CN105111249A - Method for gas phase alkali neutralization in sucralose production - Google Patents
Method for gas phase alkali neutralization in sucralose production Download PDFInfo
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- CN105111249A CN105111249A CN201510597189.1A CN201510597189A CN105111249A CN 105111249 A CN105111249 A CN 105111249A CN 201510597189 A CN201510597189 A CN 201510597189A CN 105111249 A CN105111249 A CN 105111249A
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- sucralose
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- phase alkali
- neutralization
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Abstract
The invention relates to a method for gas phase alkali neutralization in sucralose production. The method comprises the step 1) of utilizing gas phase alkali to neutralize chlorinated liquid leading to a neutralization kettle at a sucralose neutralization section; the step 2) of leading the gas phase alkali to the neutralization kettle to adjust the PH of the chlorinated liquid to 6-7; the step 3) of obtaining semi-finished product sucralose after concentration, crystallization, recrystallization and drying of the neutralized neutralization liquid; and the step 4) of obtaining finished product sucralose after alcoholysis of the semi-finished product sucralose. Compared with the prior art, the method has the advantages that 1 compared with a conventional liquid diluted alkali neutralization process, the yield is improved; 2 the neutralization time is shortened and the working efficiency is improved; 3 during the gas phase alkali neutralization, no redundant water is brought into a system, generated sewage is reduced; 4 the time of the neutralization liquid in the system is shortened and by-products are reduced; and 5 the yield of the finished product sucralose is improved.
Description
Technical field
The invention belongs to chemical production technical field, relate to the method for gas phase alkali neutralization in the production of a kind of Sucralose.
Background technology
Sucralose is a kind of white powder product, very easily water-soluble, ethanol and methyl alcohol, the functional sweetener of raw material production that to be unique with sucrose be, its sugariness is 600 times of sucrose, and sweet taste is pure, and the very similar sucrose of sweet taste characteristic, without any bitter aftertaste; Empty calory, not carious tooth, good stability, stable especially especially in aqueous.Proving that its security is high through long toxicological test, is current classic functional sweetener, and now more than 30 state approval such as the existing U.S., Canada, Australia, Russia, China uses.Sucralose has been widely used in the industries such as beverage, food, medicine, makeup, because Sucralose is a kind of novel non-nutritive sweetener, be the foodstuff additive that obesity, cardiovascular diseases and diabetic subject are desirable, therefore, its application in protective foods and medicine constantly expands.
In Sucralose is in the past produced, in and workshop section always be and use liquid diluted alkaline to neutralize, during this kind of method is carried out and efficiency not high, 7 ~ 8 hours reaction times is longer, produces a large amount of waste water, every 4m
3chlorated liquid carries out neutralization and produces 600kg waste water, makes Sucralose produce total yield and only has about 35%, constrain the production of whole Sucralose.
Summary of the invention:
Object of the present invention is exactly adopt liquid diluted alkaline to neutralize to solve during existing Sucralose is produced, in generation and at the bottom of efficiency, waste water generation is large, yield is low shortcoming, and the gas phase alkali neutralization method in providing a kind of Sucralose to produce.
The object of the invention is to be achieved by the following technical programs:
1, the gas phase alkali neutralization method in Sucralose production, is characterized in that:
1), in Sucralose and workshop section, gas phase alkali is utilized to neutralize the chlorated liquid in passing into and in still;
2) chlorated liquid PH is regulated to form neutralizer during gas phase alkali passes into and in still between 6 ~ 7;
3), after neutralizer, the crystallization concentrated through comprising of routine after neutralization, recrystallization, drying step, Sucralose work in-process are obtained;
4) Sucralose work in-process through routine comprise alcoholysis, concentration crystallization step after obtain Sucralose finished product.
On the basis of technique scheme, there is following further technical scheme:
Control chlorated liquid temperature 0 ~ 6 DEG C in N-process, it is 1000 ~ 1700L/min that gas phase alkali passes into flow velocity, in and the time be 2 ~ 3 hours.
During gas phase alkali passes into and still adopt and pass into along tangential direction at the bottom of still, in and still utilize stirring fully to mix.
Gas phase alkali in technique scheme is through distillation, dehumidifying, pressurization, cooling generation gas phase alkali, and it is method well known in the art.
Sucralose provided by the present invention produce in gas phase alkali neutralization method have following advantage than neutralization method in the past: 1, liquid diluted alkaline neutralisation more in the past, yield improves; 2, in shortening and the time, improve working efficiency; 3, enter system in this gas phase alkali and without unnecessary water-band, reduce the generation of sewage; 4, shorten the neutralizer time in systems in which, decrease the generation of by product; 5, improve the yield of finished product Sucralose.
Accompanying drawing illustrates:
Fig. 1 is process flow diagram provided by the invention.
Specific implementation method:
As shown in Figure 1, contain a kind of Sucralose produce in main process flow steps, relate to basic process steps of the present invention as follows: during the glycogenetic chlorated liquid of A is sent in 1) being produced by Sucralose and still; 2) open refrigerated water to lower the temperature to chlorated liquid, until temperature arrives the index of specifying; 3), after temperature arrives index, pass into gas phase alkali and neutralize; 4) control the flow velocity of gas phase alkali, simultaneously in and process in control well in and the temperature of still; 5), after neutralization terminates, concentrated for neutralizer feeding, crystallization, recrystallization, oven dry are obtained Sucralose work in-process; 6) Sucralose work in-process are sent into next workshop section and carry out alcoholysis, obtain Sucralose finished product through alcoholysis, decolouring, condensing crystal, oven dry.
Concrete actually operating is as follows:
Example one: the glycogenetic chlorated liquid 4m of A during Sucralose is produced
3with still (this 4m in feeding
3chlorated liquid is reacted by 300kg white sugar to generate), open stirring to open refrigerated water simultaneously and lower the temperature to chlorated liquid, control temperature is 5 ~ 6 DEG C, after temperature arrives index, separately liquid phase alkali is generated gas phase alkali through distillation, dehumidifying, pressurization, cooling, control gas phase alkali temperature and reach 8 ~ 10 DEG C, after pass into and neutralize, flow velocity is 1100L/min, simultaneously in and process keep in and the temperature of still at 5 ~ 6 DEG C, the ventilation phase alkali time is 3h, and gas phase alkali input amount is 150kg, and now pH value is between 6 ~ 7.After neutralization terminates, concentrated for neutralizer feeding, crystallization, recrystallization, oven dry are obtained Sucralose work in-process 171kg, yield is 57.0%, Sucralose work in-process are sent into next workshop section and carries out alcoholysis, obtain Sucralose finished product 128kg through alcoholysis, decolouring, condensing crystal, oven dry, total yield is 42.7%.
Example two:
The glycogenetic chlorated liquid 4m of A during Sucralose is produced
3with still (this 4m in feeding
3chlorated liquid is reacted by 300kg white sugar to generate), open stirring to open refrigerated water simultaneously and lower the temperature to chlorated liquid, control temperature is 3 ~ 4 DEG C, after temperature arrives index, by liquid phase alkali through distillation, dehumidifying, pressurization, cooling, control gas phase alkali temperature and reach 8 ~ 10 DEG C, after pass into and neutralize, flow velocity is 1320L/min, simultaneously in and process keep in and the temperature of still at 3 ~ 4 DEG C, the ventilation phase alkali time is 2.5h, and gas phase alkali input amount is 150kg, and now pH value is between 6 ~ 7.After neutralization terminates, concentrated for neutralizer feeding, crystallization, recrystallization, oven dry are obtained Sucralose work in-process 176kg, yield is 58.7%, Sucralose work in-process are sent into next workshop section and carries out alcoholysis, obtain Sucralose finished product 130kg through alcoholysis, decolouring, condensing crystal, oven dry, total yield is 43.3%.
Example three:
The glycogenetic chlorated liquid 4m of A during Sucralose is produced
3with still (this 4m in feeding
3chlorated liquid is reacted by 300kg white sugar to generate), open stirring to open refrigerated water simultaneously and lower the temperature to chlorated liquid, control temperature is 1 ~ 2 DEG C, after temperature arrives index, by liquid phase alkali through distillation, dehumidifying, pressurization, cooling, control gas phase alkali temperature and reach 8 ~ 10 DEG C, after pass into and neutralize, flow velocity is 1650L/min, simultaneously in and process keep in and the temperature of still at 1 ~ 2 DEG C, the ventilation phase alkali time is 2h, and gas phase alkali input amount is 150kg, and now pH value is between 6 ~ 7.After neutralization terminates, concentrated for neutralizer feeding, crystallization, recrystallization, oven dry are obtained Sucralose work in-process 182kg, yield is 60.7%, Sucralose work in-process are sent into next workshop section and carries out alcoholysis, obtain Sucralose finished product 134kg through alcoholysis, decolouring, condensing crystal, oven dry, total yield is 44.7%.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (3)
1. the gas phase alkali neutralization method in Sucralose production, is characterized in that:
1), in Sucralose and workshop section, gas phase alkali is utilized to neutralize the chlorated liquid in passing into and in still;
2) chlorated liquid PH is regulated to form neutralizer during gas phase alkali passes into and in still between 6 ~ 7;
3), after neutralizer, the crystallization concentrated through comprising of routine after neutralization, recrystallization, drying step, Sucralose work in-process are obtained;
4) Sucralose work in-process through routine comprise alcoholysis, concentration crystallization step after obtain Sucralose finished product.
2. according to claim 1 a kind of Sucralose produce in gas phase alkali neutralization method, it is characterized in that, control chlorated liquid temperature 0 ~ 6 DEG C in N-process, it is 1000 ~ 1700L/min that gas phase alkali passes into flow velocity, in and the time be 2 ~ 3 hours.
3. according to claim 1 or 2 a kind of Sucralose produce in gas phase alkali neutralization method, it is characterized in that, during gas phase alkali passes into and still adopt and pass into along tangential direction at the bottom of still, in and still utilize stirring fully to mix.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510597189.1A CN105111249A (en) | 2015-09-19 | 2015-09-19 | Method for gas phase alkali neutralization in sucralose production |
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| CN201510597189.1A CN105111249A (en) | 2015-09-19 | 2015-09-19 | Method for gas phase alkali neutralization in sucralose production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105747184A (en) * | 2016-03-07 | 2016-07-13 | 李云军 | Sucralose chemical synthesis process |
| CN106366138A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Continuous neutralization reaction method for sucralose |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759728A (en) * | 2010-01-08 | 2010-06-30 | 江苏巨邦制药有限公司 | Method for preparing and refining sucralose |
| CN102321122A (en) * | 2011-10-21 | 2012-01-18 | 湖北益泰药业有限公司 | Method for preparing sucralose from sucralose-6-acetate |
| CN102417526A (en) * | 2011-10-19 | 2012-04-18 | 湖北益泰药业有限公司 | Method for preparing sucralose-6-ester by utilizing phase transfer catalyst to catalyze and chloridize |
| CN104387427A (en) * | 2014-10-30 | 2015-03-04 | 安徽金禾实业股份有限公司 | Method for producing sucralose |
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2015
- 2015-09-19 CN CN201510597189.1A patent/CN105111249A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759728A (en) * | 2010-01-08 | 2010-06-30 | 江苏巨邦制药有限公司 | Method for preparing and refining sucralose |
| CN102417526A (en) * | 2011-10-19 | 2012-04-18 | 湖北益泰药业有限公司 | Method for preparing sucralose-6-ester by utilizing phase transfer catalyst to catalyze and chloridize |
| CN102321122A (en) * | 2011-10-21 | 2012-01-18 | 湖北益泰药业有限公司 | Method for preparing sucralose from sucralose-6-acetate |
| CN104387427A (en) * | 2014-10-30 | 2015-03-04 | 安徽金禾实业股份有限公司 | Method for producing sucralose |
Non-Patent Citations (2)
| Title |
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| 吴妤萱，等: "三氯蔗糖工业生产中氯代反应后处理的工艺改进", 《山西化工》 * |
| 蔡基智: "不同类型的碱对三氯蔗糖合成过程中氯代液中和效果的影响", 《现代食品科技》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105747184A (en) * | 2016-03-07 | 2016-07-13 | 李云军 | Sucralose chemical synthesis process |
| CN106366138A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Continuous neutralization reaction method for sucralose |
| CN106366138B (en) * | 2016-08-30 | 2018-11-06 | 安徽金禾实业股份有限公司 | The continuous neutralization reaction method of Sucralose |
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Application publication date: 20151202 |