CN1736237A - Degradable chewing gum substrate and preparation method thereof - Google Patents
Degradable chewing gum substrate and preparation method thereof Download PDFInfo
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- CN1736237A CN1736237A CN 200510043167 CN200510043167A CN1736237A CN 1736237 A CN1736237 A CN 1736237A CN 200510043167 CN200510043167 CN 200510043167 CN 200510043167 A CN200510043167 A CN 200510043167A CN 1736237 A CN1736237 A CN 1736237A
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- chewing gum
- lactic acid
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Abstract
The invention provides a process for preparing gum base for chewing gums by using lactic acid as raw material through melting and compensating, the process comprises seasoning the lactic acid, decompressing and dewatering, carrying out condensation reaction to form resin compound, which has lower glass transformation temperature and faster degradation speed.
Description
Technical field
The invention belongs to technical field of macromolecules, relate to a kind of preparation of degradable chewing gum substrate, relate in particular to a kind of environment-friendly type degradable chewing gum base that utilizes lactic acid directly to be polymerized.
Background technology
Chewing gum claims glue relation by marriage sugar again, it is a kind of candy with anti-chewiness, it is except containing the composition that can Gong digest and assimilate, the viscoplasticity of chewing gum base also contains the matrix matrix of chewing, owing to can be removed the bacterial plaque attached to the tooth laminar surface, thereby the generation of caries prevention, can also temper simultaneously the function of chewing of human body, eliminate fatigue, functions such as brain-nourishing refreshing.Chewing gum often is used as oral health or habit-breaking candy for smokers in addition.The kind of chewing gum can be divided into sheet by shape, and fruit is granular, and sandwich shape is wrapped sugared shape; Can be divided into refrigerant chewing gum, tens kinds such as fruit-flavored chewing gum by batching.General gum components contains water-soluble major constituent, water-insoluble chewing gum base, water-insoluble aromatic.The water-insoluble chewing gum base generally contains elastomer, resin compound, fat and oil, wax, emulsifying agent, softening agent and inorganic filler etc., wherein resin compound help preparing needs chew attribute and as the elastomeric plasticizer of chewing gum base component.The prescription of chewing gum base commonly used is: butyl rubber 16%, and natural rubber 8%, polyvinyl acetate 30%, natural gum are 18%, calcium carbonate is 10%, tristerin 8%, micro-crystallization wax 4%.The matrix of conventional chewing gum is pasted on any dry surface easily, as wood, concrete, paper and cloth.When matrix during by inappropriate abandoning, be difficult to be removed, and in several years, all can not degrade from above-mentioned surface, be unfavorable for environmental protection, urban environment has not only been polluted in accumulating in a large number of it, also is the carrier of disease propagation.
Above-mentioned effects limit the sale and the use value of chewing gum.Therefore need a kind of chewing gum that absorbs of exploitation, or prepare a kind of removing easily or degradable matrix.Compare with the soft elastomer of using in the common chewing gum, typical absorbable polymer is a rigidity, and as protein and polysaccharide, so elastomer is chewed in its uncomfortable cooperation.In addition, under the situation that plasticizer such as water, ethanol, propane diols, polyalcohol exist in a large number, some protein close polysaccharide and become flexible when body temperature.On the other hand, some other absorbable polymer as starch, albumin, globulin, because its polar structure, has the tendency of rapid dissolving or dispersion in the chewer mouth.Therefore such absorbable polymer can not stand to chew for a long time.Water-soluble absorbable polymer such as prolamin, has been used to absorb the research of chewing gum manufacturing prescription.Yet great majority are the prolamin solvents effectively, as ethanol and polyalcohol, still are water-soluble or can disperse in water.Therefore, they can be extracted out when chewing.Prolamin, as the matter of zein, the ethanol plasticizer chew separate out after, it becomes hard.Therefore, need the water-insoluble plasticizer to keep the quality of its softness when chewing.Under the situation that a large amount of emulsifying agents exist, be above-mentioned purpose, need to use lipid, as beeswax, candelila wax, fat.
The chewing gum that contains prolamin and zein uses or is suggested.As see United States Patent (USP) 2154482,2469861,2489147,5482722 and 5112625.Yet from the angle of chewing gum, these products are also not exclusively satisfactory.
U.S. Pat 5672367 discloses, and chewing gum can prepare with some synthetic polymer, has the key of chemically unstable in their polymeric chain, can disconnect under the influence of light, or be degraded into water-soluble nontoxic component.The chewing gum that this patent is invented contains at least a degradable polyester polymers, and it is by cyclic ester, such as handing over the polymerisation of fat, glycolide, trimethylene carbonate, caprolactone to obtain based on third.This invention is also mentioned, and can degrade in environment with the chewing gum that these polymer are made.
U.S. Pat 6153231 discloses, the copolymer of poly lactic acid that degradable chewing gum base contains is selected from poly-(third hands over resin acid-dimer-aliphatic acid-azoles quinoline) copolymer and poly-(lactic acid-glycol-urethane) copolymer.U.S. Pat 5672367 has usually been described the polyester polymers of cyclic ester polymer manufacture.Clearly disclosed a kind of by D, the copolymer that L-third hands over fat and 6-caprolactone to form, its glass transition temperature is 15 ℃.And the present inventor also finds, natural resin ratio of component such as natural sobrerone ester can be replaced with by D the biodegradable block copolymer that L-third hands over fat and 6-caprolactone to form.Known natural resin basic non-degradable in environment.Because they generally account for the 10-50% of chewing gum base composition gross weight, this component replaces with the degradability that degradable components can significantly provide chewing gum base in the chewing gum base.Given this, the present invention attempts the PLA that obtains with the lactic acid direct polycondensation matrix as chewing gum, the exploitation environmentally friendly chewing gums.
Summary of the invention
The objective of the invention is to propose a kind of method of utilizing the direct polymerization of lactic acid to prepare the environment-friendly type degradable chewing gum base.
Processing step of the present invention is:
1. lactic acid being carried out drying handles: add molecular sieve drying more than 24 hours in lactic acid;
2. dehydration: the lactic raw material that drying is handled is 2-8 hour decompression dehydration time under temperature 40-100 ℃, the condition of vacuum 10-200mmHg; More excellent dehydration temperaturre is 50-80 ℃, dewaters under this temperature, and dewatering speed is fast, and can make lactic acid do not taken away, and can prevent the polymer variable color.
3. polymerization: will be under 100-180 ℃ the condition through the lactic acid of dehydration in temperature, polymerisation 4-14 hour the mylar compound.
4. acetone solution is used in mylar compound cooling back, use precipitation with alcohol again, vacuum drying gets degradable chewing gum substrate then.
The 1. described lactic acid of step is D, any monomer in L-lactic acid, D-lactic acid, the L-lactic acid.
The 3. described polycondensation reaction of step can be carried out under the effect of non-toxic catalyst, and the addition of catalyst is the 0.1-0.3% of lactic raw material weight.
Described catalyst is FeCl
3Or AlCl
3Or the Al that supports of Zn powder or palygorskite, or the Fe that supports of palygorskite.
Step 4. in the mylar compound with acetone solution after, can use precipitation with alcohol earlier, use the distilled water reprecipitation again, carry out vacuum drying at last and get degradable chewing gum substrate.
By the chewing gum base polyester of method for preparing, its glass transition temperature is 16-50 ℃.
The present invention compares in prior art and has the following advantages:
1, the present invention utilizes the lactic acid direct polycondensation to be prepared from resin compound, has as necessary resilient flexible of chewing gum base and the anti-performance of chewing, because its glass transition temperature is low, degradation speed is very fast, is a kind of chewing gum base of environment-friendly type.
2, the present invention is raw material with lactic acid, and technology is simple, easy to operate, with low cost, and the productive rate height helps suitability for industrialized production.
3, the present invention prepares under without catalyst or the condition at non-toxic catalyst, safety non-toxic, the PLA vitrification point for preparing suitable (for 16-50 ℃).
The specific embodiment
Embodiment 1:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 40 ℃, vacuum is to stir decompression dehydration 4 hours under the 40mmHg condition;
3. continue to be warming up to 180 ℃, make lactic acid polymerizes reaction 6 hours, form the mylar compound;
4. acetone solution is used in resin compound cooling back, and use precipitation with alcohol,, obtain vitrification point and be 25 ℃ chewing gum base then 36 ℃ of vacuum drying.
Embodiment 2:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 40 ℃, vacuum is to stir decompression dehydration 4 hours under the 40mmHg condition;
3. add 0.05g FeCl
3Catalyst continues to be warming up to 120 ℃, makes the lactic acid polymerizes reaction form the mylar compound in 6 hours;
4. with resin compound cooling back acetone solution,, precipitate with distilled water again,, obtain vitrification point and be 18 ℃ chewing gum base at last 36 ℃ of vacuum drying earlier with behind the precipitation with alcohol.
Embodiment 3:
1. be to add molecular sieve drying in 85% the L-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 50 ℃, vacuum is to stir decompression dehydration under the 60mmHg condition about 3 hours;
3. continue to be warming up to 140 ℃, make the lactic acid polymerizes reaction form the mylar compound in 6 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 20 ℃ chewing gum base 36 ℃ of vacuum drying.
Embodiment 4:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 50 ℃, vacuum is to stir decompression dehydration 3 hours under the 60mmHg condition;
3. add 0.05g AlCl
3Catalyst continues to be warming up to 140 ℃, makes the lactic acid polymerizes reaction form the mylar compound in 8 hours;
4. with resin compound cooling back acetone solution, use earlier precipitation with alcohol, precipitate with distilled water again,, obtain vitrification point and be 32 ℃ chewing gum base at last 36 ℃ of vacuum drying.
Embodiment 5:
1. at D, add molecular sieve drying in the L lactic acid more than 24 hours;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 60 ℃, vacuum is to stir decompression dehydration 2 hours under the 80mmHg condition;
3. add 0.08g AlCl
3Catalyst continues to be warming up to 160 ℃, makes the lactic acid polymerizes reaction form the mylar compound in about 9 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 38 ℃ chewing gum base 36 ℃ of vacuum drying.
Embodiment 6:
1. be 85% D in purity, add molecular sieve drying in the L lactic acid more than 24 hours;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 70 ℃, vacuum is to stir decompression dehydration 5 hours under the 80mmHg condition;
3. add 0.10g AlCl
3Catalyst continues to be warming up to 170 ℃, makes the lactic acid polymerizes reaction form the mylar compound in 10 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 45 ℃ chewing gum base 36 ℃ of vacuum drying.
Embodiment 7:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 80 ℃, vacuum is to stir decompression dehydration 6 hours under the 90mmHg condition;
3. add 0.08g
ZnThe powder catalyst continues to be warming up to 180 ℃, makes the lactic acid polymerizes reaction form the mylar compound in 11 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 18 ℃ chewing gum base 36 ℃ of vacuum drying.
Embodiment 8:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 90 ℃, vacuum is to stir decompression dehydration 4 hours under the 40mmHg condition;
3. add Al that the 0.08g palygorskite supports for the powder catalyst continues to be warming up to 140 ℃, make the lactic acid polymerizes reaction form the mylar compound in 12 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 45 ℃ chewing gum base 36 ℃ of vacuum drying.
Embodiment 9:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 40 ℃, vacuum is to stir decompression dehydration 4 hours under the 40mmHg condition;
3. add Fe that the 0.05g palygorskite supports for the powder catalyst continues to be warming up to 120 ℃, make the lactic acid polymerizes reaction form the mylar compound in 13 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 48 ℃ chewing gum base 36 ℃ of vacuum drying.
Embodiment 10:
1. be to add molecular sieve drying in 85% the D-lactic acid more than 24 hours in purity;
2. get the lactic acid of 50g drying, add 250ml and be furnished with in the three neck round-bottomed flasks of thermometer, water knockout drum, at 40 ℃, vacuum is to stir decompression dehydration 4 hours under the 40mmHg condition;
3. adding the Fe that the 0.1g palygorskite supports is the powder catalyst, continues to be warming up to 180 ℃, makes the lactic acid polymerizes reaction form the mylar compound in 14 hours;
4. acetone solution is used in resin compound cooling back, and with behind the precipitation with alcohol,, obtain vitrification point and be 25 ℃ chewing gum base 36 ℃ of vacuum drying.
Claims (8)
1, a kind of preparation method of degradable chewing gum substrate comprises following processing step:
1. lactic acid being carried out drying handles;
2. dehydration: the lactic raw material that drying is handled is 2-8 hour decompression dehydration time under temperature 40-100 ℃, the condition of vacuum 10-200mmHg;
3. polymerization: will be under 100-180 ℃ the condition through the lactic acid of dehydration in temperature, polymerisation 4-14 hour the mylar compound;
4. acetone solution is used in mylar compound cooling back, use precipitation with alcohol again, vacuum drying gets degradable chewing gum substrate then.
2, the preparation method of degradable chewing gum substrate according to claim 1, it is characterized in that: described lactic acid is D, any monomer in L-lactic acid, D-lactic acid, the L-lactic acid.
3, the preparation method of degradable chewing gum substrate according to claim 1 is characterized in that: step is 1. described carries out drying to lactic acid and is treated to: add molecular sieve drying more than 24 hours in lactic acid;
4, the preparation method of degradable chewing gum substrate according to claim 1, it is characterized in that: step 4. in the mylar compound with acetone solution after, earlier use precipitation with alcohol, use the distilled water reprecipitation again, carry out vacuum drying at last and get degradable chewing gum substrate.
5, as the preparation method of claim 1,2,3,4 described any degradable chewing gum substrates, it is characterized in that: the 3. described polycondensation reaction of step is to carry out under the effect of non-toxic catalyst, and the addition of catalyst is the 0.1-0.3% of lactic raw material weight.
6, as the preparation method of degradable chewing gum substrate as described in the claim 5, it is characterized in that: described catalyst is FeCl
3Or AlCl
3Or the Al that supports of Zn powder or palygorskite, or the Fe that supports of palygorskite.
7, the chewing gum base polyester of method preparation according to claim 1.
8, chewing gum base polyester as claimed in claim 7, its glass transition temperature is 16-50 ℃.
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CNB2005100431677A CN100527977C (en) | 2005-08-25 | 2005-08-25 | Degradable chewing gum substrate and preparation method thereof |
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CNB2005100431677A CN100527977C (en) | 2005-08-25 | 2005-08-25 | Degradable chewing gum substrate and preparation method thereof |
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CN1736237A true CN1736237A (en) | 2006-02-22 |
CN100527977C CN100527977C (en) | 2009-08-19 |
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Cited By (1)
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CN106858026A (en) * | 2017-03-30 | 2017-06-20 | 河源市兴睿食品科技开发有限公司 | Chewing gum that can be digested and preparation method thereof |
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Cited By (1)
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CN106858026A (en) * | 2017-03-30 | 2017-06-20 | 河源市兴睿食品科技开发有限公司 | Chewing gum that can be digested and preparation method thereof |
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