JPS60251846A - Production of gum base - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to techniques for manufacturing chewing gum bases, and more particularly to improved manufacturing methods that allow chewing gum bases to be manufactured more efficiently and with less energy consumption.

BACKGROUND OF THE INVENTION Chewing gums known today include a water-soluble portion that disappears during chewing and a base portion that is insoluble, inert and remains in the oral cavity during chewing. Flavor and sweetness generally derive from the water-soluble portion, while organoleptic properties such as texture, elasticity, film-forming ability, stickiness, and softness typically derive from the base portion. . To obtain the desired properties in a gum product, its specific organoleptic properties,
The base is manufactured using components selected to suit processability and compatibility.

As research continues into the commercialization of new types of gum products, a variety of different base ingredients are being considered to impart novel properties to the final gum product.

As a result, there is an increasing demand for incorporating this new found ingredient in gum base processing. For very hard ingredients, i.e. ingredients that are resistant to partial deformation due to penetration or shear, it is necessary to use relatively high energy methods to crush the material prior to mixing with the other base ingredients. Examples of such materials include hard elastomeric materials, particularly synthetic elastomers such as polyisobutylene, styrene-butadiene copolymers and imbutylene-isoprene copolymers.

Other ingredients that are a little difficult to mix with the gum base ingredients include:
Including, but not limited to, resins such as high and low molecular weight polyvinyl acetate, which provide excellent film-forming properties to the resulting base and final gum compositions.

For example, U.S. Pat. No. 4,187,320 (Kochet et al.
al), a two-step process for producing chewing gum bases using solid elastomers such as butadiene-styrene copolymers, polyimbutylene and inbutylene-isoprene copolymers is disclosed, in which: First, the solid elastomer is highly mixed under high shear stress conditions into a substantially homogeneous, lump-free material;
The elastomer solvent is added in portions to the mixer containing the kneaded solids, followed by the oil-based OT plasticizer in portions. A high degree of mixing is maintained during the gradual addition of the nidistomer solvent and oil plasticizer until a substantially molten homogeneous mass is obtained. The second part of this process
The step is to add in portions the remaining chewing gum base ingredients, such as hydrophobic plasticizers, non-toxic vinyl polymers and other oils, such as primary plasticizers and emulsifiers.

Additional optional ingredients, including fillers, may be added in either the first stage or the second stage, preferably the fillers are added during the second stage as the first component of a typical Kn second stage.

Further in this regard, U.S. Pat. No. 3,995,064 (EhrgOtt et al.) discloses a batch or continuous process for producing chewing gum bases, which involves subjecting chewing gum elastomers and solvents to high shear conditions. τ to form a first dry solid mixture, and this first dry solid mixture is mixed with a hydrophobic plasticizer and a hydrophilic plasticizer under high folding action under low shear conditions. This second mixture is then mixed with an oil-based plasticizer and an emulsifier under high-speed folding action and substantially no shear to form a chewing gum base. Similarly, US Pat. No. 4,329,369 (T
An interesting method is mentioned in Ezuka et al., in which all the necessary gum ingredients are placed in an intensive mixing device and kneaded until thoroughly mixed. ' has been disclosed.

As mentioned above, these methods require the consumption of a large amount of energy for the preparation and/or mixing of the base components. The obsession with widely practiced mechanical cross-crossing methods is that unraveling the polymeric structure of an elastomer or resin by any other method will cause a reduction in the properties that should be imparted by the use of the elastomer or resin. This is thought to be due to the belief that

SUMMARY OF THE INVENTION The present invention relates to a method of making a gum base having a hard elastomer component, the method comprising: blending a filler with a hard elastomer; mixing a plasticizer with a filler-hard elastomer mixture to loosen the elastomer; The method involves subjecting the plasticized blend to intensive mixing and then adding the remaining desired gum base ingredients.

Additionally, either batch or continuous methods require additional time to cut and loosen the ingredients and mix them until a single, relatively uniform gum penis is obtained. However, according to the present invention, these and other problems that arise during the manufacture of gum bases are greatly improved.

According to the present invention, a gum base is produced containing difficult-to-mix polymeric components, such as hard elastomers, by first mixing such components, preferably in the form of particulates, with filler components, and then mixing the mixture with filler components. After incorporating the plasticizer into the gum base, it is subjected to further processing such as high shear mixing, and further gum base ingredients are added. Preferably, the plasticizer is in liquid form, while the filler may be any mineral adjuvant commonly used in gum bases, such as calcium carbonate (CaC03), MgC
Examples include O3, Al2O3 and talc.

The ratio of plasticizer to hard elastomer component is approximately 0.1:
1.0 to about 3.0:1.0, preferably about 0
．． The ratio is from 25:10 to about 2.00:1.0, most preferably from about 0.5:'1.0 to about 1.0:1.0.

On the other hand, the ratio of filler to hard distomer component is approximately 1
5.0:1.0 to about 1.0:1.0. Be nice,
About 8.0:1.0 to about 2.0:1.0, most preferably about 3.0:1.0.

Advantageously, the hard polyisobutylene elastomer is thus treated with calcium carbonate and fines before introducing the base components and subjecting it to a suitable processing step with the intensive mixing steps and low torque required for high-throughput processed gum bases. Can be mixed with crystalline waxes, thus reducing energy requirements and thus increasing throughput. The overall process is therefore more effective than any other gum-based process known in the art. In fact, in accordance with the present invention, the gum base treatment contains about 0.32 A per pound of product.
mp or less, in most cases about 0 per pound of processed material.
．． Strong mixing is possible below 16 Amp.

Furthermore, since the present invention can be used in both batch and continuous processes, a suitable gum base addition system suitable for obtaining the above-mentioned energy-saving properties can be easily applied.

Next, the present invention will be explained in more detail using the accompanying drawings. FIG. 1 is a schematic flow sheet showing the steps of the present invention. Dashed lines indicate optional additives Typical chewing gum bases are made of natural gums or elastomers, examples of which include natural rubber,
chicle, balata, 5orva, gutta percha, 11chi, caspi and jelutong and/or synthetic gums or elastomers such as polyisobutylene,
Including butylene resin-isoprene copolymer and butylene-styrene copolymer.

Among these, synthetic elastomers, butadiene-styrene copolymers, polyisobutylene, imbutylene-isoprene copolymers, or mixtures thereof are preferred. The elastomer selected is preferably in the form of fine particles, and is By blending Ca
It is mixed with fillers which are inorganic materials such as CO3, MgCO3, Al2O3, talc, etc. This mixture is then mixed with a suitable plasticizer, preferably in liquid form, and then the mixture is introduced into an intensive mixing device, for example at point (2) of the accompanying drawing.

It has been found that oily plasticizers can be used particularly effectively in the process of the invention for further mixing and processing the nidistomers. Oily plasticizers include waxes such as petroleum waxes such as paraffin wax and polyethylene waxes, oily substances such as cocoa butter and hydrogenated vegetable oils. Experience has shown that, for example, the trade names Mobilwax and No(
Bareco wax vc, a commercially available microcrystalline wax, has been found to be particularly effective in the present invention. Other plasticizers include fatty acid esters such as n-butyl stearate, butyl sebacate,
Butyl benzyl monouccinate, butyl oleate, oleic acid, caprylic acid, butyric acid, capric acid, caproic acid,
Mono-, di- or triglyceryl esters of saturated or unsaturated fatty acids such as lauric acid, mineral oils, liquid petroleum hydrocarbons, squalane, squalene, castor oil and other ricinoleic acid ester derivatives, diethylene or propylene glycol and its derivatives, citric acid Tributylacetyl, tributyl citrate, lecithin, coconut oil, glyceryl tributyrate, zinc laurate, calcium stearate, propylene glycol monostearate, f.

Examples include propylene glycol monolaurate, fatty acids, diacetyl tartrate esters of mono-diglycerides of edible fatty oils or edible fat-forming acids, petrolatum, stearyl citrate monoglyceride, limonene, polylimonene, natural waxes, butyl lactate, butyl oleate, etc. .

Prior to the present invention, in practice, liquid elastomer plasticization, which effectively dissociates the intramolecular and intermolecular bonds of the elastomer by "opening up" the elastomer, for further processing in a powerful mixer/grinder; Agent 1-t was said to be unusable because the fractured elastomer would be too "dilute" for processing in intensive mixing equipment.

The present invention solves this problem by incorporating an amount of filler into the plasticized elastomer to impart body to the treated material. As a result of the combination of plasticizer and filler, the hard elastomer component is sufficiently "unraveled" to reduce the energy required for processing in powerful mixing equipment and to facilitate effective processing. Gum base treatment for retaining sufficient body and consistency in the material.

Although not to be limited to any of the foregoing theories, the present invention is believed to result from increased mobility of the hard elastomer macromolecules such that the disentanglement of the liquid V into a near mass. Plasticizers increase the softness, flexibility and elongation of the hard disstomeric component, while decreasing the yield point, elastic modulus and tensile strength. Plasticizers reduce the forces between molecules and allow molecules to move relative to each other. In the technical field of producing gum bases, it is currently believed that "unraveling" by external forces causes irreversible loss in the properties of the polymer. However, the present invention provides sufficient "unraveling" of the hard elastomer fibers for efficient processing without compromising the desired polymeric properties of the gum base product.

In particular, the use of this new method allows the use of highly powerful mixers.
(3) (Baker Perkins MP mixer) power requirements have been reduced by 50%.

The novel process of the invention can be advantageously applied to either batchwise or continuous implementation, with the latter being preferred. After processing with a powerful mixer, the ejected material is processed into a homogeneous rubber product containing no undispersed elastomer particles.
Intermediate mixer (4) (Lyra mixer (R+itz Mi
xer) etc.).

Here, a gum component is further added and mixed with the plasticized elastomer. Intermediate mixers have a large gap between moving surfaces, so they have a small shearing effect and a large bending effect. Examples of pace ingredients that can be added at this point are additional fillers, resins, ester gums and polyethylene, which are typically mixed together in a blender (5) and then mixed with the elastomeric rope. Before this, plasticization is performed as necessary, for example, at point (6) in the figure.

Resins that can be added to the gum base include vinyl polymers, such as polyvinyl acetate, partially hydrolyzed polyvinyl alcohol, vinyl acetate-vinyl laurate copolymers, ethylene-vinyl acetate copolymers, or mixtures thereof; , ester gums include rosin derivatives such as trimerized rosin esters, glycerol esters of polymerized rosins; terpene resins such as polymers of α-pinene or β-pinene. To ensure compatibilization with the elastomer and with each other, suitable plasticizers can be added to the formulation. Glyceryl triacetate (triacetin) has been found to be particularly useful as an effective compatibilizer when high molecular weight polyvinyl acetate is one of the additional base components. Further, known plasticizers that can be used here include esters of rosin and hydrogenated esters of rosin, such as glyceryl esters of hydrogenated rosins and glyceryl esters of partially hydrogenated rosins.

Other special aJ ffl agents include glyceryl tributyrate, trimethyl citrate, benzyl benzoate, benzyl butyrate, cresyl acetate, ethyl acetate, diethyl malonate, diethyl sebacate, ethyl acetoacetate, diethyl tartrate, ethyl lactate. , butyl lactate, acetyl triethyl citrate, diethyl conotate, diethyl oleate, lactic acid, sucrose acetate, diacetyl tartrate of mono- and diglycerides, stearyl monoglyceridyl tartrate, castor oil and other ricinoleic acid esters. derivatives, succinic acid monoglyceride,
Mention may be made of fatty acid raftiric or glyceryl lact esters alone or in combination with acetylated monoglycerides. The type of plasticizer used will of course depend on the nature of the additional ingredients added at this point and the desired consistency and properties of the gum base.

The processed gum product exiting the intermediate mixer (4) is a dough-like substance that can be spread into a uniform film and has no particulate matter.Then, it is passed through the final high-speed mixer (7) (Id
entity Littleford Mixer)
, into which additional base components are introduced at the same time. This high speed mixer provides essentially no shearing action, but a very rapid bending action.

These final groups of ingredients typically include waxes,
Softeners, additional nidistomers and optionally fillers are used. The wax may be the same as the elastomer plasticizer used to prepare the elastomer, and is preferably dissolved in a melter (8) together with the optional plasticizer, softener and additional elastomer; A filler can be added at point (9) in the figure if desired.

As used herein, the term "plasticizer" includes masticating substances that act as softeners; Refers to the same or similar material used in a process.

The various components are generally used in the following weights.

Gum base components Weight percent elastomer relative to gum base 5-15 Nystomer plasticizer 8-15 Filler 5-35 Resin 25-35 Resin 8-15 Wax 0-12 When the base is conditioned by a continuous process, Preferably, each group is blended separately before being fed to each mixing step. However, the components can also be metered into separate V-mixers without being pre-blended. Furthermore, the various mixing operations performed using the mixer after the initial plasticization may be performed with a single variable mixer. In all cases, all blenders and mixers are jacketed and heat can be supplied when necessary to ensure effective mixing, especially at the beginning of the process.

Next, the present invention will be explained in more detail with reference to Examples.

Example 1 Hard polyisobutylene resin granules f are fed to a blender with CaCO3 filler at a rate of 30 bosides/hour and 100 pounds/hour, respectively. The mixed nidistomers/fillers were taken out and placed in an intensive mixer (M, P) with a feed rate of 142 bonds/hour of melted microcrystalline wax at a rate of 130 poside/hour.

Mixer, feeding 100100 rpm.

During this operation, the power requirement of the high-power mixer is 25 Amps.
The operating temperature of the mixer was 340°F. This is 100% without using an elastomer plasticizer.
Over 55 Amp at rpm, about 400°F
Operating temperatures are required, as opposed to energy requirements. Therefore, high-power mixers are typically operated at speeds below 5 Q rpm, but around 60-100 Q rpm.
The process can be operated at rpmVc and thus the gum base throughput can be quite large. The process material exiting the high-power mixer is a smooth, homogeneous rope of rubber-like base material, commonly known as an "eye".
s) Particles called J, that is, discontinuities were not observed.

Example 2 Talc was added as a filler at a feed rate of 99 bonds/hour, and molten microcrystalline wax (Mo'bi1wax) 21°8 poside/hour was added to a high-intensity mixer (M, P, mixer, 1
All other gum bases were prepared in the same manner as in Example 1, except that they were fed at 0100 rpm. □ The amount of electricity required for the strong mixer is 15 to 1
7Ami:I, the operating temperature of the mixer is approximately 340
below °F. The obtained processed product is smooth,
No discontinuities and/or undesirable rubbery particles were observed.

Example 3 In this example, hard polyisobutylene granules't
Feed the blender at 30 lb/hr while Merck is added at a rate of 315 pos/hr. This blended elastomer/filler is fed with 22.5 posides/hour of solid polyethylene microcrystalline wax and 31 pounds/hour of mobile wax into an intensive mixer operating at 1'00 rpm.

As in the previous example, a very favorable gum base rope was obtained at less than 40 Amps during the entire run.

To demonstrate the effectiveness of the present invention when using styrene-butadiene rubber as the hard distomer, the following Examples 4 and 5f were performed, comparing the process of the present invention with a known SDR process. In addition, in the known 8BR process, it was not possible to operate the strong mixer at a speed of 60 rpm or higher.

Example 4 In this example, 8 B Rf CaC0+ is introduced into a blender with a filler at a rate of 100 posides/hour and 400 posides/hour, respectively. This nidistomer/filler is mixed with solid Bareco wax (Bareco wax).
wax) 21.8 poside/powerful mixer over time
(100 rpm).

Soft extruded gum base ropes are produced at about 40 Amps or less. This is in contrast to the past, where intensive mixing of 8BH could not be achieved above about 60 rpm.

Example 5 This example uses an SBR feed rate of 92 lb/hr and a C
a. The production will be conducted at a CO3 supply rate of 149 pounds/hour. The plasticizer, n-butyl stearate, is added to an intensive mixer (100 rpm) at a feed rate of 60 poside/hour and mixed with the filler/elastomer mixture. Good quality extrudates are obtained with only 25 Amps at maximum operation.

It is clear that these examples demonstrate the effects of the present invention, which can be achieved without compromising the quality of the product.

[Brief explanation of drawings]

FIG. 1 is a flow sheet showing the steps of the present invention. The main symbols in the diagram are as follows. 1... Plender, 3 High intensity mixer - 14... Intermediate mixer. Patent Applicant Nahisco Blang Incorporated

Claims (9)

[Claims] (1) Blend the filler with a hard elastomer, mix the filler-hard elastomer mixture with a plasticizer to loosen the elastomer, and subject the plasticized blend to intensive mixing before adding the remaining desired gum base ingredients. 1. A method for producing a gum base having a hard distomer component. (2) The method according to item (1) above, wherein the hard distomer is in the form of fine particles. (3) The hard elastomer is polyimbutylene, iso7'
The method according to item (1) or item (2) above, which is an L/in-butylene copolymer or a styrene butadiene copolymer. (4) The method according to any one of paragraphs (1), (2), and (3) above, wherein the plasticizer is in a liquid state. (5) The plasticizer is n-butyl stearate/oleic acid; mono of saturated or unsaturated fatty acids, oleic acid, caprylic acid, butyric acid, capric acid, caproic acid, lauric acid;
Dimata, liglyceryl esters, mineral oils, liquid petroleum hydrocarbons, squalane, squalene, castor oil and other ricinoleic acid derivatives, diethylene or glopylene glycol and derivatives, tributylacetyl citrate, tributyl citrate, lecithin, coconut oil, Glyseptyl tributyrate, zinc laurate, calcium stearate, propylene glycol monostearate, propylene glycol monolaurate 1, fatty acids, butyl sebacate, butyl benzyl sebacate, edible fatty oil or edible fat-forming acid mono and The above (1) diacetyl tartrate of diglyceride, petrolatum, stearyl citrate monoglyceride, limonene, polylimonene, natural wax, butyl lactate or butyl oleate;
), (2) or (3). (6) The elastomer is polyisobutylene resin and the plasticizer is liquid microcrystalline wax, or the elastomer is a styrene-butadiene copolymer and the plasticizer is n-butyl stearate. Section method/ (7) Full '175E, caco3, MgCO2, Al2
O3'! ft n The method according to any one of the above items (1) to (8), which involves coating with talc. (8) The ratio of plasticizer to hard distomer is approximately 0°1
:10 to about 3.0+1.0, the above-mentioned items (1) to (
7) Any one method. (9) Item (1) above, wherein the ratio of the filler to the hard distomer is about 15°0:1.0 to about 1.0:1.0.
Any one of the methods in paragraph (8). The method of any one of paragraphs (1) to (9) above, wherein the αO intensive mixer is operated at about 60 to about 10 Orpm. 01) The method of any one of paragraphs (1) to 1tO, comprising successive steps in which the additional gum base ingredients are incorporated by a subsequent intermediate intensive mixing step followed by a high speed mixing step.