The synthetic method of para-ester

A synthesis 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, mild reaction conditions, and easy-to-obtain reaction raw materials

Active Publication Date: 2019-01-04
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 synthetic method of the para-position ester that embodiment 1 provides, comprises the steps:

[0066] (a) Sulfonation reaction: After adding 20 mol of fuming sulfuric acid into the reaction tank, cool down to 12°C, add 5mol of chlorosulfonic acid, stir and react for 2 hours, add 10mol of acetanilide, control the reaction temperature to 15°C, and react 4 Hour;

[0067] (b) Chlorination reaction: warming up the reacted solution to 45° C., adding 14 mol of thionyl chloride, and adding carbon tetrachloride as an auxiliary agent, and reacting for 4 hours;

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

[0069] (d) Condensation reaction: Add 15mol of ethylene oxide into the reduction reaction liquid, heat up to 60°C, and react for 4 hours;

[0070] (e) Hydrolysis and esterification reaction: a...

Embodiment 2

[0073] The synthetic method of the para-position ester that embodiment 2 provides, comprises the steps:

[0074] (a) Sulfonation reaction: After adding 15 mol of fuming sulfuric acid into the reaction tank, cool down to 15°C, add 5mol of chlorosulfonic acid, stir and react for 2 hours, add 10mol of acetanilide, control the reaction temperature to 15°C, and react 3 Hour;

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

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

[0077] (d) Condensation reaction: Add 15mol of ethylene oxide into the reduction reaction solution, heat up to 55°C, and react for 4 hours;

[0078] (e) Hydrolysis and esterification reaction: a...

Embodiment 3

[0081] The synthetic method of the para-position ester that embodiment 3 provides, comprises the steps:

[0082] (a) Sulfonation reaction: After adding 24 mol of oleum into the reaction tank, cool down to 12°C, add 6mol of chlorosulfonic acid, stir and react for 3 hours, add 10mol of acetanilide, control the reaction temperature to 20°C, and react 5 Hour;

[0083] (b) Chlorination reaction: the solution after the reaction is warmed up to 50°C, and 15mol of phosphorus pentachloride is added, and reacted for 5 hours;

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

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

[0086] (e) Hydrolysis and esterification reaction: add sulfuric acid to carry out esterification...

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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 synthesis method of a para-ester. Background technique [0002] p-Aminophenyl-β-hydroxyethyl sulfone sulfate, referred to as para-ester, is the most important intermediate of vinylsulfone reactive dyes, and is used to synthesize reactive dyes such as KM type, M type and KN type. [0003] At present, the traditional production is to use acetanilide as raw material, use chlorosulfonic acid for chlorosulfonation, chloroethanol as condensation agent for condensation, add sulfuric acid for hydrolysis and esterification to obtain para-ester. 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. Moreover, in the process of chlorosulfonation with chlorosulfonic acid alone, part of the chlorine atoms are directly connect...

Claims

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Application Information

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Patent Type & Authority Patents(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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