CN112174911A - Large-particle double-sweet crystallization method - Google Patents
Large-particle double-sweet crystallization method Download PDFInfo
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- CN112174911A CN112174911A CN202011282471.8A CN202011282471A CN112174911A CN 112174911 A CN112174911 A CN 112174911A CN 202011282471 A CN202011282471 A CN 202011282471A CN 112174911 A CN112174911 A CN 112174911A
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- China
- Prior art keywords
- sweet
- reaction
- aspartame
- double
- acesulfame
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D291/00—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
- C07D291/02—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
- C07D291/06—Six-membered rings
Abstract
The invention relates to a large-particle double-sweet crystallization method which is characterized by comprising the following steps: a. adding a certain amount of water into a reaction kettle, controlling the water temperature to be 5-20 ℃, and putting the aspartame and the acesulfame with equal molar quantity into the reaction kettle for reaction for 2-10 times; b. after adding the materials each time, carrying out heat preservation stirring reaction for 0.5-2 hours, and then carrying out the next feeding; C. and after the last material is added, continuously stirring and reacting for 0.5-2 hours, and then filtering and drying to obtain the double sweet. The invention has the advantages that: the crystal-separated double sweet has a granularity of more than 140 meshes and can reach more than 85 percent, the fluidity of the product is greatly improved, the temperature is not required to be reduced after the crystallization, the centrifugal separation can be directly carried out, and the energy consumption can be reduced.
Description
Technical Field
The invention belongs to the technical field of food additive chemical industry, and relates to a large-particle double-sweet crystallization method.
Background
The traditional preparation method of the double sweet is that the aspartame is put into water, the acesulfame is added at one time at room temperature, the mixture is stirred and dissolved to become clear, and then the aspartame (called double sweet for short) is separated out by cooling, and the crystal precipitation by the method is fine and has poor liquidity.
Disclosure of Invention
The invention aims to overcome the defects of fine precipitated crystal and poor fluidity of the double-sweet crystal in the prior art, and provides a large-particle double-sweet crystallization method.
The technical scheme adopted by the invention is as follows:
a large particle double sweet crystallization method is characterized by comprising the following steps:
a. adding a certain amount of water into a reaction kettle, controlling the water temperature to be 5-20 ℃, and putting the aspartame and the acesulfame with equal molar quantity into the reaction kettle for reaction for 2-10 times;
b. after adding the materials each time, carrying out heat preservation stirring reaction for 0.5-2 hours, and then carrying out the next feeding;
C. and after the last material is added, continuously stirring and reacting for 0.5-2 hours, and then filtering and drying to obtain the double sweet.
The further technical proposal controls the concentration of the crystallization reaction of the aspartame and the acesulfame to be 0.2 to 1 mol/L.
According to a further technical scheme, the content of the aspartame and the content of the acesulfame added each time are respectively 0.1 mol/L.
The double sweet in the technical scheme is aspartame.
The invention has the advantages that:
the crystal-separated double sweet has a granularity of more than 140 meshes and can reach more than 85 percent, the fluidity of the product is greatly improved, the temperature is not required to be reduced after the crystallization, the centrifugal separation can be directly carried out, and the energy consumption can be reduced.
The specific implementation mode is as follows:
in the case of the example 1, the following examples are given,
1) 60.8g (0.2 mol) of aspartame with the content of 99 percent and 34.5g (0.2 mol) of acesulfame with the content of 99 percent are respectively weighed for standby.
2) 1000ml of water was added to a three-necked flask and the temperature was controlled at 5 ℃.
3) Putting the materials into a crystallization reaction for two times, adding 30.4g (0.1 mol) of aspartame and 17.3g (0.1 mol) of acesulfame for the first time, controlling the temperature at 5 ℃, and keeping the temperature and stirring for 0.5 hour after the materials become clear and separate out crystals; and feeding for the second time, finishing feeding the rest materials, continuing to keep the temperature and stirring for 0.5-2 hours, filtering, separating and drying to obtain 71g of the double sweet product. Then sampling and detecting.
4) The detection results are as follows; the grain size of the double sweet crystal is 20 meshes accounting for 2%, 40 meshes accounting for 25%, 60 meshes accounting for 30%, 80 meshes accounting for 15%, 100 meshes accounting for 15%, 140 meshes accounting for 5%, 180 meshes accounting for 8%.
Example 2:
1) 120g (0.4 mol) of aspartame with the content of 99 percent and 67g (0.4 mol) of acesulfame with the content of 99 percent are respectively weighed for standby.
2) 1000ml of water was added to a three-necked flask and the temperature was controlled at 10 ℃.
3) The materials are put into crystallization reaction for four times, and 0.1mol of aspartame and acesulfame are added each time. And (3) after the first feeding is finished, keeping the temperature and stirring for 0.5 hour after the materials become clear and separate out crystals, feeding for the second time, wherein the feeding amount and the heat preservation time are the same as those in the first reaction process, repeating the steps, feeding the materials, keeping the temperature and stirring for 0.5-2 hours after the materials are fed, filtering, separating and drying to obtain 164g of the bisweet product. Then sampling and detecting.
4) The detection results are as follows; the grain size of the double sweet crystal is 20 meshes accounting for 2%, 40 meshes accounting for 15%, 60 meshes accounting for 28%, 80 meshes accounting for 25%, 100 meshes accounting for 12%, 140 meshes accounting for 11%, and 180 meshes accounting for 7%.
Example 3
1) 240g (0.8 mol) of aspartame with the content of 99 percent and 133g (0.8 mol) of acesulfame with the content of 99 percent are respectively weighed for standby.
2) 1000ml of water was added to a three-necked flask and the temperature was controlled at 15 ℃.
3) The materials are put into crystallization reaction for eight times, and 0.1mol of aspartame and acesulfame are added each time. And (3) after the first feeding is finished, controlling the temperature to be 15 ℃, keeping the temperature and stirring for 0.5 hour after the materials become clear and separate out crystals, then feeding for the second time, wherein the feeding amount and the heat preservation time are the same as those in the first reaction process, repeating the steps, feeding the materials, keeping the temperature and stirring for 0.5-2 hours after the materials are fed, filtering, separating and drying to obtain 349g of the double sweet product. Then sampling and detecting.
4) The detection results are as follows; the grain size of the double sweet crystal is 20 meshes accounting for 4%, 40 meshes accounting for 11%, 60 meshes accounting for 25%, 80 meshes accounting for 35%, 100 meshes accounting for 10%, 140 meshes accounting for 5%, 180 meshes accounting for 10%.
Example 4
1) 299g (1 mol) of aspartame with the content of 99 percent and 165g (1 mol) of acesulfame with the content of 99 percent are respectively weighed for standby.
2) 1000ml of water was added to a three-necked flask and the temperature was controlled at 20 ℃.
3) The materials are put into crystallization reaction for ten times, and 0.1mol of aspartame and acesulfame are added each time. And (3) after the first feeding is finished, controlling the temperature to be 20 ℃, keeping the temperature and stirring for 0.5 hour after the materials become clear and separate out crystals, then feeding for the second time, wherein the feeding amount and the heat preservation time are the same as those in the first reaction process, repeating the steps, feeding the materials, keeping the temperature and stirring for 0.5-2 hours after the materials are fed, filtering, separating and drying to obtain 438g of the double sweet product. Then sampling and detecting.
4) The detection results are as follows; the grain size of the crystal of the double sweet is 20 meshes accounting for 4%, 40 meshes accounting for 10%, 60 meshes accounting for 15%, 80 meshes accounting for 24%, 100 meshes accounting for 20%, 140 meshes accounting for 15%, and 180 meshes accounting for 325%.
Claims (3)
1. A large particle double sweet crystallization method is characterized by comprising the following steps:
a. adding a certain amount of water into a reaction kettle, controlling the water temperature to be 5-20 ℃, and putting the aspartame and the acesulfame with equal molar quantity into the reaction kettle for reaction for 2-10 times;
b. after adding the materials each time, carrying out heat preservation stirring reaction for 0.5-2 hours, and then carrying out the next feeding;
C. and after the last material is added, continuously stirring and reacting for 0.5-2 hours, and then filtering and drying to obtain the double sweet.
2. The method of crystallizing a large particle of bis-sweet of claim 1, wherein:
the concentration of the reaction liquid of the aspartame and the acesulfame crystal is controlled to be 0.2-1 mol/L.
3. A crystallization method of large granular bis-sweet according to claim 1 or 2, characterized in that: the content of the added aspartame and the content of the added acesulfame are respectively 0.1 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011282471.8A CN112174911A (en) | 2020-11-17 | 2020-11-17 | Large-particle double-sweet crystallization method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011282471.8A CN112174911A (en) | 2020-11-17 | 2020-11-17 | Large-particle double-sweet crystallization method |
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| CN112174911A true CN112174911A (en) | 2021-01-05 |
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| CN202011282471.8A Pending CN112174911A (en) | 2020-11-17 | 2020-11-17 | Large-particle double-sweet crystallization method |
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Citations (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES8604766A1 (en) * | 1985-09-20 | 1986-03-16 | Palomo Coll Alberto | Sweetening salts |
| JPS63146768A (en) * | 1986-12-09 | 1988-06-18 | Nippon Kayaku Co Ltd | Aspartame-containing saccharide and production thereof |
| CA2137625A1 (en) * | 1994-12-08 | 1996-06-09 | Hubertus J. M. Slangen | Process for the treatment of aspartame |
| CN1155995A (en) * | 1995-10-11 | 1997-08-06 | 荷兰加甜剂公司 | Sweetener salt |
| NL1009323C2 (en) * | 1998-06-05 | 1999-12-07 | Holland Sweetener Co | Preparation and purification of an organic salt of aspartame. |
| CN1323792A (en) * | 2001-05-15 | 2001-11-28 | 张家港浩波化学品有限公司 | Synthesis of acetyl sulfanilic acid and its potassium salt |
| US6364914B1 (en) * | 1998-03-23 | 2002-04-02 | Ajinomoto Co., Inc. | Method of crystallization with the particle size distribution being controlled |
| JP2004033951A (en) * | 2002-07-04 | 2004-02-05 | Mitsubishi Chemicals Corp | Crystallization method and crystallizer |
| WO2005002365A1 (en) * | 2003-07-03 | 2005-01-13 | Nutrinova Nutrition Specialties & Food Ingredients Gmbh | Method for the production of a sweetener salt based on aspartame and acesulfame |
| KR100926414B1 (en) * | 2008-06-09 | 2009-11-12 | 케이엔디티앤아이 주식회사 | Preparation method of massive crystalline particles by separate feeding of reaction materials |
| KR20090127656A (en) * | 2008-06-09 | 2009-12-14 | 케이엔디티앤아이 주식회사 | Preparation method of massive crystalline particles by controlling the solubility |
| CN101869256A (en) * | 2010-06-04 | 2010-10-27 | 上海师范大学 | Preparation method of high sweetener double sweet |
| JP2011051911A (en) * | 2009-08-31 | 2011-03-17 | Shinshu Univ | Method for producing organic crystal microparticle |
| CN102731252A (en) * | 2012-06-28 | 2012-10-17 | 浙江华康药业股份有限公司 | Crystallization method for xylitol or maltol |
| CN102816204A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Preparation process of aspartame |
| CN103145547A (en) * | 2013-03-28 | 2013-06-12 | 中粮生物化学（安徽）股份有限公司 | Citric acid crystal and production method thereof |
| CN104605219A (en) * | 2015-02-14 | 2015-05-13 | 姚洪齐 | Cocrystallization method for asparaginic acid derivative and sweet acid salt |
| CN104719827A (en) * | 2015-02-14 | 2015-06-24 | 许建刚 | Co-crystallization method of aspartic acid derivative and sweetening acid |
| CN107744131A (en) * | 2017-10-27 | 2018-03-02 | 浙江三和食品科技有限公司 | A kind of high sweetener composition and preparation method thereof |
| CN109535100A (en) * | 2018-12-26 | 2019-03-29 | 常茂生物化学工程股份有限公司 | The preparation method of L-aspartyl-L-phenylalanine methylester acesulfame |
| CN111034986A (en) * | 2019-12-19 | 2020-04-21 | 南通市常海食品添加剂有限公司 | Production method of aspartame |
-
2020
- 2020-11-17 CN CN202011282471.8A patent/CN112174911A/en active Pending
Patent Citations (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES8604766A1 (en) * | 1985-09-20 | 1986-03-16 | Palomo Coll Alberto | Sweetening salts |
| JPS63146768A (en) * | 1986-12-09 | 1988-06-18 | Nippon Kayaku Co Ltd | Aspartame-containing saccharide and production thereof |
| CA2137625A1 (en) * | 1994-12-08 | 1996-06-09 | Hubertus J. M. Slangen | Process for the treatment of aspartame |
| CN1155995A (en) * | 1995-10-11 | 1997-08-06 | 荷兰加甜剂公司 | Sweetener salt |
| US5827562A (en) * | 1995-10-11 | 1998-10-27 | Holland Sweetener Company V.O.F. | Sweetener salts |
| US6364914B1 (en) * | 1998-03-23 | 2002-04-02 | Ajinomoto Co., Inc. | Method of crystallization with the particle size distribution being controlled |
| NL1009323C2 (en) * | 1998-06-05 | 1999-12-07 | Holland Sweetener Co | Preparation and purification of an organic salt of aspartame. |
| CN1323792A (en) * | 2001-05-15 | 2001-11-28 | 张家港浩波化学品有限公司 | Synthesis of acetyl sulfanilic acid and its potassium salt |
| JP2004033951A (en) * | 2002-07-04 | 2004-02-05 | Mitsubishi Chemicals Corp | Crystallization method and crystallizer |
| WO2005002365A1 (en) * | 2003-07-03 | 2005-01-13 | Nutrinova Nutrition Specialties & Food Ingredients Gmbh | Method for the production of a sweetener salt based on aspartame and acesulfame |
| KR100926414B1 (en) * | 2008-06-09 | 2009-11-12 | 케이엔디티앤아이 주식회사 | Preparation method of massive crystalline particles by separate feeding of reaction materials |
| KR20090127656A (en) * | 2008-06-09 | 2009-12-14 | 케이엔디티앤아이 주식회사 | Preparation method of massive crystalline particles by controlling the solubility |
| JP2011051911A (en) * | 2009-08-31 | 2011-03-17 | Shinshu Univ | Method for producing organic crystal microparticle |
| CN101869256A (en) * | 2010-06-04 | 2010-10-27 | 上海师范大学 | Preparation method of high sweetener double sweet |
| CN102731252A (en) * | 2012-06-28 | 2012-10-17 | 浙江华康药业股份有限公司 | Crystallization method for xylitol or maltol |
| CN102816204A (en) * | 2012-08-13 | 2012-12-12 | 南通市常海食品添加剂有限公司 | Preparation process of aspartame |
| CN103145547A (en) * | 2013-03-28 | 2013-06-12 | 中粮生物化学（安徽）股份有限公司 | Citric acid crystal and production method thereof |
| CN104605219A (en) * | 2015-02-14 | 2015-05-13 | 姚洪齐 | Cocrystallization method for asparaginic acid derivative and sweet acid salt |
| CN104719827A (en) * | 2015-02-14 | 2015-06-24 | 许建刚 | Co-crystallization method of aspartic acid derivative and sweetening acid |
| CN107744131A (en) * | 2017-10-27 | 2018-03-02 | 浙江三和食品科技有限公司 | A kind of high sweetener composition and preparation method thereof |
| CN109535100A (en) * | 2018-12-26 | 2019-03-29 | 常茂生物化学工程股份有限公司 | The preparation method of L-aspartyl-L-phenylalanine methylester acesulfame |
| CN111034986A (en) * | 2019-12-19 | 2020-04-21 | 南通市常海食品添加剂有限公司 | Production method of aspartame |
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