Method for reducing tempering time of deposited confectionery products

文档序号:862110 发布日期:2021-03-16 浏览:16次 中文

阅读说明:本技术 用于减少沉积型糖食产品回火时间的方法 (Method for reducing tempering time of deposited confectionery products ) 是由 刘京萍 于 2019-07-25 设计创作,主要内容包括:本发明提供了一种制造熔融沉积型糖食产品例如咀嚼胶的方法。在一些实施方式中,通过常规方式混合包含至少一种胶基、风味剂和至少两种糖醇的咀嚼胶组合物。随后将所述咀嚼胶组合物熔融,并沉积到例如在包装泡罩中形成的模具中。随后将沉积的胶在高温下热回火一段时间。热回火过程减少了可以干净地从所述模具中取出沉积的咀嚼胶片并被消费者享用前所需的时间。本发明也提供了所述方法的产品。(The present invention provides a method of making a fused deposition confectionery product such as chewing gum. In some embodiments, the chewing gum composition comprising at least one gum base, a flavor, and at least two sugar alcohols is mixed by conventional means. The chewing gum composition is then melted and deposited into a mold, for example, formed in a packaging blister. The deposited glue is then thermally tempered at an elevated temperature for a period of time. The thermal tempering process reduces the time required before the deposited chew sheet can be cleanly removed from the mold and consumed by a consumer. The invention also provides the product of the method.)

1. A process for producing a chewing gum product, the process comprising the steps of;

a. preparing a chewing gum composition comprising at least one gum base, one flavor, and at least two sugar alcohols,

b. melting and maintaining the chewing gum composition at a temperature sufficient to allow deposition of the chewing gum composition,

c. depositing the molten chewing gum composition,

d. thermally tempering the deposited chewing gum composition at a temperature of at least 25 ℃ for a total tempering time that is reduced by at least 20% as compared to tempering at 20 ℃.

2. The method of claim 1, wherein the total tempering time is reduced by at least 30% compared to tempering at 20 ℃.

3. The method of claim 1, wherein the total tempering time is reduced by at least 40% compared to tempering at 20 ℃.

4. The method of claim 1, wherein the total tempering time is reduced by at least 50% compared to tempering at 20 ℃.

5. The method of claim 1, wherein the total tempering time is reduced by at least 60% compared to tempering at 20 ℃.

6. The method of claim 1, wherein the total tempering time is less than 24 hours.

7. The method according to any one of the preceding claims, wherein the total tempering time is at least 4 hours.

8. The method of any of the preceding claims, wherein the chewing gum composition is thermally tempered at a temperature of at least 30 ℃.

9. The method of any of the preceding claims, wherein the chewing gum composition is thermally tempered at a temperature of at least 35 ℃.

10. The method of any of the preceding claims, wherein the chewing gum composition is thermally tempered at a temperature of at least 40 ℃.

11. The method of any one of the preceding claims, wherein the chewing gum composition is thermally tempered at a temperature within 5 ℃ below the lowest melting point of the saturated fat and/or microcrystalline wax in the chewing gum base.

12. The method of any one of the preceding claims, wherein the tempering occurs at a relative humidity of less than 50%.

13. The method of claim 12, wherein the tempering occurs at a relative humidity of less than 35%.

14. The method of claim 12, wherein the tempering occurs at a relative humidity of less than 20%.

15. The method of any of the preceding claims, wherein the chewing gum composition is thermally tempered for at least 6 hours.

16. The method of claim 15 wherein the chewing gum composition is thermally tempered for at least 8 hours.

17. The method of claim 15 wherein the chewing gum composition is thermally tempered for at least 12 hours.

18. The method of claim 15 wherein the chewing gum composition is thermally tempered for at least 24 hours.

19. The method of claim 15 wherein the chewing gum composition is thermally tempered for at least 7 days.

20. The method of any of the preceding claims, wherein the chewing gum is fully tempered after heat tempering.

21. The method of any one of claims 1 to 19, wherein the chewing gum requires additional tempering at ambient conditions after thermal tempering.

22. The method of any one of claims 1-19, wherein the chewing gum requires tempering at ambient conditions for at least three weeks after heat tempering.

23. The method of any one of claims 1-19, wherein the chewing gum requires tempering at ambient conditions for at least two weeks after heat tempering.

24. The method of any one of claims 1 to 19, wherein the chewing gum requires tempering at ambient conditions for at least one week after heat tempering.

25. The method of any one of claims 1 to 19, wherein the chewing gum requires tempering in the environment until the chewing gum piece can be demolded without distortion or deformation.

26. The method of any of the preceding claims, wherein the chewing gum composition comprises two sugar alcohols.

27. The method of any of the preceding claims, wherein the chewing gum composition comprises three sugar alcohols.

28. The method of any of the preceding claims wherein the chewing gum composition comprises at least one alcohol selected from the group consisting of sorbitol, maltitol, xylitol, mannitol, erythritol, isomalt, and combinations thereof.

29. The method of any of the preceding claims wherein the chewing gum composition comprises a sugar alcohol blend that is a binary blend of xylitol and sorbitol.

30. The method of any of the preceding claims wherein the chewing gum composition comprises a sugar alcohol blend that is a binary blend of xylitol and isomalt.

31. The method of any of the preceding claims wherein the chewing gum composition comprises a sugar alcohol blend that is a binary blend of sorbitol and isomalt.

32. The method of any of the preceding claims wherein the chewing gum composition comprises a sugar alcohol blend that is a binary blend of erythritol and xylitol.

33. The process according to any one of the preceding claims, wherein the two sugar alcohols are present in a ratio of 1:9 to 9: 1.

34. The process according to any one of the preceding claims, wherein the two sugar alcohols are present in a ratio of 1:3 to 3: 1.

35. The process according to any one of the preceding claims, wherein the two sugar alcohols are present in a ratio of 1:2 to 2: 1.

36. The process of any of the preceding claims, wherein the surface on which the molten chewing gum composition is deposited is a conveyor belt.

37. The method of any one of claims 1 to 35, wherein the surface on which the molten chewing gum composition is deposited is a mold.

38. The method of claim 37 wherein the mold into which the molten chewing gum composition is deposited is part of a consumer package.

39. The method of claim 38 wherein the mold into which the molten chewing gum composition is deposited is a blister of a blister pack.

40. The method of any of the preceding claims, wherein the chewing gum composition comprises at least one ingredient selected from the group consisting of high intensity sweeteners, encapsulated high intensity sweeteners, colors, emulsifiers, fillers, nutritional supplements, and combinations thereof.

41. A product manufactured according to the method of any preceding claim.

Technical field and background

The present invention relates to confectionery products, such as chewing gums, formed by shaping the product in a molten state. In some embodiments, the mold is part of a product package.

Consumers have enjoyed chewing gums for over a hundred years because they provide flavor and a fresh feeling over an extended period of time and meet the urge of people to chew. There are many forms of chewing gum on the market, but the most popular are sticks, tablets and coated pellets. These forms have the advantage of being easily produced in commercial quantities using high speed forming equipment. However, they can only produce products with limited shape variations. They do not produce complex three-dimensional shapes such as the shape of animals, fruits or other objects.

Traditional chewing gum forms, such as bars and tablets, typically require a period of tempering, such as 24 to 72 hours at ambient conditions, to allow the gum to "set up" and become sufficiently hard to be baled and packaged. Cooling the glue may accelerate such tempering.

Consumers are constantly looking for new confectionery experiences. Products having a three-dimensional shape are attractive and offer the opportunity to manufacture products related to seasonal or special events. Attempts have been made in the past to form chewing gum into three-dimensional shapes, but it is known that such efforts have never resulted in commercially successful products.

It has been proposed that new consumer products can be prepared by depositing molten confectionery products into preformed packaging film sheets that will serve as molds for shaping the deposited sheets. This can be done as a "so-called" blister pack in which a sheet comprising a plurality of blister moulds is covered with a covering material (typically a foil or foil laminate) and then typically further packaged.

One problem with molten confectionery processing is that the product may require a long time to temper, i.e. to reach a final stable texture after forming. Although the product may undergo further processing, such as shipping and further packaging, after cooling for a few minutes, the product may not reach its final intended texture until weeks or even months after cooling to ambient temperature (i.e., about 20 ℃). A long tempering time may result in the product reaching the consumer before it has been tempered and may therefore not provide the best desired texture. For example, it may be too soft and/or lack cohesion. In addition, if the chewing gum is deposited in the blisters of a blister pack, it may be difficult or impossible to cleanly remove the tablet from the blister mold without the composition sticking to the mold or distorting as it is removed.

Attempts to reformulate confectionery products to reduce tempering time can result in products that lack the proper chew texture or have shelf stability or other problems.

There is a need for a method of manufacturing high quality deposited and molded confectionery products with a relatively short tempering time.

Disclosure of Invention

In one embodiment, the present invention provides a method of producing a confectionery product comprising the steps of:

a. preparing a chewing gum composition comprising at least one gum base, one flavor, and at least two sugar alcohols,

b. melting and maintaining the chewing gum composition at a temperature sufficient to allow deposition of the chewing gum composition,

c. depositing the molten chewing gum composition,

d. thermally tempering the deposited chewing gum composition at a temperature of at least 25 ℃ for a total tempering time that is reduced by at least 20% as compared to tempering at 20 ℃.

In some embodiments, thermal tempering reduces tempering time by at least 20% as compared to tempering at 20 ℃. In some embodiments, the tempering time is reduced by at least 30%, or at least 40%, or at least 50%, or at least 60%.

In some embodiments, the confectionery composition as a chewing gum composition is thermally tempered at a temperature of at least 25 ℃, at least 30 ℃, at least 35 ℃, or at least 40 ℃. In some embodiments, the chewing gum composition is thermally tempered at a temperature within 5 ℃ below the lowest melting point of the saturated fat and/or microcrystalline wax in the chewing gum base.

In some embodiments, tempering occurs at a relative humidity of less than 50%, or less than 35%, or less than 20%.

In some embodiments, the chewing gum composition is heat tempered for at least 4 hours, at least 6 hours, at least 8 hours, at least 12 hours, at least 24 hours, or at least seven days.

In some embodiments, the chewing gum composition is heat tempered for less than 10 days, less than 48 hours, less than 36 hours, less than 24 hours, less than 12 hours, less than 8 hours, less than 6 hours, or less than 5 hours.

In some embodiments, the chewing gum composition is heat tempered for a period of time between 2 hours and 24 hours, between 4 hours and 24 hours, between 6 hours and 12 hours, between 36 hours and 48 hours, between 2 days and 7 days, between 7 days and 14 days, between 24 hours and 36 hours, between 12 hours and 24 hours, between 8 hours and 12 hours, or between 6 hours and 8 hours.

In some embodiments, the chewing gum is fully tempered after the thermal tempering. In some embodiments, the composition requires additional tempering at ambient conditions after thermal tempering. In some embodiments, the additional tempering at ambient conditions will be less than three weeks or less than two weeks or less than one week. In some embodiments, the composition is tempered until the product can be demolded without distortion or deformation.

In some embodiments, the composition will need to be tempered at ambient conditions for at least four weeks without a thermal tempering step. In other embodiments, the composition will require tempering at ambient conditions for at least eight weeks or at least twelve weeks without a thermal tempering step.

In some embodiments, the composition will comprise two sugar alcohols or three sugar alcohols. In some embodiments, the composition will comprise at least one alcohol selected from the group consisting of sorbitol, maltitol, xylitol, mannitol, erythritol, isomalt, and combinations thereof.

In some embodiments, the chewing gum composition will comprise a sugar alcohol blend that is a binary blend of xylitol and sorbitol, or xylitol and isomalt, or sorbitol and isomalt, or erythritol and xylitol in a ratio in the range of 1:9 to 9:1, preferably in the range of 1:3 to 3:1 or in the range of 1:2 to 2: 1.

In some embodiments, the mold in which the composition is deposited is part of a consumer package. In some embodiments, the composition is deposited in a blister of a blister pack.

In some embodiments, the composition further comprises at least one ingredient selected from the group consisting of a high intensity sweetener, an encapsulated high intensity sweetener, a color, an emulsifier, a bulking agent, and a nutritional supplement.

The invention also includes products made by any of the above methods.

For non-chewing gum confectionery products (e.g., chewing gum, soft candy, or hard candy) and methods thereof, ingredients specific to the chewing gum described herein (e.g., gum base) can be replaced with ingredients appropriate for the desired confectionery product.

Drawings

Figure 1 is a graph of 5mm and 10mm thick chewing gum pieces and tempering time versus temperature to achieve a minimum acceptable tempering time.

Figure 2 is a graph showing the tempering times to achieve full temper and minimum acceptable temper conditions at 20, 30 and 40 ℃.

Figure 3 is a plot of enthalpy measured at the center and surface of the chew sheet of example 3 after tempering for 0 to 60 days at ambient conditions.

Figure 4 is a plot of the crusting thickness of the chewing gum of example 3 after tempering for 2 to 15 days in refrigerator, ambient and oven conditions.

FIG. 5 is a graph comparing the crusting thickness of the chewing gum of example 2 after tempering for 2 days and 7 days in refrigerator, ambient and oven conditions.

Fig. 6A-C are photographs of bisected chew films of example 3 showing the formation of crusts after 7 days of tempering under refrigerator, ambient and oven conditions.

Detailed Description

The present invention is based on the following findings: when held at elevated temperatures, the deposition formed product actually tempers faster. It is believed that the mechanism of tempering chewing gum products is the formation of large crystals in the gum mass. To form such large crystals, the small crystals need to migrate within the micelle to attach to the already formed larger crystals (without being bound by theory). (the presence of gum base in the composition limits the temperature at which the composition can melt due to potential degradation of the gum base components.) the ability of small crystals to migrate and thus the rate of tempering depends on the viscosity of the mass, which in turn depends on the temperature. Thus, an increase in the chewing gum deposition temperature reduces the tempering time required, as opposed to what might be expected.

Typically, the tempering time decreases logarithmically with increasing temperature up to a temperature of about the melting point of the saturated fat and/or microcrystalline wax in the gum base. These fats and waxes usually melt in the range of 50 to 60 ℃. The thermal tempering temperature can thus be chosen to be just below the melting point of the lowest melting of the fully hydrogenated fat or microcrystalline wax, for example 10 ℃ or 5 ℃ or 3 ℃ or even 1 ℃ below this temperature.

In practice, it is often not necessary to temper the product completely before shipping. This is because the product will continue to temper as it is transported through the dispensing system. It is important that the product is completely or almost completely tempered when it is received by the consumer. At least, the product should then be tempered sufficiently so that it can be easily removed from the packaging mould without distorting the shape of the product or leaving any visible residue on the mould. The product should also be sufficiently close to its fully tempered texture that it is acceptable and not significantly different from the intended final texture. Figure 1 shows a plot of tempering time versus temperature for 5mm and 10mm thick chewing gum pieces and for achieving a minimum acceptable tempering time. Figure 2 shows a graph of the tempering times to reach full temper and minimum acceptable temper conditions at 20, 30 and 40 ℃.

Thus, when the product will be fully tempered after a period of time, e.g. two, three, four or six weeks, in which the tempering is adapted to the dispensing speed under ambient conditions, the thermal tempering can be interrupted and the product can be transported.

The integrity of the temper can be measured in several ways. The quick test is simply removing the sheet from the mold. The fully tempered product will be easy to remove leaving no visible residue on the mould. The demolded sheet will not exhibit distortion, deformation, or cracking. A sheet exhibiting only small cracks is close to being fully tempered.

Another way to determine the degree of temper is to look at the crust thickness. As the product is tempered, encrustations of tempered material begin to form on the outer surface of the sheet and steadily thicken until the entire sheet is tempered. The crust can be seen and measured by cutting the sheet in half. In connection with the testing of the examples, an accurate method of measuring the crusting and thus determining the progress of the tempering using TMA was described.

Chewing gums generally comprise a water-insoluble gum base portion and a water-soluble portion containing sweeteners, flavors, and other ingredients. Any chewing gum base and chewing gum formulation can be used in the chewing gum of the present invention.

The insoluble gum base may generally comprise any combination of elastomers, vinyl polymers, elastomer plasticizers, fillers, softeners, waxes, and other optional ingredients such as colorants and antioxidants. The various gum base ingredients commonly used provide the ability to alter the chewing characteristics of gums made from the gum base.

Elastomers provide the glue with elastic, cohesive properties that vary depending on the chemical structure of the component and how it is compounded with other components. Natural elastomers may include natural rubbers such as smoked or liquid latex and guayule, natural gums such as jelutong (jelutong), lechi caspi (lechi caspi), perrilol (perrilo), masasa blue bablata (massarandubaba balata), masasa blue baboo (masasaranduba chocolate), nisoba (nispero), ross gha (rosidinha), erythro (chicle), tagoka (gutta percha), gutta percha (gutta kataiu), nile gutta (niger gutta), tara (tenu), gutta (chilte), erythroqueba (chiquigel), gutta hand (hypertang). Synthetic elastomers may include high molecular weight elastomers such as butadiene-styrene copolymers and isobutylene-isoprene copolymers. Other polymers sometimes used as elastomers include polybutadiene and polyisobutylene, vinyl polymers (e.g., polyvinyl acetate, polyethylene), vinyl copolymer elastomers (e.g., vinyl acetate/vinyl laurate, vinyl acetate/vinyl stearate, ethylene/vinyl acetate), polyvinyl alcohol, or mixtures thereof. These polymers perform best when used in combination with butadiene-styrene copolymers and isobutylene-isoprene copolymers.

Vinyl polymer and copolymer type elastomers provide block resistance, modify the chewing characteristics of gums made from these gum bases, and provide hydrophilicity which is beneficial to the sensory perception of the final gum. For copolymer types, the amount of vinyl laurate, vinyl stearate, or ethylene present in vinyl laurate/vinyl acetate (VLNA), vinyl stearate/vinyl acetate (VSNA), or ethylene/vinyl acetate (EVA) copolymers, respectively, is typically in the range of about 10% to about 60% by weight of the copolymer. The average molecular weight of these polymers may range from about 2,000 to about 80,000. The spherical and ring softening points of these polymers may be in the range of about 50 to 120 ℃. Polyvinyl acetates having average molecular weights of from about 8,000 to about 52,000 are preferably used in the gum bases and gums of the present invention. More preferred for chewing gum bases are those having a molecular weight of about 10,000 to about 35,000, and more preferred for bubble gum bases are those having a molecular weight of about 30,000 to about 60,000. Vinyl polymers generally release flavor rapidly, and use of isoparaffin waxes exhibiting a small crystal structure with these vinyl polymers can prolong flavor release.

Petroleum waxes aid in the solidification of the finished gum made from the gum base and improve shelf life and texture. The hard wax crystal size also improves flavor release. The crystal size of those waxes having a high content of isoparaffins is smaller than the crystal size of waxes having a high content of normal paraffins, in particular those having a carbon number of less than 30. Smaller crystal sizes allow for slower flavor release due to the greater resistance to flavor escape from such waxes as compared to waxes having larger crystal sizes.

Synthetic waxes are produced by atypical petroleum wax production means. Synthetic waxes may include waxes containing branched alkanes and copolymerized with monomers such as, but not limited to, propylene and polyethylene and Fischer-Tropsch type waxes. Polyethylene waxes are not in the same class as polyethylene (a polymer of ethylene monomers).

Elastomer solvents (sometimes referred to as elastomer plasticizers) alter the hardness of the gum base. When used in gum bases, their specificity for the intermolecular chain cleavage (plasticization) of the elastomer and their varying softening points can lead to varying degrees of hardness in the finished gum. It is also important when one wishes to expose more of the elastomeric chains of the alkyl chain provided to the wax. Elastomer solvents include natural rosin esters such as glycerol esters of partially hydrogenated rosin, glycerol esters of polymerized rosin, glycerol esters of partially dimerized rosin, glycerol esters of tall rosin, pentaerythritol esters of partially hydrogenated rosin, methyl esters of partially hydrogenated rosin, pentaerythritol esters of rosin, synthetic elastomer plasticizers such as terpene resins derived from alpha-pinene, beta-pinene, and/or d-limonene, and mixtures thereof. The elastomer solvent used may be one kind or a combination of one or more kinds. Generally, the ratio of one to the other depends on the respective softening point, the respective effect on flavour release and the respective degree of stickiness they cause to the glue. The spherical and ring softening points of the rosin esters described above may be in the range of about 60 to about 120 ℃. The terpene resin may have a softening point in the range of about 60 to about 130 ℃ and an average molecular weight of about 500 to 2,000. In some cases, both terpenes and rosin ester resins can be used together.

Softeners modify the texture, make the hydrophobic and hydrophilic components of the gum base miscible, and may also plasticize the synthetic elastomer of the gum base. Softeners include the fully hydrogenated oils of cottonseed, soybean, palm kernel, coconut, safflower, and the like, as well as monoglycerides, diglycerides, acetylated monoglycerides, distilled monoglycerides and diglycerides, and de-oiled or "powdered" lecithin. The glycerides and lecithins are sometimes referred to as emulsifiers.

Fillers used in gum bases modify the texture of the gum base and aid in processing. Fillers include carbonate or precipitated carbonates such as magnesium and calcium carbonate, ground limestone and silicates such as magnesium and aluminum silicate, clay, alumina, talc, and titanium oxide, mono-, di-and tri-calcium phosphate, cellulosic polymers such as ethyl cellulose polymer, methyl cellulose polymer and lignocellulose polymer, or mixtures thereof.

Other optional ingredients such as antioxidants and colorants may also be used in the gum base. Antioxidants extend the shelf life and storage of gum bases, finished gums, or their respective components, including fats and flavor oils. Antioxidants suitable for use in the gum base or gum of the present invention include Butylated Hydroxyanisole (BHA), Butylated Hydroxytoluene (BHT), beta-carotene, tocopherols, acidulants such as vitamin C, propyl gallate, other synthetic and natural antioxidants or mixtures thereof in free-flowing ground or comminuted form.

The soluble portion of the chewing gum is comprised of flavoring agents (including sensates such as physiological cooling agents, warming agents, and stinging agents), bulking agents (also known as bulk sweeteners), high intensity sweeteners, colors, acidulants, fillers, emulsifiers, water soluble softeners, and binders.

High intensity artificial sweeteners may also be used alone or in combination with the above. Preferred sweeteners include, but are not limited to, sucralose, aspartame, N-substituted APM derivatives such as neotame, salts of acesulfame, alitame, saccharin and its salts, cyclamic acid and its salts, glycyrrhizin, dihydrochalcones, thaumatin, monellin, stevia, and the like, used alone or in combination. In order to provide longer lasting sweetness and flavor perception, it may be desirable to encapsulate or control the release of at least a portion of the artificial sweetener. Techniques such as wet granulation, wax granulation, spray drying, spray cooling, fluid bed coating, coacervation, and fiber extrusion can be used to achieve the desired release characteristics.

Various flavoring agents may also be used if desired. The flavoring may be used in an amount of about 0.1% to about 15% by weight of the gum, and preferably about 0.2% to about 5% by weight. 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, wintergreen, anise, and the like. Artificial flavors and ingredients may also be used. Natural and artificial flavors may be combined in any sensorially acceptable fashion. Included in the general class of flavoring agents are sensates, chemicals that impart a physiological sensation in the mouth, such as cooling agents, warming agents, and stinging agents. Examples of cooling agents include menthol, WS-23, WS-3, WS-5, isopulegol, esters of menthol such as menthyl succinate, menthyl lactate, menthyl glutarate, and the like. Warming and stinging agents include capsaicin, piperine, jambu, and spilanthol.

In the case of non-chewing gum confectionery products, any of the ingredients typically used in these products may be used in the methods and products of the present invention.

Detailed Description

Examples 1 to 3

Chewing gum samples were made according to the formulation in table 1 and the following method.

The gum base was heated in an oven at 70 ℃. After thawing, the gum base, powdered sugar alcohol, softener and humectant were mixed in a Sigma Blade mixer at 55-60 ℃ until a gum mass was formed. Flavor, high intensity sweetener, and antioxidant were added and mixed until homogeneous for a total of about 14 minutes. The mixed gum was removed from the mixer. At this point, the gum may optionally be tableted or granulated. The gum at about 55 ℃ was introduced into a six-zone Clextral BC21 extruder as per table 2.

The molten gel was deposited into both the silicone mold and the PVC blister sheet. The sample in the silica gel mold was placed in a high barrier packaging (HBO) bag and the PVC blister was sealed with aluminum foil.

The samples were then aged under the following three conditions: refrigerator (3-10 ℃), ambient (20-23 ℃, 20% RH) and oven (26-28 ℃, 44% RH). Samples were taken on days 1, 2, 7, 9, 12, 15 and 30 for DSC and TMA testing.

Melting point and crystallinity measurements

The Discovery DSC (differential scanning calorimetry) system was operated to test samples under the following methods:

sample pan and lid: tzero discs and Hermetic covers;

heating rate: 20 ℃/minute;

and (3) circulation: heating-cooling-heating;

temperature range: -85 ℃ to 180 DEG C

Relative crystallinity (melting enthalpy after melt extrusion/melting enthalpy before melt extrusion (%)

Crust thickness measurement

The thickness of the crust was measured according to the following procedure using a Mettler Toledo TMA/SDTA2+ with internal cooling temperature control.

The sample pairs were half cut and the soft center portion carefully removed with a mini wooden spatula. The remaining hard crusts were cut into squares of 2x2 mm. The instrument was run for 5 minutes at 25 ℃ in isothermal creep test mode with 0.02N load. This is basically a method of accurately measuring the thickness of the crust.

The enthalpy results for tempering at ambient conditions (20-22 ℃) for example 3 are shown in FIG. 3. The center material and the surface material were tested separately to show faster crystallization at the surface (where the crust started to form) and the center (last crystallization). Figure 4 shows a crusting thickness plot for the chewing gum of example 3 after tempering for 2 to 15 days in refrigerator, ambient and oven conditions. FIG. 5 shows a comparative plot of crusting thickness for chewing gum of example 2 after tempering for 2 days and 7 days in refrigerator, ambient and oven conditions

TMA measurements of the crust thickness of example 3 are shown in table 3. It can be seen that the crust thickness grows 33% faster with the heat treatment at 26-28 ℃ compared to ambient tempering. Photographs of the tempered samples (fig. 6A-C) show that the heat treated samples have been substantially fully tempered, while the other two samples tempered in the refrigerator and ambient conditions were only partially tempered.

The crust thickness of example 1 as measured by TMA is shown in table 4. The samples were demolded after 15 days tempering in a refrigerator and ambient conditions, and the results are described in table 4. The heat-tempered product was demolded on day 7, but had a thicker crust and did not deform upon demolding. These results indicate that thermal tempering reduces tempering time by more than 50%.

Example 4 surface tension Effect

The molten gum samples were deposited on molds made of silicone rubber, polyethylene terephthalate (PET), and aluminum, respectively. As shown in Table 5, all samples were tempered for a period of time at ambient conditions (20-23 deg.C, 20-40% RH). The sample in the silica gel mold formed a thicker crust than the crust formed on the sample in the PET mold, which was thicker than the crust formed on the sample in the aluminum dish. The sample in the aluminum dish was still sticky and could not be demolded.

Literature data, Van Krevelen, d.w. & Nijenhuis, k.te. polymer properties, page 235 (Elsevier, 2009); mark, j. handbook of physical properties of polymers, page 670 (AIP press, 1996).

In order to shorten the tempering time, preferably a low surface tension material (e.g. less than 35mN/m, less than 30mN/m or less than 25mN/m) is used as the molding device or as a coating on the surface of the molding device. These materials include, but are not limited to, aliphatic hydrocarbon polymers or oligomers, aliphatic polyesters or polyethers, silicones, fluoropolymers such as polytetrafluoroethylene, polypropylene, polyethylene, polydimethylsiloxane, polyoxyisobutylene, polyoxypropylene, vinyl polyoctoate, and combinations thereof.

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