Method for preparing 4-aminophenyl-beta-hydroxyethyl sulfone sulfate

A technology of hydroxyethyl sulfone and aminophenyl, applied in the field of preparation of sulfate, can solve the problems of high environmental protection cost, excessive chlorosulfonic acid, etc., and achieves the effects of easy handling, pure color and low production

Inactive Publication Date: 2008-09-03
HEILONGJIANG INST OF PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing 4-aminophenyl-β-hydroxyethyl sulfone sulfate in order to solve the problems of a large amount of excessive chlorosulfonic acid used in the preparation of para-esters and high environmental protection costs.

Method used

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specific Embodiment approach 1

[0008] Specific embodiment one: the preparation method steps of 4-aminophenyl-beta-hydroxyethyl sulfone sulfate in the present embodiment are as follows: one, with beta-mercaptoethanol and p-nitrohalobenzene according to the ratio of 1~1.5:1 The molar ratio is dissolved in the solvent, and the temperature is raised to 30-50°C while stirring, and then the temperature is controlled at 30-50°C, and the acid-binding agent is added dropwise within 2-4 hours, and the reaction is kept for 2-6 hours. 20-37% hydrochloric acid makes the reaction solution neutral, then suction filtration, vacuum distillation, hot water washing three times, after liquid separation, 4-nitrophenyl-β-hydroxyethyl sulfide is obtained; two, the 4- After mixing nitrophenyl-β-hydroxyethyl sulfide, catalyst and water, add the oxidant dropwise at 30-100°C for 2-4 hours, then stir at constant temperature for 2-4 hours, then cool to room temperature. Add a sodium carbonate solution with a mass concentration of 10-20...

specific Embodiment approach 2

[0009] Embodiment 2: This embodiment is different from Embodiment 1 in that the molar ratio of β-mercaptoethanol to p-nitrohalobenzene in step 1 is 1.1:1. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0010] Embodiment 3: This embodiment is different from Embodiment 1 in that the molar ratio of β-mercaptoethanol to p-nitrohalobenzene in step 1 is 1.4:1. Others are the same as in the first embodiment.

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Abstract

The invention relates to a preparation method for 4-(beta-sulfatoethyl sulfone sulfonyl) aniline, and relates to a preparation method for a sulfuric ester. The invention solves the problems that chlorosulfonic acid is greatly overused and environmental protection cost is high in the preparation process of para-ester at present. The preparation method of the invention comprises: condensing nitro halogeno benzene and beta-mercaptoethanol to produce 4-(beta-sulfatoethyl sulfone sulfide) nitrobenzene, adding hydrogen peroxide in aqueous medium after separating out dissolvent, water and salts to produce 4-nitrobenz-beta-hydroxyethyl sulfone by catalytic oxidation, deoxidizing nitro of 4-nitrobenz-beta-hydroxyethyl sulfone to be amino by catalytic hydrogenation reaction, and homogeneously esterifying with sulfuric acid to obtain the product. The method does not use chlorosulfonic acid, generation amount of waste waters is little and easy to treat, by-product is few and easy to separate. The purity of the product is high, the amino number and ester number are higher than 97. 0and 95. 0respectively, the difference between the two number is less than 2, and the product has light color and pure tint.

Description

technical field [0001] The present invention relates to a kind of preparation method of sulfuric acid ester. Background technique [0002] 4-Aminophenyl-β-hydroxyethyl sulfone sulfate, referred to as p-ester, is an important intermediate of ethyl sulfone reactive dyes. The early synthesis method of para-ester is to use acetanilide as raw material, undergo chlorosulfonation, condensation, use chlorohydrin as condensation agent, add sulfuric acid to hydrolyze and esterify to obtain para-ester. The disadvantages of this process are: the yield of chlorosulfonation is low, a large amount of chlorosulfonic acid is excessive, it is difficult to recycle, a large amount of acid-containing wastewater is produced, and the equipment is severely corroded; chlorohydrin is used as a condensation agent, the reaction temperature is high, there are many by-products, and the yield is low. Also on the low side; using sulfuric acid hydrolysis, frying and dry esterification, uneven heating, larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/34C07C315/02C07C315/04
Inventor 田勇韩大维胡永玲黎庆张秀斌王焕民
Owner HEILONGJIANG INST OF PETROCHEM
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