CN1583719A - Preparation of cyclohexanyl calcium sulfamate - Google Patents
Preparation of cyclohexanyl calcium sulfamate Download PDFInfo
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- CN1583719A CN1583719A CN 200410027428 CN200410027428A CN1583719A CN 1583719 A CN1583719 A CN 1583719A CN 200410027428 CN200410027428 CN 200410027428 CN 200410027428 A CN200410027428 A CN 200410027428A CN 1583719 A CN1583719 A CN 1583719A
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- hexahydroaniline
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Abstract
A process for preparing calcium cyclohexylamino sulfonate includes such steps as reacting between cyclohexamine and sulfoamino acid, concentrating its resultant, reacting on cyclohexamine, adding calcium hydroxide and H2O, displacing reacting, regulating pH value, and recovering product.
Description
Technical field
The present invention relates to a kind of preparation method of calcium cyclamate.
Background technology
Along with making rapid progress of food service industry, people also constantly improve the pursuit of food, drink flavour.But it is found that, now various food on the market, beverage all ubiquity mouthfeel and send out puckery, fragrant and sweet inadequately problem.In addition, people know that calcium is one of most important element in the human body, and it participates in all vital movement processes, especially calcium deficiency cause not only that rickets, bone growth and development are bad, osteoporosis and hyperplasia, also easily suffer from diseases such as hypertension, diabetes, arteriosclerosis and senile dementia.Calcium cyclamate is a kind ofly can make food, the beverage mouthfeel foodstuff additive fragrant and sweet, that can replenish the calcium again that become.And at present, China is almost blank to the production of this foodstuff additive of calcium cyclamate.
Summary of the invention
For remedying the defective of prior art, the invention provides a kind of preparation method of calcium cyclamate.
Technical scheme of the present invention is as follows: a kind of preparation method of calcium cyclamate may further comprise the steps:
(1) make hexahydroaniline and para-aminobenzenesulfonic acid in pH6.8-7.2 and reaction below 80 ℃;
(2) step (1) gained reaction product is concentrated and obtain enriched product;
(3) described enriched product and hexahydroaniline are reacted under the temperature between 135 to 142 ℃ and generate work in-process;
(4) adding calcium hydroxide and water in step (3) gained work in-process carries out replacement(metathesis)reaction and obtains product mixtures;
(5) adjust described product mixtures;
(6) from adjusted product mixtures, reclaim the calcium cyclamate product.
In one embodiment, described method also is included in and adds the step that reclaims the residue ring hexylamine before calcium hydroxide and the water.
In one embodiment, described adjustment comprises decolouring, the removal of impurity and adjustment potential of hydrogen.
In one embodiment, the step of described recovery calcium cyclamate product comprises filtration, crystallization and separating step.
In one embodiment, the concentration process of above-mentioned steps (2) carries out under the temperature between 90 to 110 ℃.
In one embodiment, the replacement(metathesis)reaction of above-mentioned steps (4) is carried out under the temperature between 100 to 120 ℃.
In one embodiment, the adjustment process of above-mentioned steps (5) comprises adding gac or diatomite, the pH value is controlled between the 9-10, and temperature is remained between 50 to 55 ℃.
In one embodiment, the process of described recovery hexahydroaniline is carried out under the temperature between 90 to 105 ℃.
In one embodiment, described filtration will make the material transparency after the filtration reach more than 98%.
In one embodiment, described crystallisation process carries out under the temperature between 55 to 60 ℃.
The invention has the beneficial effects as follows the blank of having filled up this foodstuff additive of domestic production calcium cyclamate.The inventive method technology is simple, and raw material is easy to get, and energy consumption is low, the yield height, and the product purity height is applicable to large-scale commercial production.Product by the inventive method preparation has following characteristics: (1), good water solubility: cold water, hot water are all solvable; (2), sweet taste is salubrious: the same with sucrose; (3), nontoxicity and low in calories: harmless, can also play the effect of replenishing the calcium; (4), stability is high: the heat of general use range, acid, alkali do not decompose, and undergo no deterioration.The product of producing by the inventive method satisfies the requirement of foodstuff additive standard, is the ideal sweetening agent, is applicable to that field such as food and medicine uses.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.These embodiment only are used to illustrate the present invention, limit the scope of the invention never by any way.
Embodiment 1
Add hexahydroaniline and para-aminobenzenesulfonic acid in reactor, and control material pH value is 6.8, temperature is 75 ℃, reacts 4 hours.With steam heating and vacuum concentration 10 hours, Heating temperature was 90 ℃ with the gained mixture.Add hexahydroaniline, generated work in-process in 52 hours steam-heated the reaction simultaneously, Heating temperature is 142 ℃.About 100 ℃, reclaim remaining hexahydroaniline and be used for recycling.In remaining mixture, add calcium hydroxide and water then, reacted 45 hours down, obtain product mixtures at 100 ℃.Add gac and decolour, the removal of impurity, and adjust potential of hydrogen, and pH is controlled at about 9, temperature remains on 50-55 ℃, and the time is 5 hours.Then, the filtration of gained mixture is reached more than 98% until the filtrate transparency.Make gained filtrate about 55 ℃ of following Concentrated and crystallized in vacuum 32 hours.Isolate the calcium cyclamate product with whizzer then.At last, the finished product oven dry is removed surface-moisture and screening packing.
Embodiment 2
Add hexahydroaniline and para-aminobenzenesulfonic acid in reactor, and control material pH value is 7.2, temperature is 75 ℃, reacts 4 hours.With steam heating and vacuum concentration 8 hours, Heating temperature was 110 ℃ with the gained mixture.Add hexahydroaniline, generated work in-process in 55 hours steam-heated the reaction simultaneously, Heating temperature is 135 ℃.About 100 ℃, reclaim remaining hexahydroaniline and be used for recycling.In remaining mixture, add calcium hydroxide and water then, reacted 40 hours down, obtain product mixtures at 120 ℃.Add gac and decolour, the removal of impurity, and adjust potential of hydrogen, and pH is controlled at about 10, temperature remains on 50-55 ℃, and the time is 5 hours.Then, the filtration of gained mixture is reached more than 98% until the filtrate transparency.Make gained filtrate about 60 ℃ of following Concentrated and crystallized in vacuum 30 hours.Isolate the calcium cyclamate product with whizzer then.At last, the finished product oven dry is removed surface-moisture and screening packing.
Embodiment 3
Add hexahydroaniline and para-aminobenzenesulfonic acid in reactor, and control material pH value is 7.0, temperature is 65 ℃, reacts 4 hours.With steam heating and vacuum concentration 9 hours, Heating temperature was 100 ℃ with the gained mixture.Add hexahydroaniline, generated work in-process in 53 hours steam-heated the reaction simultaneously, Heating temperature is 140 ℃.About 100 ℃, reclaim remaining hexahydroaniline and be used for recycling.In remaining mixture, add calcium hydroxide and water then, reacted 42 hours down, obtain product mixtures at 110 ℃.Add gac and decolour, the removal of impurity, and adjust potential of hydrogen, and pH is controlled at about 9.5, temperature remains on 52 ℃, and the time is 5 hours.Then, the filtration of gained mixture is reached more than 98% until the filtrate transparency.Make gained filtrate about 58 ℃ of following Concentrated and crystallized in vacuum 31 hours.Isolate the calcium cyclamate product with whizzer then.At last, the finished product oven dry is removed surface-moisture and screening packing.
Gained finished product calcium cyclamate is of many uses, both can be used for icing food, beverages such as fine jade pouring, refreshment drink, coffee, biscuit, bread, jelly, pickles; Also can be used for home-use food flavouring; The sweet taste material that also can be used for medicine and makeup; And, also can be used for diabetic subject or obesity patient's sugared sweetener of generation.
Claims (10)
1, a kind of preparation method of calcium cyclamate may further comprise the steps:
(1) make hexahydroaniline and para-aminobenzenesulfonic acid in pH 6.8-7.2 and reaction below 80 ℃;
(2) step (1) gained reaction product is concentrated and obtain enriched product;
(3) described enriched product and hexahydroaniline are reacted under the temperature between 135 to 142 ℃ and generate work in-process;
(4) adding calcium hydroxide and water in step (3) gained work in-process carries out replacement(metathesis)reaction and obtains product mixtures;
(5) adjust described product mixtures;
(6) from adjusted product mixtures, reclaim the calcium cyclamate product.
2, method according to claim 1 also is included in the step that adding calcium hydroxide and water reclaim the residue ring hexylamine before.
3, method according to claim 1, wherein said adjustment comprise decolouring, the removal of impurity and adjustment potential of hydrogen.
4, method according to claim 1, the step of wherein said recovery calcium cyclamate product comprises filtration, crystallization and separating step.
5, method according to claim 1, wherein the concentration process of step (2) carries out under the temperature between 90 to 110 ℃.
6, method according to claim 1, wherein the replacement(metathesis)reaction of step (4) is carried out under the temperature between 100 to 120 ℃.
7, method according to claim 1, wherein the adjustment process of step (5) comprises adding gac or diatomite, the pH value is controlled between the 9-10, and temperature is remained between 50 to 55 ℃.
8, method according to claim 2, the process of wherein said recovery hexahydroaniline is carried out under the temperature between 90 to 105 ℃.
9, method according to claim 4, wherein said filtration will make the material transparency after the filtration reach more than 98%.
10, method according to claim 4, wherein said crystallisation process carries out under the temperature between 55 to 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027428 CN1249027C (en) | 2004-05-29 | 2004-05-29 | Preparation of cyclohexanyl calcium sulfamate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410027428 CN1249027C (en) | 2004-05-29 | 2004-05-29 | Preparation of cyclohexanyl calcium sulfamate |
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| Publication Number | Publication Date |
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| CN1583719A true CN1583719A (en) | 2005-02-23 |
| CN1249027C CN1249027C (en) | 2006-04-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410027428 Expired - Fee Related CN1249027C (en) | 2004-05-29 | 2004-05-29 | Preparation of cyclohexanyl calcium sulfamate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016889A (en) * | 2014-06-08 | 2014-09-03 | 中国科学院上海有机化学研究所 | Isotope labeled sodium cyclamate and preparation method thereof |
| CN106083661A (en) * | 2016-06-06 | 2016-11-09 | 江苏联威生化实业有限公司 | A kind of preparation method of calcium cyclamate |
| CN113387849A (en) * | 2021-07-08 | 2021-09-14 | 金城化学(江苏)有限公司 | Sodium cyclamate production process and device |
| CN113956186A (en) * | 2021-11-03 | 2022-01-21 | 苏州纽特食品科技有限公司 | Preparation method of sodium cyclamate |
| CN114014785A (en) * | 2021-11-03 | 2022-02-08 | 苏州纽特食品科技有限公司 | Preparation method of low-purity sodium cyclamate |
-
2004
- 2004-05-29 CN CN 200410027428 patent/CN1249027C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016889A (en) * | 2014-06-08 | 2014-09-03 | 中国科学院上海有机化学研究所 | Isotope labeled sodium cyclamate and preparation method thereof |
| CN104016889B (en) * | 2014-06-08 | 2016-04-13 | 中国科学院上海有机化学研究所 | A kind of isotope-labeled Sodium Cyclamate and preparation method thereof |
| CN106083661A (en) * | 2016-06-06 | 2016-11-09 | 江苏联威生化实业有限公司 | A kind of preparation method of calcium cyclamate |
| CN113387849A (en) * | 2021-07-08 | 2021-09-14 | 金城化学(江苏)有限公司 | Sodium cyclamate production process and device |
| CN113956186A (en) * | 2021-11-03 | 2022-01-21 | 苏州纽特食品科技有限公司 | Preparation method of sodium cyclamate |
| CN114014785A (en) * | 2021-11-03 | 2022-02-08 | 苏州纽特食品科技有限公司 | Preparation method of low-purity sodium cyclamate |
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| Publication number | Publication date |
|---|---|
| CN1249027C (en) | 2006-04-05 |
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Owner name: SHANTOU WEIXIN CO., LTD. Free format text: FORMER NAME: WEIXIN FOOD CO., LTD., SHANTOU CITY |
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Address after: 515021 Guangdong province Shantou Jinyuan Industrial Zone 3A3 Patentee after: Shantou Weixin Industry Co., Ltd. Address before: 515021 Guangdong province Shantou Jinyuan Industrial Zone 3A3 Patentee before: Weixin Food Co., Ltd., Shantou City |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060405 Termination date: 20180529 |