CN102742761A - Erythritol crystal and preparation method of erythritol crystal - Google Patents

Erythritol crystal and preparation method of erythritol crystal Download PDF

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CN102742761A
CN102742761A CN2012102425863A CN201210242586A CN102742761A CN 102742761 A CN102742761 A CN 102742761A CN 2012102425863 A CN2012102425863 A CN 2012102425863A CN 201210242586 A CN201210242586 A CN 201210242586A CN 102742761 A CN102742761 A CN 102742761A
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crystallization
erythritol
temperature
sweetener
antierythrite
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刘宗利
王乃强
栾庆民
张祥奎
周焕霞
袁卫涛
李克文
熊小兰
张莉
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Baolingbao Biology Co Ltd
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Baolingbao Biology Co Ltd
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Abstract

The invention relates to the technical field of compound sugar, in particular to an erythritol crystal, which comprises erythritol and sweet agents accounting for 1 to 2.5 percent of the weight of the erythritol. A preparation method of the erythritol crystal comprises the following steps that the erythritol and the sweet agents are mixed and dissolved to obtain liquid solution, the solution is simultaneously evaporated and crystallized, and the erythritol crystals are obtained; the erythritol and the sweet agents are mixed and are dissolved to obtain liquid solution, the liquid solution is subjected to non-evaporation crystallization, the filtering is carried out after the crystallization completion, and the erythritol crystals are obtained; the erythritol and the sweet agents are mixed in a solid from; and the mixed solids are subjected to melting, crystallization, crushing and drying to obtain the erythritol crystals. The sweetness of the erythritol is improved and reaches more than 80 percent of the sweetness of the cane sugar, the consistency of ingredients of compound products of the erythritol and the sweet agents is realized, the problem of cocrystallization of the erythritol and the sweet agents easily carbonized at high temperature is solved, the crystallization rate is improved to the maximum degree, the crystallization efficiency is 5 to 20 percent higher than that of the traditional crystallization technology, and the application field of the product is enlarged.

Description

A kind of erythritol crystal and preparation method thereof
Technical field
The present invention relates to composite sugared technical field, particularly a kind of erythritol crystal also relates to the preparation method of erythritol crystal.
Background technology
Antierythrite is wide at the occurring in nature distributed pole, like fruit, mushroom, lichens etc.In addition, in fermented food and mammalian body, also existing, is a kind of natural saccharic.In the industry, antierythrite is a kind of white crystal that is obtained through fermentation by glucose, has sweet taste, and sugariness is the 70%-80% of sucrose, and its heat is merely 0.2kcal/g.Antierythrite is a kind of tetrose alcohol, and its fusing point is 118-122 ℃, and cracking temperature is 329 ℃, and molecular formula is CH 4O 4H 10
Antierythrite has unique nutrition feature, has than higher digestibility, is absorbed rapidly by small intestine easily; Antierythrite does not influence blood sugar and insulin level, thereby is suitable for diabetes patient; Because bacterium can't utilize antierythrite in the oral cavity, thereby can not produce decayed tooth.
Because antierythrite has above-mentioned good characteristic, thereby is widely used in candy, beverage, baked goods, and in the industry such as health food and medicine, demand increases day by day.
Compare with most of non-sugar sweeteners, antierythrite shows good processing characteristics.Antierythrite has the sweet taste of tasty and refreshing and similar sucrose; Can give mellow and full sense of product and texture; Shelter disagreeable taste, and have refrigerant sense; Can with the synergy of other sweetener generation sweet taste; Processing conditions such as heat and acid are shown extraordinary stability.
Therefore on Application of Erythritol was promoted, composite product began to occur, and traditional method is to do antierythrite and sweetener mixed; Composite product mesoerythrit is what to separate with sweetener; Composite product mixes inhomogeneous easily, causes the use of product inconsistent, influences result of use.
Summary of the invention
For solve above with antierythrite and sweetener simply mix inhomogeneous, use inconsistent, as to influence result of use problem, the invention provides a kind of erythritol crystal that antierythrite and sweetener cocrystallization are made.
The present invention also provides the preparation method of above-mentioned erythritol crystal.
The present invention realizes through following measure:
A kind of erythritol crystal comprises antierythrite, also comprises the sweetener that accounts for antierythrite weight 1-2.5%.
Described erythritol crystal, said sweetener are that Sucralose, stevioside, stevioside, Aspartame, acesulfame potassium, knob are sweet, in Radix Glycyrrhizae, honey element, mogroside and the alitame more than one.
The preparation method of described erythritol crystal, adopt a kind of in the following method:
Method a: antierythrite and sweetener mixed dissolution are obtained liquid solution,, make erythritol crystal to solution crystallization while evaporating;
Method b: antierythrite and sweetener mixed dissolution are obtained liquid solution, solution is carried out not evaporative crystallization, crystallization is intact filters, and makes erythritol crystal;
Method c, antierythrite is mixed with solid forms with sweetener; Hybrid solid is carried out fusion, crystallization, pulverizing, drying, make erythritol crystal.
Described preparation method; Among method a and the method b sweetener be that Sucralose, stevioside, stevioside, Aspartame, acesulfame potassium, knob are sweet, in Radix Glycyrrhizae, honey element, mogroside and the alitame more than one, among the method c sweetener be that stevioside, stevioside, Aspartame, acesulfame potassium, knob are sweet, in Radix Glycyrrhizae, honey element, mogroside and the alitame more than one.
Liquid solution mesoerythrit mass concentration is 60-90% among the method a, and the sweetener mass concentration is 0.2-10.0%, the crystallization while evaporating; Crystallization temperature 90-10 ℃, per hour lower the temperature more than 60 ℃ 5~6 ℃, per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃; Per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃; Crystallization finishes, and moisture is removed in evaporation, obtains crystal.
Liquid solution mesoerythrit mass concentration is 20-90% among the method b, and 90 ℃-10 ℃ of crystallization temperatures are per hour lowered the temperature more than 60 ℃ 5~6 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃; Per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization finishes to centrifugalize and removes moisture, obtains crystal.
150-180 ℃ of method c mesoerythrit and sweetener melt temperature, aeration-cooling speed 15-20 ℃/h, be cooled to 50 ℃-20 ℃ of temperature, crystallization finishes and pulverizes drying.
Described preparation method, the crystal of cocrystallization is sent into fluid bed or drying machine or box-type drying equipment and is carried out drying among the method c.
Beneficial effect: adopt the cocrystallization of antierythrite and sweetener, improved the sugariness of antierythrite, reach more than 80% of sweetness of cane sugar; Realized the uniformity of antierythrite and sweetener joint product composition; Solved the problem of the sweetener and the antierythrite cocrystallization of easy carbonization under the high temperature; Farthest improve percent crystallization in massecuite, crystalline rate is higher than conventional junction crystal technique 5-20%; Enlarged the application of product.
The specific embodiment
For a better understanding of the present invention, further specify below in conjunction with specific embodiment.
Embodiment 1:Antierythrite and Sucralose cocrystallization
Table 1 is antierythrite and Sucralose product mix heating and melting tables of data, can find out that from table antierythrite and the heating of Sucralose product mix in two kinds of melting point substance 130-155 ℃ scopes, all have the impurity stain to produce.Therefore, antierythrite and Sucralose cocrystallization can not adopt the mode of fusion, can only adopt the mode of liquid solution to carry out crystallization.
Table 1 antierythrite and Sucralose product mix heating and melting tables of data
Figure 20121024258631000021
1. raw material mixes
Get the 200g antierythrite, water is dissolved in the container, adds Sucralose 5.0g, stir liquid solution, the mass concentration of liquid solution mesoerythrit is 70%.
2, cocrystallization preparation and preparation of product
Stir decrease temperature crystalline since 70 ℃ with liquid solution is uncovered, be cooled to 10 ℃, per hour lower the temperature 5~6 ℃ more than 60 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃; Per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization terminal point no liquid water carries out drying with the cocrystallization crystal; Drying mode can adopt fluid bed or drying machine or box-type drying equipment; Sieve processing through screening machine at last, obtain the crystal product of variable grain degree content or mixing, crystallization yield 100% at the Clean room finished product packing.
Can adopt the mode of heating to accelerate dissolving when dissolving antierythrite in the step 1, the temperature of heating is that those skilled in the art can oneself select.
Embodiment 2:Antierythrite and Sucralose cocrystallization
1. raw material mixes
Get the 200g antierythrite, water is dissolved in the container, adds Sucralose 2.4g, stir liquid solution, the mass concentration of liquid solution mesoerythrit is 75%.
2, cocrystallization preparation and preparation of product
Stir decrease temperature crystalline since 80 ℃ with liquid solution is uncovered, be cooled to 15 ℃, per hour lower the temperature 5~6 ℃ more than 60 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃, per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization terminal point no liquid water; The cocrystallization crystal is carried out drying, and drying mode can adopt fluid bed or drying machine or box-type drying equipment, sieves processing through screening machine at last; Obtain the crystal product of variable grain degree or mixing, crystallization yield 100% at the Clean room finished product packing.
Embodiment 3:Antierythrite and stevioside cocrystallization
Table 2 is antierythrite and stevioside product mix heating and melting tables of data, can find out that from table antierythrite and the heating of stevioside product mix under melt temperature, do not have the impurity stain to produce.
Table 2 antierythrite and stevioside product mix heating and melting tables of data
Figure DEST_PATH_845146DEST_PATH_IMAGE004
1. raw material mixes
Get 200g antierythrite solid, stevioside solid 2.0g stirs mixed material.
2, cocrystallization preparation and preparation of product
With mixed material at 155 ℃ of high-temperature fusion 1-2h, decrease temperature crystalline then, aeration-cooling 15-20 ℃/h, be cooled to 30 ℃, the cocrystallization crystal is pulverized, send into fluid bed or drying machine then or box-type drying equipment carries out drying.Sieve processing through screening machine at last, obtain the crystal product of variable grain degree or mixing, crystallization yield 100% at the Clean room finished product packing.
Embodiment 4:
1. raw material mixes
Get the 200g antierythrite, water is heated to 80 ℃ and is dissolved in the container, and the concentration of antierythrite solution is 75%, and 80 ℃ of temperature add stevioside 2.4g, and mixed material is stirred.
2, cocrystallization preparation and preparation of product
Stir decrease temperature crystalline since 80 ℃ with mixed material is uncovered, be cooled to 15 ℃, per hour lower the temperature 5~6 ℃ more than 60 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃, per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization terminal point no liquid water; The cocrystallization crystal is sent into fluid bed or drying machine or box-type drying equipment carry out drying; Sieve processing through screening machine at last, obtain the crystal product of variable grain degree or mixing, crystallization yield 100% at the Clean room finished product packing.
Embodiment 5:
1, raw material mixes
Get the 200g antierythrite, water is heated to 80 ℃ and is dissolved in the container, and the concentration of antierythrite solution is 75%, and 80 ℃ of temperature add stevioside 2.4g, and Sucralose 2.4 g stir mixed material.
2, cocrystallization preparation and preparation of product
Stir decrease temperature crystalline since 80 ℃ with mixed material is uncovered, be cooled to 15 ℃, per hour lower the temperature 5~6 ℃ more than 60 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃, per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization terminal point no liquid water; The cocrystallization crystal is sent into fluid bed or drying machine or box-type drying equipment carry out drying; Sieve processing through screening machine at last, obtain the crystal product of variable grain degree or mixing, crystallization yield 100% at the Clean room finished product packing.
Embodiment 6:
1, raw material mixes
Get the 200g antierythrite, water is heated to 80 ℃ and is dissolved in the container, and the concentration of antierythrite solution is 75%, and 80 ℃ of temperature add Sucralose 2.4 g, and mixed material is stirred.
2, cocrystallization preparation and preparation of product
Mixed material sealed since 80 ℃ stir decrease temperature crystalline, be cooled to 15 ℃, per hour lower the temperature 5~6 ℃ more than 60 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃; Per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, the crystallization terminal point has liquid water, the centrifugal crystal that gets; The cocrystallization crystal is sent into fluid bed or drying machine or box-type drying equipment carry out drying; Sieve processing through screening machine at last, obtain the crystal product of variable grain degree or mixing, crystallization yield 81.2% at the Clean room finished product packing.
Table 3 antierythrite and sweetener cocrystallization product sweetness
Embodiment Antierythrite and sweetener cocrystallization product quality The deionized water quality The test of mouthfeel sugariness
Embodiment 1 2 98 15 times of sweetness of cane sugar
Embodiment 2 2 98 7 times of sweetness of cane sugar
Embodiment 3 2 98 3 times of sweetness of cane sugar
Embodiment 4 2 98 3 times of sweetness of cane sugar
Embodiment 5 2 98 9 times of sweetness of cane sugar
Embodiment 6 2 98 1 times of sweetness of cane sugar
The conventional art comparative example:
Traditional crystallization technique, crystallization process seals, feed concentration 50-60%, 70 ℃~25 ℃ of cooling scopes.
1, raw material mixes
Get the 200g antierythrite, water is heated to 80 ℃ and is dissolved in the container, and the concentration of antierythrite solution is 55%, and 70 ℃ of temperature add Sucralose 2.4g, and mixed material is stirred.
2, cocrystallization preparation and preparation of product
Mixed material sealed since 70 ℃ stir decrease temperature crystalline, be cooled to 25 ℃, per hour lower the temperature 10 ℃ more than 60 ℃, per hour lower the temperature 5~6 ℃ for 60 ℃~45 ℃, per hour lower the temperature 6~8 ℃, drop to below 25 ℃ centrifugal for 45 ℃~25 ℃.The crystallization terminal point has liquid water; The centrifugal crystal that gets is sent the cocrystallization crystal into fluid bed or drying machine or box-type drying equipment and is carried out drying, sieves processing through screening machine at last; Obtain the crystal product of variable grain degree or mixing, crystallization yield 75.8% at the Clean room finished product packing.
Do not describe part in detail among technique scheme and the embodiment, all can be with reference to prior art.
Method of the present invention is equally applicable to the cocrystallization preparation of product of other sweetener and antierythrite; Sweetener is that Sucralose, steviol glycoside (stevioside), stevioside, Aspartame, acesulfame potassium, knob are sweet, Radix Glycyrrhizae, honey element, mogroside, alitame, includes but not limited to above sweetener.
Preparation principle is in the crystallization process of antierythrite, and sweetener is added, and realizes sweetener and antierythrite intergrowth of crystals, forms brand-new crystal product, and product is used for fields such as food, mensal sweetening agent, health products, pharmaceutic adjuvant.
Should be appreciated that shown in the invention is not restricted to here and the specific embodiment of describing.Be not intended to describe in detail those those of ordinary skills at this and reading all conspicuous variation and the changes that to accomplish on the basis of specification of the present invention.But, should be understood that all these variations and change in the scope of the present invention all be included in appended claims and limited.

Claims (8)

1. an erythritol crystal comprises antierythrite, it is characterized in that also comprising the sweetener that accounts for antierythrite weight 1-2.5%.
2. erythritol crystal according to claim 1 is characterized in that said sweetener is that Sucralose, stevioside, stevioside, Aspartame, acesulfame potassium, knob are sweet, in Radix Glycyrrhizae, honey element, mogroside and the alitame more than one.
3. the preparation method of the described erythritol crystal of claim 1 is characterized in that adopting a kind of in the following method:
Method a: antierythrite and sweetener mixed dissolution are obtained liquid solution,, make erythritol crystal to solution crystallization while evaporating;
Method b: antierythrite and sweetener mixed dissolution are obtained liquid solution, solution is carried out not evaporative crystallization, crystallization is intact filters, and makes erythritol crystal;
Method c, antierythrite is mixed with solid forms with sweetener; Hybrid solid is carried out fusion, crystallization, pulverizing, drying, make erythritol crystal.
4. preparation method according to claim 3; It is characterized in that sweetener among method a and the method b is that Sucralose, stevioside, stevioside, Aspartame, acesulfame potassium, knob are sweet, in Radix Glycyrrhizae, honey element, mogroside and the alitame more than one, among the method c sweetener be that stevioside, stevioside, Aspartame, acesulfame potassium, knob are sweet, in Radix Glycyrrhizae, honey element, mogroside and the alitame more than one.
5. preparation method according to claim 3 is characterized in that liquid solution mesoerythrit mass concentration is 60-90% among the method a, and the sweetener mass concentration is 0.2-10.0%; The crystallization while evaporating, is per hour lowered the temperature more than 60 ℃ 5~6 ℃ by crystallization temperature 90-10 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃, per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization finishes; Moisture is removed in evaporation, obtains crystal.
6. preparation method according to claim 3; It is characterized in that liquid solution mesoerythrit mass concentration is 20-90% among the method b, 90 ℃-10 ℃ of crystallization temperatures are per hour lowered the temperature more than 60 ℃ 5~6 ℃; Per hour lower the temperature 3~4 ℃ for 60 ℃~45 ℃; Per hour lower the temperature 6~8 ℃ for 45 ℃~10 ℃, crystallization finishes to centrifugalize and removes moisture, obtains crystal.
7. preparation method according to claim 3 is characterized in that 150-180 ℃ of method c mesoerythrit and sweetener melt temperature, aeration-cooling speed 15-20 ℃/h, be cooled to 50 ℃-20 ℃ of temperature, and crystallization finishes and pulverizes drying.
8. preparation method according to claim 7, the crystal that it is characterized in that cocrystallization among the method c is sent into fluid bed or drying machine or box-type drying equipment and is carried out drying.
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CN103262972A (en) * 2013-01-21 2013-08-28 武汉科技大学 Erythritol and sucralose cocrystal product and cocrystallization method thereof
CN103271260A (en) * 2013-06-26 2013-09-04 武汉科技大学 Eutectic product of honey and erythritol and cocrystallization method of eutectic product
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CN103637159A (en) * 2013-11-27 2014-03-19 湖南希尔天然药业有限公司 Natural compound sweetening agent and preparation method thereof
CN104431688A (en) * 2014-12-12 2015-03-25 保龄宝生物股份有限公司 Method for improving erythritol sweetness by co-crystallizing withstevioside
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CN110771856A (en) * 2019-12-02 2020-02-11 保龄宝生物股份有限公司 Method for melting and co-crystallizing erythritol and high sweetener and obtained product
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CN103262972A (en) * 2013-01-21 2013-08-28 武汉科技大学 Erythritol and sucralose cocrystal product and cocrystallization method thereof
CN103271260A (en) * 2013-06-26 2013-09-04 武汉科技大学 Eutectic product of honey and erythritol and cocrystallization method of eutectic product
CN103271260B (en) * 2013-06-26 2014-11-05 武汉科技大学 Eutectic product of honey and erythritol and cocrystallization method of eutectic product
CN103535579A (en) * 2013-10-16 2014-01-29 天津大学 Xylitol/menthol co-crystallization body and preparation method thereof
CN103637159B (en) * 2013-11-27 2015-07-29 湖南希尔天然药业有限公司 A kind of natural built-up sweetener and preparation method thereof
CN103637159A (en) * 2013-11-27 2014-03-19 湖南希尔天然药业有限公司 Natural compound sweetening agent and preparation method thereof
CN104431688A (en) * 2014-12-12 2015-03-25 保龄宝生物股份有限公司 Method for improving erythritol sweetness by co-crystallizing withstevioside
CN104621318A (en) * 2015-01-27 2015-05-20 张雨生 Zero-calorie health care type siraitia grosvenorii candy and preparation method thereof
CN104996970A (en) * 2015-06-08 2015-10-28 桂林莱茵生物科技股份有限公司 Compound crystalline sweetener and preparation method thereof
US11718594B2 (en) 2016-09-21 2023-08-08 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
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CN110215732B (en) * 2019-07-16 2021-11-12 山东奔月生物科技股份有限公司 Method for cocrystallization of neotame and erythritol
CN110215732A (en) * 2019-07-16 2019-09-10 山东奔月生物科技股份有限公司 The method of neotame and antierythrite cocrystallization
CN110771856A (en) * 2019-12-02 2020-02-11 保龄宝生物股份有限公司 Method for melting and co-crystallizing erythritol and high sweetener and obtained product
CN111000201A (en) * 2019-12-27 2020-04-14 亿利耐雀生物科技有限公司 Natural compound sweetener and preparation method thereof
WO2024139030A1 (en) * 2022-12-25 2024-07-04 浙江华康药业股份有限公司 Preparation system for compound crystals of erythritol and high-intensity sweeteners and method therefor

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Application publication date: 20121024