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Neutralization method of chlorination solution

A technology of chlorination reaction and reaction solution, applied in chemical instruments and methods, neutralized water/sewage treatment, sugar derivative preparation, etc., can solve problems such as irritating odor, decomposition, increase environmental protection treatment costs, etc. degree, reduce losses, and promote the effect of reducing pollution and consumption

Active Publication Date: 2019-08-02
WENGYUAN GUANGYE QINGYI FOOD TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN106366138A uses ammonia water to continuously neutralize the chlorinated reaction solution. However, the neutralization process in ammonia water will bring irritating odor, and also greatly increase the ammonia nitrogen value in wastewater, increasing the cost of environmental protection treatment
The neutralization process of sodium hydroxide solution easily causes the hydrolysis of sucralose-6-acetate and the decomposition of solvent DMF
At present, the chlorination reaction solution in the process of industrial production of sucralose at home and abroad is mostly neutralized by a single alkaline solution, resulting in various follow-up problems. In order to solve the above problems, the existing process must be optimized

Method used

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  • Neutralization method of chlorination solution
  • Neutralization method of chlorination solution
  • Neutralization method of chlorination solution

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Take by weighing 270g of reaction solution and place in conical flask, this reaction solution is obtained by chlorination reaction of sucrose-6-ethyl ester in DMF solvent or under the environment of DMF solvent and other solvents and thionyl chloride or carbonyl chloride, Wherein other solvents may be toluene, pyridine or tetrahydrofuran, etc., after cooling and stirring, 30 wt% sodium carbonate aqueous solution is added dropwise at 25°C to neutralize to a pH value of 6.5.

[0026] Add dropwise a 32 wt% sodium hydroxide solution to neutralize to a pH of 9.0, and stir for 0.5 hours until the pH is stable.

[0027] Concentrated hydrochloric acid solution was added dropwise to adjust the pH of the reaction solution to 7.0.

[0028] As detected by HPLC, the content of sucralose-6-acetate was 5.63 wt%, and the content of DMF was 8.19 wt%. According to the mass calculation, 11.5246g of sucralose-6-acetate and 16.7649g of DMF were obtained in this implementation

Embodiment 2

[0039] Take by weighing 270g of reaction solution and place in conical flask, this reaction solution is obtained by chlorination reaction of sucrose-6-ethyl ester in DMF solvent or under the environment of DMF solvent and other solvents and thionyl chloride or carbonyl chloride, Wherein other solvents may be toluene, pyridine or tetrahydrofuran, etc., after cooling and stirring, 28wt% sodium carbonate aqueous solution is added dropwise at 25°C to neutralize to a pH value of 6.8.

[0040] Add 32 wt% aqueous sodium hydroxide solution dropwise to neutralize to a pH of 9.0, and stir for 0.5 hours until the pH is stable.

[0041] Concentrated hydrochloric acid solution was added dropwise to adjust the pH of the reaction solution to 7.0.

[0042] As detected by HPLC, the content of sucralose-6-acetate was 5.38wt%, and the content of DMF was 7.91wt%. According to the mass calculation, 11.0692 g of sucralose-6-acetate and 16.4886 g of DMF were obtained in this implementation.

Embodiment 3

[0044] Take by weighing 270g of reaction solution and place in conical flask, this reaction solution is obtained by chlorination reaction of sucrose-6-ethyl ester in DMF solvent or under the environment of DMF solvent and other solvents and thionyl chloride or carbonyl chloride, Wherein other solvents may be toluene, pyridine or tetrahydrofuran, etc., cooled and stirred to 25°C. Use recovered tower top water, its DMF content is 2.7wt%, preparation 28wt% sodium carbonate aqueous solution. At a temperature of 25° C., a 28 wt % sodium carbonate aqueous solution was added dropwise to neutralize to a pH value of 6.8.

[0045] Add 32 wt% aqueous sodium hydroxide solution dropwise to neutralize to a pH of 9.0, and stir for 0.5 hours until the pH is stable.

[0046] Concentrated hydrochloric acid solution was added dropwise to adjust the pH of the reaction solution to 7.0.

[0047]As detected by HPLC, the content of sucralose-6-acetate was 5.38wt%, and the content of DMF was 8.59wt%...

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Abstract

The invention discloses a neutralization method of a chlorination solution. The neutralization method comprises the steps as follows: cooling the chlorination solution, then, adding a weak alkaline aqueous solution for neutralization until the pH value is 5.5-7.5, adding a strong alkaline aqueous solution for neutralization until the pH value of the reaction solution is 8.5-9.5, finally, adding aconcentrated hydrochloric acid aqueous solution to the reaction solution, and adjusting the pH value of the reaction solution to 6.5-7.5. The weak alkaline aqueous solution and the strong alkaline aqueous solution are combined for use, excessive hydrolysis of sucralose-6-acetate is effectively inhibited in the chlorination solution neutralization process, and the yield of sucralose-6-acetate is increased; meanwhile, the decomposition degree of a DMF solvent in the system is slowed down, and loss of the solvent is reduced. Non-ammonia nitrogen alkaline solutions are used, low-concentration DMFwastewater is fully utilized as water for alkali dissolution, the wastewater treatment cost in the production process is reduced, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of sucralose, and in particular relates to a method for neutralizing a chlorinated reaction liquid, in particular to a method for neutralizing the chlorinated reaction liquid produced in the production process of sucralose by using a combined alkali. Background technique [0002] Sucralose, chemically named 4,1',6'-trichloro-4,1',6'-trideoxygalactose, is currently the only sweetener produced from sucrose. The sweetness intensity of sucralose is 600 times that of sucrose. It has the advantages of pure sweetness, no bitter aftertaste, no dental caries, no calories, good water solubility, and stability in acidic environment. It is currently the most excellent functional sweetener. one. [0003] The synthesis methods of sucralose mainly include single-group protection method and whole-group protection method, among which the single-group protection method has low raw material cost, high selectivity and simple p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F1/66C07H1/06C07H13/04C02F103/36
CPCC02F1/66C07H1/06C07H13/04C02F2103/36
Inventor 曾伟山陈少华张伟薇吴翁宏王锡茂
Owner WENGYUAN GUANGYE QINGYI FOOD TECH
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