredients.
s Other synthetic antioxidants, and natural antioxidants, volatilize or degrade to some extent curing gum base manufacture. These other antioxidants 3 include, for example, tert-butyl hydroquinone
(TBHQ)
and tocopherols. In order to minimize the degradation of antioxidant, and reduce the amount of unwanted chemical by-products, there is a demand for a process which efficiently combines the gum base ingredients using less severe conditions.
SUMMARY OF THE INVENTION The present invention includes a stabilized chewing gum base made using lower initial antioxidant to levels than conventional gum bases, and a method of making gum base which causes less volatilization and degradation of antioxidants. The results are a finished gum base which includes a normal level of remaining antioxidant, and less unwanted degradation by-products, compared to conventional finished cum bases, and a corresponding stabilized chewing gum which contains less chemical by-products.
A gum base is prepared initially using an anicx:idant in the range of about 10 to about 2000 com S based o the weight of the um bas. level used will depend on the particular antioxidant being used, local regulations, shelf life expectations and other actors. The antioxidant may be synthetic or natural and is preferably selected from 5:A, T3H~Q," propCy g allate, or combinations thereof. After the gum base :ngre ients have been mixed with each other, and combined with other chewing gum ingredients to form a finished product, at least about two-thirds of the initial antioxidant will remain, and will be present in 3j the chewing gum product at about 7 to about 1000 ppm based on the weight of the chewing gum.
The level of the antioxidant present in the finished chewing gum is conventional. The differences are that the starting level of antioxidant added during 3y manufacture of the gum base is lower than in a conventional method, and the percentage of the initial 4 antioxidant remaining in the finished gum base and chewing gum product is higher. Because less antioxidant is lost during processing, especially due to degradation, there is less quantity of unwanted 6 reaction products of the antioxidant. The result is a cleaner, better tasting chewing gum product.
In order to accomplish these objectives, the chewing gum base is prepared using a process which is gentler than conventional batch processes. Bvy' S "gentler", it is meant that the gum base is made using less mixing time, less temperature, less shear, or some combination of the foregoinc. Preferably, the gum base is prepare using a continuous mixer havin an av residence te for gum base manufacture of not more than about 2- minutes, and an average cum ba=se mixn temperature cf no t more than about 1400C (with a peak S-miin tem.erature cf not more than about !60 0
C).
Preferably, =he manufacture of the gum base and chewin gum are integrated into a single efficient continuous Ao mixer.
With fne forecoinc in mind, t is a -eature anc acvantage of the invention to provide a method of ma.:ing gum base during which a higher percentage of an.ioxidant i-nitally added is retained, co7-ared to conventional gum base manufacturing methods.
It is also a feature and advantage of the invention to provide a gum base and corresponding chewing gum in which higher percentages of antioxidant initially added are retained, compared to conventional products.
It is also a feature and advantage of the invention to provide a gum base and chewing gum having normal levels of antioxidant in the finished products, and lower levels of degraded antioxidant chemicals, 3; compared to conventional products.
The foregoing and other features and advantages of the invention will become further 0 I 5 apparent from the following detailed description of the presently preferred embodiments, read in conjunction with the accompanying examples and drawings. The detailed description, examples and drawings are intended to be merely illustrative rather than limiting, the scope of the invention being defined by the appended claims and equivalents thereof.
BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a partial exploded perspective view °o of a preferred Buss high efficiency continuous mixer used to practice the method of the invention, illustrating a mixing barrel and mixing screw arrangement.
Fig. 2A is a perspective view of an on-screw element used on the upstream side of a restriction rin= assembly, in the presently preferred high e=ffciency mixer configuration.
Fig. 2B is a perspective view of an on-screw element usea on the downstream side of the restricti d -i asebily in the esently preferred high efficiency mixer configuration.
ig. 2C is a perspecive view of a resricoln ring assembly use d in the presently preerred high efficiency mixer confiuration.
Si. 3 is a perspective view showinc the lative positioning of the elements of Figs. 2A, 2B and 2C in the presently preferred high efficiency mixer configuration.
Fig. 4 is a perspective view of a low-shear SO mixing screw element used in the presently preferred high efficiency mixer configuration.
Fig. 5 is a perspective view of a high-shear mixing screw element used in the presently preferred high efficiency mixer configuration.
6 Fig. 6 is a perspective view of a barrel pin element used in the presently preferred high efficiency mixer configuration.
Fig. 7 is a schematic diagram of a presently preferred arrangement of mixing barrel pins and ingredient feed ports used to practice the method of the invention.
Fig. 8 is a schematic diagram of a presently preferred mixing screw configuration used to practice 1o the method of the invention.
DETAILED DESCRIPTION OF THE PRESENTLY PREFERRED
EMEODIMENTS
zn accordance wi:h th:e uivenic- a Z'u ase ae. cew:n gum are m ui ce or more S anticxi-dants added durinc manufacure cf c e gum base, in suc a way tha: at leas about two-hirds of the total antioxidant iniially added to the gum base is still present after the chewing gum manufacture has been comoeted. Preferably, at least about three- S rourns of the antioxidant initially added to the cum base is still present in the final chewing gum product.
This means that no more than about one-third, and preerably no more than about one-fourth, of the total anticxidant added to the gum base, is volatilized, degraded, or otherwise lost during the manufacture of cum base and chewing gum. This represents a significant improvement over the prior art, in which more than 40% of the antioxidant initially added to the gum base was lost during manufacture of the gum base S3 alone.
The level of antioxidant present in the finished chewing gum made according to the invention is comparable to the levels of antioxidant present in conventional finished chewing gums. Because less 4- antioxidant is lost during manufacture of the gum base, the level of antioxidant initially added to the gum base may be lower for the gum base and chewing gum made 7 according to the invention. Also, the finished chewing gum of the invention has less degraded antioxidant byproducts (for example, complex furans and biphenyl compounds) than prior art chewing gums containing the same antioxidant levels. Generally, the level of antioxidant in the finished chewing gum will be about 1-1000 ppm, depending primarily on which antioxidant is used. Preferably, the chewing gum will include about 27-300 ppm antioxidant.
The level of antioxidant initially added to the gum base may be determined based on the level of the particular antioxidant desired in the chewing gum product, the level of gum base to be used in the chewing gum, and the amount of antioxidant lost during '6 manufacture of the gum base and chewing gum. The antioxidant level initially added to the gum base should be about 1-1000 ppm based on the weight of the chewing gum, preferably about 8-300 ppm based on the weight of the chewing gum, to be produced from the cum o ase. This requires a starting level of about 10-2000 ppm based on the weight of the um ase, preferably aDout 40-1000 Dpm.
it is expected that the amount of anticxidant ost curng manufa-cture of the chewin.g um will b smal or neli--ible compared to the amount lost durinmanufacture of the gum base. Put another way, at least aoout two-thirds, and preferably at least about threefourths, of the antioxidant initially added to the gum base will remain after the gum base manufacture has 3o been completed, and will still remain (with only minor variation) after the chewing gum manufacture has been completed. When gum base is prepared separately from chewing gum, the finished gum base should contain about 7 to about 2000 ppm antioxidant, preferably about 27 to 3- about 1000 ppm antioxidant.
The present invention contemplates the use of any commercially acceptable synthetic or natural 8antioxidant in the chewing gum base. Preferred antioxidants include one or more of BHT, BHA, TBHQ, and propyl gallate. Of these, BHT, BHA and combinations thereof are especially suitable for use with the D nvention, because there is a desire to reduce the amount of conventional synthetic antioxidants added in chewing gum and, particularly, to reduce their degradation by-products.
in addition to the antioxidant, the gum base :ncludes elastomers, elastomer plasticer (rsn) fats, oils, waxes, soFt_-ener-s and inorganic fillers.
The omers consrz-u-e about S to about 95 per cent z)eln te b aSe, pref'erably bertween 10 and_ 70 e av an an d cS r e Fe r a b L be t we en 1san pe We= cy eich. -aszomers may incl1ude svn's-ch s~ -L n :DC'lVybUt ae szyrene-buta.--3c yv nipr a c eta t e, vinylaet -v ly] v ene v -i atetate, n_ M mi4ue tneec z~storters may a-,sc cuae natural elastomers, ~utncnatural rube sch as smoked or li auid late.
=ne as well1 as naurl ums sucn. as jeluronc, t2.tasz_ perillo rassarandub= balatia, mass-ra-4"- C OChC. -zero, rcsindinha, chce utta hang k==n c--Xt-e tnereo:. z.Iastomers crovidie the rucobery, r, 2 rure to tne cum which varies decenalinn on lastomer's chemical and physical properties, and howv, the elastomer ts hiended with other ingredients.
S,---heti c elastomers are preferred for use with the pres ent: invention.
Elastomer Pliasticizers modify the finished :uIrmness when used in the gum base. Elastomer r,'as ticizers typically constitute from about 0 to ab~out 6. 75 per cent by weight of the gum base, preferably 5 to Der cent by weight and most preferably 10 to 30 per cent_ by weight. Elastomer plasticizers include natural 9 rosin esters such as glycerol ester of partially hydrogenated rosin, glycerol ester of polymerized rosin, glycerol ester of partially dimerized rosin, glycerol ester of rosin, glycerol ester of tall oil S rosin, pentaerythritbl esters of partially hydrogenated rosin, methyl and partially hydrogenated methyl esters of rosin, pentaerythritol ester of rosin or mixtures.
Elastomer plasticizers also include synthetics such as terpene resins derived from alpha-pinene, beta-pinene, *o dipentene or di-limonene, and combinations thereof.
Waxes include synthetic polyethylene and Fischer-Tropsch waxes) and natural (candelilla carnauba, beeswax, rice bran or mixtures thereof) and petroleum microcrystalline and paraffin). Waxes, IS when used, generally constitute up to 30 weight per cent of the gum base. When used, waxes aid in the curing of finished gum made from the gum base and also help improve the release of flavor, increase the shelf life and improve the chewing texture.
illers modify the texture of the cum base and aid processing. Fillers/exturizers include magnesium and calcium carbonate, ground limestone and silicate types such as magnesium and aluminum siicae, clay, alumina, talc as well as titanium cide mono- AT di- and tricalcium phosphate, cellulose polymers su Ca ethylcelu e and methyl:eltulose, wood, or ixtures thereof. The filler typically comprises about 1 to about 60 per cent by weight of the gum base. Gum bases which utilize acidic ingredients preferably g3 contain a filler that is inert to acids, most preferably talc.
Softeners and emulsifiers modify the texture and cause the hydrophobic and hydrophilic components of the gum base and chewing gum to become more miscible.
dj Softeners/emulsifiers include tallow, hydrogenated tallow, lard, hydrogenated and partially hydrogenated vegetable oils, cocoa butter, glycerol monostearate, 10 glycerol triacetate, lecithin, mono-, di- and triglycerides, acetylated mono-, di- and triglycerides, distilled mono-, di- and triglycerides, and fatty acids stearic, palmitic, oleic, linoleic and linolenic acids) or mixtures thereof. Softeners/emulsifiers generally constitute between 0.5 and 40 weight per cent of the gum base.
Colorants and whiteners impart desired color cr remove undesired color by whitening the base and/or io the chewing gum. Colorants and whiteners include
FD&C
:ype lakes, plant extracts, titanium dioxide or ixtures thereof.
The gum base constitutes about 5-95% by eight c: the chewi n gum, preferably about 10-50% >b weight cf the chewing cum, most preferably about 20-30% Sweight of the chewing gum. In addition to the crase, which s cenerally water-insoluble, the chewingu- includes a water-soluble bulk portion and one or o-e flavoring agents. The water-soluble portion 0o dissipates over a period of time during chewinc. base remains in the mouth throughout the chewino trocess.
The water soluble portion of the chewing cum may include softeners, bulk sweeteners, hich intensity s;weeteners, flavoring agents and combinations thereof.
Softeners are added to the chewing gum in order to op:imize the chewability and mouth feel of the gum.
The softeners, which are also known as plasticizers or plasticizing agents, generally constitute between about o 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 11 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 (o 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.
'1 High intensity sweeteners may also be oresent and are commonly used with sugarless sweeteners. When used, high inensity sweeteners typically constitute between 0.001-5% by weight of the chewing gum, preferably between 0.01-1% by weight of the chewing 2o gum. Typically, hich intensity sweeteners are at leas_ 22 times sweeter than sucrose. These may include but are not limited to sucralose, aspartame, salts of acesulfame, alitame, saccharin and its salts, cyclamic aid and its salts, glycyrrhizin, dihydroc alcones, j t.haumatin, monellin, and the like, alone or in 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 3 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 cnewing gum in an amount within the range of about 0.1- 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 12 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 o0 acceptable fashion.
Optional ingredients such as colors, emulsifiers, pharmaceutical agents and additional flavoring agents may also be included in chewin gc-.
:n accordance wit- the invention, the cum zase should be made usina a continuous mixer. The average mixer res ence time used to complete the m.anuacture of the gum base should be no more than about 45 minutes, preferably no more than about minutes, most preferably about 20 minutes or less.
I0 Also, the average mixer temperature used to manufacture the gum base should be no more than about 140 0
C,
preferably no more than about 125 0 C. By so limiting the average residence time and temperature, the volatilization and degradation of antioxidants added i during manufacture of the gum base can be minimized.
In order to minimize the residence time, the continuous mixer should be capable of providing thorough mixing of the gum base ingredients, to form a homogeneous gum base, using a relatively short distance 3o or length of the mixer. This distance can be expressed as a ratio of the length of a particular active region of the mixer screw, which is composed of mixing elements, divided by the maximum diameter of the mixer barrel in this active region. This ratio is abbreviated as L/D.
The method of the invention contemplates that the gum base manufacture should be performed using an 13 L/D of not more than about 40. This means that the gum base ingredient's are added to the continuous mixer and blended to a homogeneous mass using an L/D of not more than about 40. Preferably, the gum base should be made using a mixing L/D of not more than about 30, most preferably not more than about A variety of continuous mixers can be properly configured to manufacture the gum base in accordance with the invention. The continuous mixer io may be a properly configured twin screw extruder (with corotating or counterrotating screws), a single screw extruder, a blade-and-pin mixer, or another continuous mixing apparatus. One particularly suitable continuous mixer is a high efficiency blade-and-Din mixer as S described further herein. Another very suitable mixer for making the gum base is a ZSK58 corotating twinscrew extruder available from Werner-Pfleiderer CorD.
in Ramsey, N.J.
In a preferre embodiment, the manufacture of <u the cum base, and the combining of the cum base with Zne remaining chewing gum ingredients, are both per:ormed in a single integrated high efficiency continuous mixing process. When the manufacture of cum ase an c nLewng gum are so integrated, the method of tne invention comprises performing the following sZeos a s -inle continuous mixer: a) adding and thoroughly mixing at least a portion of the chewing gum base ingredients (elastomer, elastomer plasticizer, filler, etc.) in a continuous 3 mixer, using an L/D of not more than about b) adding at least a portion of the remaining (non-base) chewing gum ingredients (sweeteners, flavors, softeners, etc.), and thoroughly mixing these ingredients with the gum base in the same mixer, using an L/D of not more than about 15; and c) sufficiently completing the entire addition and mixing operation in the same mixer, so 14 that the ingredients exist as a substantially homogeneous chewing gum mass, using a total L/D of not more than about When performing the above integrated method, it is preferred that the gum base ingredients be completely added and mixed upstream from the remaining chewing gum ingredients, and that the remaining ingredients be completely added downstream for mixing with the already blended gum base. However, the S invention also includes those variations wherein a portion of the gum base ingredients may be added downstream with or after some of the remaining -i Ingreients, ad/crwherein a portion of the remai i (non-base) ingredients are added upstream with or before some cf the base ingredients. The imortant :eature is tha: a substanzially homogeneous chewing cum procuct mass be formed in a single continuous mixer, using an L/D of not more than about When performing the integrated method to make ao cum base and chewing gum in a single mixer, a bladeand-pin mixer can be used. A blade-and-pin mixer, exemplified in Fig. 1, uses a combination of selectively configured rotating mixer blades and stationary barrel pins to provide efficient mixino 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. i, 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 surrounds the mixing screw 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. The mixing blades 124 protrude 15 radially outward from the shaft 122, with each one resembling the blade of an axe.
The mixing barrel 140 includes an innerbarrel housing 142 which is generally cylindrical when the barrel 140 is closed around the screw 120 during operation-of the mixer 100. Three rows of stationary pins 144 are arranged at evenly spaced locations around the strew shaft,.-i42, 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 inside the barrel 140 and is driven by a variable soeed motor (not shown). During rotation, the mixing screw iS 120 also moves back and forth in an axial direction, creating a combination of rotational and axial mixinc 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 o o=ther. Also, the radial edges 126 of the blades 124 never touch the barrel inner surface 142, and the ends 146 of the pins 144 never touch the mixing screw shaft 122.
Figs. 2-6 illustrate various screw elements j- which can be used to configure the mixing screw 123 for cplimum use. Figs. 2A and 2B illustrate on-screw elements 20 and 21 which are used in conjunction with a restriction ring assembly. The on-screw elements and 21 each include a cylindrical outer surface 22, a 3, plurality of blades 24 projecting outward from the surface 22, and an inner opening 26 with a keyway 28 for receiving and engaging a mixing screw shaft (not shown). The second on-screw element 21 is about twice as long as the first on-screw element Fig. 2C illustrates a restriction ring assembly 30 used to build back pressure at selected locations along the mixing screw 120. The restriction 16 ring assembly 30 includes two halves 37 and 39 mounted to the barrel housing 142, which halves engage during use to form a closed ring. The restriction ring assembly 30 includes a circular outer rim 32, an inner 6 ring 34 angled as shown, and an opening 36 in the inner ring which receives, but does not touch, the on-screw elements 20 and 21 mounted to the screw shaft.
Mounting openings 35 in the surface 32 of both halves of the restriction ring assembly 30 are used to mount ic the halves to the barrel housing 142.
Fig. 3 illustrates the relationship between t=e restriction ring assembly 30 and the on-screw elements 20 and 21 dring operation. When the mii screw 120 is turn--n inside the barrel 140, and -s reciprocating axially, the clearances between the onscrew elements 20 and 21 and the inner rinc 34 prov de t~ne primar means of passage of material from one side of the restriction ring assembly 30 to the other. The on-screw element 20 on the upstream side of the o restriction ring assembly includes a modified blade 27 erittinc clearance of the inner ring 34. The other on-screw element 21 is placed generally downstream of the restriction ring assembly 30, and has an end blade (not visible) which moves close to and wines the opposite surface of the inner ring 34.
The clearances between outer surfaces 22 of the on-screw elements 20 and 21 and the inner ring 34 of the restriction ring assembly 30, which can vary and preferably are on the order of 1-5mm, determine to a large extent how much pressure build-up will occur in the upstream region of the restriction ring assembly during operation of the mixer 100. It should be noted that the upstream on-screw element 20 has an L/D of about 1/3, and the downstream on-screw element 21 has an L/D of about 2/3, resulting in a total L/D of about for the on-screw elements. The restriction ring assembly 30 has a smaller L/D of about 0.45 which 17 coincides with the L/D of on-screw elements 20 and 21, which engage each other but do not touch the restriction ring assembly.
Figs. 4 and 5 illustrate the mixing or "kneading" elements which perform most of the mixing work. The primary difference between the lower shear mixing element 40 of Fig. 4 and the higher shear mixing element 50 of Fig. 5 is the size of the mixing. blades which project outward on the mixing elements. In Fig.
to 5, the higher shear mixing blades 54 which project outward from the surface 52 are larger and thicker than the lower shear mixing blades 44 projecting outward from the surface 42 in Fig. 4. For each of the mixing elements 40 and 50, the mixing blades are arranged in three circumferentially-spaced rows, as explained above with respect to Fig. 1. The use of thicker mixing blades 54 in Fig. 5 means that there is less axial distance between the blades and also less clearance between the blades 54 and the stationary pins 144 as the screw 120 rotates and reciprocates axially (Fie.
SThis recuction in clearance causes inherently higher shear in the vicinity of the mixing elements Fig. 6.illustrates a single stationary cin d oetac:he from the barrel 140. The cin 144 incudes a chreaded base 14-5 which Permits attacnhment at selected locions along the inner barrel shaft 12.
s also pssible to configure some of the cins 14 as liquid injection ports by providing them with hollow center openings.
Fig. 7 is a schematic view showing the presently preferred barrel configuration, including the presently preferred arrangement of barrel pins 144.
Fig. 8 is a corresponding schematic view illustrating the presently preferred mixing screw configuration.
The mixer 200 whose preferred configuration is illustrated in Figs. 7 and 8 has an overall active mixing L/D of about 19.
18 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 smaller linuid injection ports 241, 243, 261, 263 and 264 which can be used to add liquid ingredients. The liquid injection (o ports 241, 243, 261, 263 and 264 include special barrel pins 144 formed with hollow centers, as exp'lained above.
Referring to Fig. 7, barrel pins 144 are preferably present in most or all of the available iccations, in all three rows as shown.
Referring to Fig. 8, the presentlv referred configuration of the mixing screw 120 for most chewinc gum products is schematically illustrated as follows.
Zone 210, which is the initial feed zone, is configured .A 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 p-rpose is merely to convey ingredients into the mixing Szones.
The first mixing zone 220 is configured, from left to right (Fig. with two low shear mixing elements 40 (Fig. 4) followed by two high shear elements 50 (Fig. The two low shear mixing o elements contribute about 1-1/3 L/D of mixing, and the two high shear mixing elements contribute about 1-1/3 L/D of mixing. Zone 220 has a total mixing L/D of about 3.0, including the end part covered by a 57mm restriction ring assembly 30 with cooperating on-screw b elements 20 and 21 (not separately designated in Fig.
8).
19 The restriction ring assembly 30 with cooperating on-screw elements 20 and 21, straddling the end of the first mixing zone 220 and the start of the second 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 40 and 1.5 high shear mixing elements 50. The three low shear mixing elements contribute about 2.0 L/D of mixing, and the i/ 1.5 high shear mixing elements contribute about 1.0 L/D of mixing. Zone 230 has a total mixing L/D of about Straddling the end of the second mixing zone 230 and the start of the third mixing zone 240 is a 60mm restriction ring assembly 30 with cooperating onscrew elements 20 and 21, contributing a combined
L/D
cf about 1.0. Then, zone 240 is configured, from left to right, with 4.5 high shear mixing elements contributing a mixing L/D of about 3.0. Zone 240 also A0 has a total mixing L/D of about Straddling the end of the third mixino zone 240 and the start of the fourth mixing zone 250 is another 60mm restriction ring assembly 30 with cooperatin: on-screw elements 20 and 21, contributi-c a Scobined L/D of about 1.0. Then, the remainder of the fourtnh mixng zone 250 and the fifth mixino zone 260 are conicure with eleven low shear mixing elements contributing a mixing L/D of about 7 1/3. Zone 250 has a total mixing L/D of about 4.0, and zone 260 has a 3, total mixing L/D of about As stated above, it is generally preferred mnat the gum base and ultimate chewing gum product are maoe continuously in the same mixer. Generally, the gum base portion is made using a mixing L/D of about cr less, preferably about 20 or less, most preferably about 15 or less. Then, the remaining chewing gum ingredients are combined with the gum base to make a 20 chewing gum product using a mixing L/D of about 15 or less, preferably about 10 or less, most preferably about 5 or less. The mixing of the gum base ingredients and the remaining chewing gum ingredients may occur in distinct parts of the same mixer or may overlap, so long as the total mixing is achieved using an L/D of about 40 or less, preferably about 30 or less, most preferably about 20 or less.
When the preferred blade-and-pin mixer is io used, having the preferred configuration described about, the total chewing gum can be made using a mixine L/D of about 19.. The gum base can be made using an L/D cf about 15 or less, and the remaiinng gum ingredi-es can be cobined with the gum base using a further
L/D
i of about 5 or less.
Sorder to minimize the shear and, thus, minimize the volatilization an degradation of an antioxidant using the preferred blade-and-pin mixer 200, 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 is preferably optimized so that the gum base is at about 130°? or lower when it initially meets the other cnewing gum ingredients, and the chewing gum product is or about 1300F or lower (preferably 125 0 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.
S 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 first large feed port 212 in the feed zone 210 of the mixer 200, and are subjected jf to efficient dispersive mixing in the first mixing zone 220 while being conveyed in the direction of the arrow 122. The remaining elastomer solvent (if any) and 21 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, colors and antioxidants are added to the liquid injection ports 241 and 243 in the third mixing zone 240, and the ingredients are subjected to distributive mixing in the mixing zone 240 while being conveyed in 'o the direction of the arrow 122. At this point, the gum base manufacture should be complete, and the gum base should leave the third mixing zone 240 as a substantially homogeneous, lump-free comoound with a uniform color. At this point, at least about twothirds and, preferably, at least about three-fourths of the antioxidant initially added, should still remain in the base.
The fourth mixing zone 250 is used primarily to cool the gum base, although minor ingredient .o addition mav be accomplished. Then, to manufacture the final chewing gum product, glycerin, corn syrup, other bulk sugar sweeteners, high intensity sweeteners, and flavors can be added to the fifth mixing zone 260, and -te ingredients are subjected to distributive mixinc.
I If the g-um roduct is tc be sugarless, hydrogenated starch hydrclyzate or sorbitol solution can be substituted for the corn svrup and nowdered alditols can be substituted for the sugars.
Preferably, glycerin is added to the first 33 liquid injection port 261 in the fifth mixing zone 260.
Solid ingredients (bulk sweeteners, encapsulated high intensity sweeteners, etc.) are added to the larce feed port 262. Syrups (corn syrup, hydrogenated starch hydrolyzate, sorbitol solution, etc.) are added to the ,j 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 22 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 continuous stream or "rope". The continuous stream or rope can be deposited onto a moving conveyor and carried to a forming station, where the gum is shaped into the desired form such as by pressing it into ,c sheets, scoring, and cutting into sticks. Because the entire gum manufacturing process 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 simplified mechanical and thermal histories.
Because there is very little antioxidant loss durinc the chewing gum manufacturing stage, the final product ould sill contain at leas aout two-thirds and, preferably, at least about three-fourths of the antioxidant added during manufacture of the gum base.
4 A wide range of changes and modifications to the preferred embodiments of the invention will be apparent to persons skilled in the art. The above preferred embodiments, and the examples which follow, are merely illustrative of the invention and should not J' be construed as imposing limitations on the invention.
For instance, different continuous mixing equipment and different mixer configurations can be used without ceparting from the invention as long as the preparation of a chewing gum base is accomplished in an efficient continuous mixer using a mixing L/D of not more than about EXAMPLE 1 (COMPARATIVE) The following gum base composition was prepared using a conventional batch process: 23 InaredientI By Weight Butyl Rubber (shredded) 9.89 Calcium Carbonate 13.19 Polyvinyl Acetate (Mol. Wt. 25,000) 21.77 Polyisobutylene 15.83 Cocoa Powder 0.50 Glycerol Monostearate 2.64 Hydrogenated Cottonseed Oil 13.19 Hydrogenated Soybean Oil 13.19 Partially Hydrogenated Soybean Palm Oil 9.76 BHT 0.04 TOTAL 100.0 The foregoing composition was made using a Werner-Pfleiderer dual sigma blade mixer having a 757pcund batch size. The mixer was run using front and rear blade speeds of 43.8 and 33.8 rpm and was heated with 45 psi steam. The tozal mixing time for making the batch was 135 minutes.
The buty rubber, calcium carbonate, polvinvl acetate, volyistutylene and cocoa Dowder were added to the batch mixer and blended during the first 75 minutes. The hydCrogenated soybean oil was added at 75 minutes and blended with the above Ingrealens. As mixiro continued, the hdro enat e cottonseed cil was added a: 30 minutes. Tn B7:, Slvlcercl =znoSt-earate ant partially nydroenatec soybean ant palm oil were all added at 105 min-tes, after which all the ingredients were blended for an additional 30 minutes.
Analytical testing of the finished gum base d. showed BHT present at a level of 232 ppm. This renresented a 42% loss from the 400 ppm BHT initially added. One month later, the gum base was tested again, and the BHT was detected at 223 ppm.
The following chewing gum composition was made from the above gum base using a laboratory batch mixing process.
24 Incredient By Weight Sugar 64.4 Gum Base 20.0 Corn Syrup 13.3 Sorbitol 0.9 Glycerin 0.7 Peppermint Flavor 0.7 TOTAL 100.0 Analytical testing of the finished chewing gum showed BHT present at 43.7 ppm, possibly indicatinc a slight additional loss during the mixing of chewin cum. The total ET loss for both phases of production.
Was 5. EXAMPLE 2 The same chewing gum product composition of Example 1 was manufact-ure using a Buss kneader with a 1o 100mm screw diameter, configured in the preferred manner described above for integrated manufacture of the gum base and chewing gum in a single continuous mixer. As described above, the mixer was configured with five mixing zones, a total mixing L/D of 19, and i' an initial conveying L/D of 1 1/3. Nc die was used at the end of the mixer, and the chewing gum product exited as a continuous rope. The example was designed to yield a production rate of about 300.1 pounds per hour finished gum.
Ao Liquid ingredients were fed using volumetric pumps into the large feed ports and/or smaller liquid injection ports generally positioned as described above, unless otherwise indicated. The pumps were appropriately sized and adjusted to achieve the desired 4- feed rates.
Dry ingredients were added using gravimetric screw feeders into the large addition ports positioned as described above. Again, the feeders were 25 appropriately sized and adjusted to achieve the desired feed rates.
Temperature control was 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 100 0 C, and oil cooling was used at higher temperatures.
Where water cooling was desired, tap water (typically at about 55 0 F) was used without additional chilling.
0 o 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. 7 and and are reported below as Z1, Z2, Z3, Z4 and Z5, respectively.
S Fluid temperatures were also set for the mixing screw 120, and are reported below as Si.
Actual mixture temperatures were recorded near the downstream end of mixing zones 220, 230, 240 and 250; near the middle of mixing zone 260; and near d the end of mixing zone 260. These mixture temoeratures are reported below as Tl, T2, T3, T4, T5 and T6, respectively. Actual mixture temperatures are influenced by the temperatures of the circulating uidc, t-e heat exchange properties of the mixture and s surrounding barrel, and the mechanical heating from the .mixing rocess, and often differ from the set temperatures due to the additional factors.
All ingredients were added to the continuous mixer at ambient temperatures (about 77°F) unless 3; otherwise noted.
For this run, the zone temperatures were set (in OF) at 350, 350, 300, 78 and 78, respectively. The screw temperature S1 was set at 150 0 F. Actual mixture temperatures (T1-T6, OF) were -9 measured, at steady state, as 325, 293, 256, 127, 114 and 115, respectively. The screw rotation was 90 rpm.
26 A dry mixture of 57% butyl rubber and 43% calcium carbonate was added, at 13.9 pounds per hour, into the first large feed port (port 212 in Figs. 7 and Polyisobutylene, preheated to 1000C, was also S added at 9.5 pounds per hour into this port.
Low molecular weight polyvinyl acetate (weight average Mol. Wt. 25,000) was added at 13.0 pounds per hour into the second large feed port 232.
Cocoa powder was also added at 0.3 pounds per hour in o Sthis port.
A mixture of 0.1% BHT, 34.0% hydrogenated cottonseed oil, 34.0% hydrogenated soybean oil, 6.7% glycerol monostearate and 25.2% partiallv hydrocen.
soybean and palm cil was -ehnc-ed to abou 1 P-e tec to about 80-90°C fo CS about .5 hours before the szart of the run. Durinc the run, this mixtu-re was injecte into two licuid jecion pors 241 and 243 in the third nmixin zo 240, at a total rate of 23.3 pounds per hour. This resulted in an initial BHT concentration of 77.6 ppm based on the weight of the chewing gum, comparable to tne 80 ppm used for Example 1.
Glycerin was injected at 2.1 pounds per hour nt o licuid injection port 261 in the fifth mixing zone 260.
A mixture of 98.6% sugar and 1.4% sorbitol was added at 196 pounds per hour into the feed port 262 in the mixing zone 260.
Corn syrup (at about 40 0 C) was injected at 39.9 pounds per hour into liquid injection port 263 in S3 zone 260. Peppermint flavor was injected at 2.1 pounds per hour into liquid injection port 264 in zone 260.
The chewing gum product, which exited at a temperature of about 50 0 C, was judged to be of acceptable quality. Analytical testing showed the final product to contain BHT at a level of 59.6 ppm, versus the 77.6 ppm that was initially added. This represented only a 23% loss in BHT during the 27 integrated manufacture of the gum base and chewing gum, far less than the 45% loss experienced in Example 1, when the gum base and chewing gum were prepared using conventional techniques.
EXAMPLE 3 As explained above, Example 2 was performed using the same starting level of BHT as Example 1.
Because the BHT loss during production of the gum base and chewing gum was substantially less for Example 2 to than for Example 1, the finished product of Example 2 had a higher BHT content than the finished product of Example 1. In order to provide a product using the method or Example 2 which has a BHT content of only 43.7 ppm (to match the product of Example it would be necessary to perform the method of Example 2 usinc a lower starting quantity of BHT.
Given that the method of Example 2 resulted n a 23% loss of T, the desired starting cantit can e cd~trin y iv tart ed uantizt by a n a C t e 43.7 DSr S (1 .00-.23) pp ,th start: z a t t-v _C as: :ntn rodzuctio. rate r::h au. A: a r tion rate cf 300.i onds Z h oU, the BHT should be initially added to the mixer at 0.0170 pounds per hour. Instead of combininc 0.1% BHT inct the preheated mixture of BHT and oils which is added via injection ports 241 and 243, the preheated 3 mixture need only contain about 0.073% BHT.
It should be appreciated that the method of the present invention is capable of being incorporated in the form of a variety of embodiments, only a few of which have been illustrated and described above. The 53 invention may be embodied in other forms without 28 departing from its spirit or essential characteristics.
It will be appreciated that the addition of certain other ingredients, process steps, materials or components not specifically included will have an adverse impact on the present invention. The best mode of the invention may therefore exclude ingredients, process steps, materials or components other than those listed above for inclusion or use in the invention.
However, the described embodiments are to be considered io in all respects only as illustrative and not restrictive, and the scope of the invention is, therefore, indicated by the appended claims rather thn by the foregoing descriptin. All changes which come i r-ir tne meaning and range of equivalency of the claims are to be erbraced within their scope.

Claims (31)

1. A chewing gum base',' comprising: about
5-95% by weight elastomer; o to about, 45%- by weight elastomer plasticizer; o to about 30%- by weight wax; about 1-60% by weight filler; and ~about 0.5-40% by weight s~ftener/emu-sai-,er '0 about 7 to about 2000 ppm antioxidant; wherein the amount of antioxidant in the gum base is at least about two-thirds of the amount ofE antioxidant initially added during manufacture the gum bDase. i52. The chewi~ gC um bDase of7 claim1,<hri
7- LfC Z case. w~ ~Gu b Ceofclaim, n :e-c an:ioxidan: ceig gu bseo claim 3, r 6. criewing gum base of.L claim 3, whre-the a2oia.t cOMMcQrise E:KT and iA 7. The chewing gum base of claim 1, wherein the 3, antioxidant is pre sent at about 27 to about iooo ppm of the gum base. I 30
8. A chewing gum including the chewing gum base of claim 1.
9. A chewing gum, comprising: about 5-95% by weight chewing gum base; about 5-95% by weight bulk sweetener; about 0.1-15% by weight flavoring agent; and about 1-1000 ppm antioxidant contributed by the chewing gum base; wherein the amount of antioxidant present in to the chewing gum is at least about two-thirds of the amount of antioxidant added during manufacture of the -ase. The chewing cum of claim 9, wherein the amount of antioxidant presen: in the chewinc Cu is at S least about hree-out hre urths of the amount of anticxidant added during manufacture of the gum nase.
11. The chewing cum of claim 9, wherein the an cxaidant comprises a synthetic antioxidant selected from the croup consisting of EA., E.T, TBHQ, propyl o gallate, and combinations thereof.
12. The chewing gum of claim 11, wherein the antioxidant comprises BHT.
13. The chewing gum of claim 11, wherein the antioxidant comprises BHA.
14. The chewing gum of claim 11, wherein the antioxidant comprises BHT and BHA. The chewing gum of claim 9, wherein the antioxidant is present at about 8 to about 300 ppm of the chewing gum. 31
16. A method of making a chewing gum base, comprising the 'steps of: adding, to a continuous mixer, about 5-95% by weight elastomer, 0 to about 45% by weight elastomer i plasticizer,' 0 to about 30% by weight wax, about 1-60% by weight filler, about 0.5-40% by weight softener/emulsifier, and about 10-2000 ppm antioxidant; and blending the ingredients together in the t continuous mixer to form a gum base; wherein the amount of antioxidant preset in the gum base is at least about two-thirds of the amount of antioxidant added to the continuous mixer.
17. The method of claim 16, wherein the continuous mixer comprises a blade-and-pin mixer.
18. The method of claim 16, wherein the cninucus mixer comprises a corotating twin-screw extruder.
19. The me:hod of claim 16, wherein the S cntinu-.s mixer comprises a counterrotatinw twin-screw The method of claim 16, wh rein the amout of ari:zoxican: present in the cum base is at least about :hree-fourths of the amount of antioxidant added to the *d continuous mixer.
21. The method of claim 16, wherein the antioxidant comprises a synthetic antioxidant.
22. The method of claim 21, wherein the antioxidant comprises BHT. i 32
23. The method of claim 21, wherein the antioxidant comprises BHA.
24. The method of claim 21, wherein the antioxidant comprises BHT and BHA. An integrated method of making stabilized gum base and chewing gum, comprising the steps of: preparing stabilized gum base in a continuous mixer using an amount of antioxidant initially added to the continuous mixer; 1o adding sweetener, softener and flavor to the gum base in the continuous mixer; and mixing the sweetener, softener an iflavor with the stabilized gum base in the continuous mixer provide stabilized chewinc gum; -1 whereir the s abilized chewing gum includes at least about two-thirds of the amount of antioxidant initially added to the continuous mixer.
26. The method of claim 25, wherein the stabilizer chewing gum includes at least about three- 2 fourths of the amount of antioxidant initially added to the continuous mixer.
27. A method of continuously making gum base having about the same level of antioxidant present in a base prepared using a batch process but less degradation products, comprising the steps of: determining a target amount of antioxidant desired in a gum base after manufacture of the base; estimating a percentage of antioxidant loss expected during continuous manufacture of the base, the loss being less than would be expected from a batch manufacturing process; -33 determining a starting level of antioxidant from the target amount and the percentage loss expected during continuous manufacture of the base; and manufacturing the gum base in a continuous mixer using the determined starting level of antioxidant; wherein the starting level of antioxidant is less than would be needed to achieve the same target level of antioxidant if the batch manufacturing process to were used.
28. The method of claim 27, wherein the continuous mixer comprises a blade-and-pin mixer.
29. The method of claim 27, wherein the continuous mixer c c-prises a corotating twir screw i S extruder. The method of claim 27, wherein the continuous mixer com rises a counterrotating twin screw extruder.
31. The method of claim 27, wherein the 3 ccr:inuous mixer comprises a single screw extruder
32. The method of claim 27, wherein the taroet a.ount of aJ.ioxidan:- is a: least about two-thirds of tne starting amount for continuous manufacture of the gum base.
33. The method of claim 27, wherein the target amount of antioxidant is at least about three fourths of the starting amount for continuous manufacture of the gum base.
34. A chewing gum product prepared according to 3o the method of claim i. 34 A chewing gum product prepared according to the method of claim 26.
36. A chewing gum base prepared according to the method of claim 27.
37. A chewing gum base prepared according to the method of claim 33.
38. A chewing gum base prepared by a continuous mixing process, which comprises a lower level of antioxidant degradation product than a gum base of the 1o same essential composition prepared by a batch mixinz
39. The cum base of claim 38 wherein the a.tioxican-: deradation product is selected fror the grou consisting of complex furans, biphenyl compounds, and mixtures thereof. A chewing gum product prepared according to a interated method fcr making chewing gum base and cnewing gum product in a single continuous mixer, which comprises a lower level of antioxidant degradation do product than a chewing gum of the same essential composition prepared using separate mixers for the gum base and chewing gum.
41. The chewing gum product of claim 40, wherein the antioxidant degradation product is selected from RC the group consisting of complex furans, biphenyl compounds, and mixtures thereof.
42. A chewing gum product prepared according to an integrated method for making chewing gum base and chewing gum product in a single continuous mixer, which comprises a lower level of antioxidant degradation .1 a b 35 product than a chewin- (gum of the same essential c.ompos-it-on prepared sn a gum base made ina sco-arate batch mixer. 432 The qhwn um zrod4uct of clai 42 -Lae2- S te a n ic: :da- der a deia-C'- 0r6uc C C1t' 2c: the cofls-'S z: Or C 07 u ran~ S IhZi; rmoncS a no- -xures zt-ereo: Dated 10 May, 2002 Win. Wrigley Jr. Company o Patent Attorneys for the Applicant/Nominated Person SPRUSON FERGUSON
AU40587/02A 1994-09-13 2002-05-10 Reduced antioxidant gum base and method of preparation Ceased AU775609B2 (en)

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US361776 1994-12-22
AU57166/99A AU5716699A (en) 1994-09-13 1999-11-01 Reduced antioxidant gum base and method of preparation
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Free format text: IN VOL 18, NO 30, PAGE(S) 852 UNDER THE HEADING APPLICATIONS ACCEPTED - NAME INDEX IN THE NAME OF WM. WRIGLEY JR. CO., SERIAL NO. 775609, INID (54), AMEND THE TITLE TO READ REDUCED ANTIOXIDANT GUM BASE AND METHOD OF PREPARATION