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Para-ester synthesis method

A synthetic method and para-ester technology, applied in the field of dye intermediates, can solve the problems of increased production costs and follow-up processing costs, and achieve the effects of stable product quality, reduced production, and mild reaction conditions

Active Publication Date: 2017-08-18
新乡市锦源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the excessive amount of chlorosulfonic acid, usually 3-5 times the theoretical amount, a large amount of acidic wastewater is generated, which increases the production cost and subsequent treatment costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] The method for synthesizing the para-ester provided in Example 1 includes the following steps:

[0066] (a) Sulfonation reaction: After adding 20 mol of fuming sulfuric acid to the reaction tank, cooling to 12°C, adding 5 mol of chlorosulfonic acid, stirring and reacting for 2 hours, adding 10 mol of acetanilide, controlling the reaction temperature to 15°C, and reacting 4 hour;

[0067] (b) Chlorination reaction: The reaction solution is heated to 45°C, 14 mol of thionyl chloride is added, and carbon tetrachloride is added as an auxiliary agent, and the reaction is carried out for 4 hours;

[0068] (c) Reduction reaction: add 10 mol of sodium sulfite, stir well, control the reaction temperature at 28°C, use sodium hydroxide solution to maintain pH=7.5, and react for 2.5 hours to obtain a reduction reaction solution;

[0069] (d) Condensation reaction: adding 15 mol of ethylene oxide to the reduction reaction solution, raising the temperature to 60°C, and reacting for 4 hours; ...

Embodiment 2

[0073] The method for synthesizing the para-ester provided in Example 2 includes the following steps:

[0074] (a) Sulfonation reaction: After adding 15 mol of fuming sulfuric acid to the reaction tank, cooling to 15°C, adding 5 mol of chlorosulfonic acid, stirring and reacting for 2 hours, adding 10 mol of acetanilide, controlling the reaction temperature to 15°C, and reacting 3. hour;

[0075] (b) Chlorination reaction: heat the reacted solution to 40°C, add 12 mol of thionyl chloride, and add carbon tetrachloride as an auxiliary agent, and react for 3 hours;

[0076] (c) Reduction reaction: add 11 mol of sodium sulfite, stir uniformly, control the reaction temperature at 30°C, use sodium hydroxide solution to maintain pH=7.5, and react for 2 hours to obtain a reduction reaction solution;

[0077] (d) Condensation reaction: adding 15 mol of ethylene oxide to the reduction reaction solution, raising the temperature to 55°C, and reacting for 4 hours;

[0078] (e) Hydrolysis and esterif...

Embodiment 3

[0081] The method for synthesizing the para-ester provided in Example 3 includes the following steps:

[0082] (a) Sulfonation reaction: After adding 24 mol of oleum to the reaction tank, the temperature is lowered to 12°C, 6 mol of chlorosulfonic acid is added, and after stirring for 3 hours, 10 mol of acetanilide is added, and the reaction temperature is controlled to 20°C. Reaction 5 hour;

[0083] (b) Chlorination reaction: heat the reacted solution to 50°C, add 15 mol of phosphorus pentachloride, and react for 5 hours;

[0084] (c) Reduction reaction: add 10 mol of sodium sulfite, stir uniformly, control the reaction temperature at 30°C, use sodium hydroxide solution to maintain pH=8.0, and react for 3 hours to obtain a reduction reaction solution;

[0085] (d) Condensation reaction: add 13 mol of ethylene oxide to the reduction reaction solution, raise the temperature to 65°C, and react for 5 hours;

[0086] (e) Hydrolysis and esterification reaction: add sulfuric acid for esteri...

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PUM

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Abstract

The invention relates to the technical field of dye intermediates, in particular to a para-ester synthesis method. According to the synthesis method, two reactions of a single sulfonation reaction and chlorination reaction are adopted to replace a chlorylation reaction with chlorosulfonic acid directly used in the traditional reaction; on one hand, the dosage of the chlorosulfonic acid can be reduced, and the production of waste acid is reduced; on the other hand, due to the presence of fuming sulfuric acid, the reactivity of the reacting chlorosulfonic acid and acetanilide can be changed, and the formation of chloroacetanilide by-products can be reduced. In addition, the para-ester synthesis method has the advantages that reaction raw materials are easy to obtain; the reaction condition is mild; the product quality is stable; the method is suitable for large-scale industrial production.

Description

Technical field [0001] The invention relates to the technical field of dye intermediates, in particular to a method for synthesizing para-ester. Background technique [0002] P-aminophenyl-β-hydroxyethyl sulfone sulfate, abbreviated as para-ester, is the most important intermediate for vinyl sulfone reactive dyes, used to synthesize KM, M, KN and other reactive dyes. [0003] At present, traditional production uses acetanilide as a raw material, chlorosulfonic acid for chlorosulfonation, chloroethanol as a condensation agent for condensation, and sulfuric acid for hydrolysis and esterification to obtain a para-ester. Due to the excessive amount of chlorosulfonic acid, which is usually 3 to 5 times the theoretical amount, a large amount of acidic wastewater is generated, which increases the production cost and subsequent treatment costs. Moreover, in the process of chlorosulfonation with only chlorosulfonic acid alone, part of the chlorine atoms are directly connected to the benzen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C317/36
CPCC07C303/08C07C303/12C07C313/04C07C315/00C07C315/04C07C309/46C07C309/88C07C317/40C07C317/36
Inventor 蔡红新
Owner 新乡市锦源化工有限公司
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