Method for producing amino-phenyl-beta-hydroxyethyl sulfone sulfate

A technology of hydroxyethylsulfone and p-aminophenyl, which is applied in the field of production of aminophenyl-β-hydroxyethylsulfone sulfate, can solve the problems of low product yield, consumption of raw materials and three wastes, and reduce production costs , Conducive to popularization and application, low production cost

Active Publication Date: 2009-09-09
KAIFENG LONGXING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to overcome the shortcomings of the current process such as low product yield, high consumption of raw materials and large output of three wastes, it is necessary to develop a more economical production method to replace the existing process

Method used

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  • Method for producing amino-phenyl-beta-hydroxyethyl sulfone sulfate
  • Method for producing amino-phenyl-beta-hydroxyethyl sulfone sulfate
  • Method for producing amino-phenyl-beta-hydroxyethyl sulfone sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment one: see figure 1 , the production technology of p-aminophenyl-beta-hydroxyethyl sulfone sulfate, comprises the steps:

[0034] (1) Add N,N dimethylformamide (DMF) to reactor 1, then add p-nitrochlorobenzene and mercaptoethanol, dissolve and mix well, then slowly add solid sodium hydroxide, p-nitrochlorobenzene , mercaptoethanol, N, N dimethylformamide, and the molar ratio of solid sodium hydroxide are 1:1-1.2:1.5-2:1, and the solid sodium hydroxide is controlled to be added within 3-5h. Then react with sodium for 3-5h to obtain the reaction product, and the reaction temperature is controlled at 50-80°C;

[0035] Filter the reaction product through filter pool 2 at a temperature lower than 40°C to remove solid NaCl to obtain the filtrate; the filtrate enters the vacuum distillation kettle 3, and distills the filtrate under reduced pressure at 60-150mmHg and 120-150°C for 1-2h , the vacuum still 3 is connected with the vacuum tank 5 through the condenser 4, ...

Embodiment 2

[0042] Embodiment two: see figure 1 , same as embodiment 1 step, difference is process parameter, specifically as follows:

[0043] (1) The molar ratio of p-nitrochlorobenzene, mercaptoethanol, DMF and solid sodium hydroxide in the reactor 1 is 1:1:1.5:1, and the solid sodium hydroxide is controlled to be added within 3-4h, and hydrogen is added Sodium oxide is then reacted for 3-4 hours to obtain the reaction product; the reaction temperature is controlled at 50-60°C;

[0044] The reaction product is filtered through the filter pool 2 at a temperature of 38°C, and the filtrate is obtained after removing solid NaCl; the filtrate enters the vacuum still 3, and the filtrate is distilled under reduced pressure at 60-80mmHg and 120-130°C for 1.5h;

[0045] (2) The reaction temperature of oxidation kettle 6 is 80-90° C., and the continuous addition time of hydrogen peroxide is controlled within 2-3 hours. The molar ratio of hydrogen peroxide and p-nitrophenyl-β-hydroxyethyl sulfi...

Embodiment 3

[0050] Embodiment three: see figure 1 , same as embodiment 1 step, difference is process parameter, specifically as follows:

[0051] (1) The molar ratio of p-nitrochlorobenzene, mercaptoethanol, DMF, and solid sodium hydroxide in the reactor 1 is 1: 1.2: 2: 1, and the solid sodium hydroxide is controlled to be added within 3-5h, and hydrogen is added Sodium oxide is then reacted for 3-5 hours to obtain the reaction product; the reaction temperature is controlled at 70-80°C;

[0052] The reaction product is filtered through the filter tank 2 at a temperature of 30° C., and the filtrate is obtained after removing solid NaCl; the filtrate enters the vacuum still 3, and the filtrate is distilled under reduced pressure at 90-120 mmHg and 130-140° C. for 2 hours;

[0053] (2) Add p-nitrophenyl-β-hydroxyethyl sulfide and sodium tungstate to the oxidation kettle 6, then slowly add hydrogen peroxide and stir, the temperature is controlled at 90-100°C, and the continuous addition time...

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Abstract

The invention relates to a method for producing amino-phenyl-beta-hydroxyethyl sulfone sulfate. The method comprises: nitrochlorobenzene and mercaptoethanol are added into DMF and then slowly added with sodium hydroxide, and the mol ratio among the nitrochlorobenzene, the mercaptoethanol, the DMF and the sodium hydroxide is 1:1-1.2:1.5-2:1; after the sodium hydroxide is added, the reaction lasts for 3-5h at the temperature of 50-80 DEG C; the preliminary product is obtained by reduced pressure distillation; the preliminary product, tungstate and hydrogen peroxide are added into an oxidation pot to react for 1-3h at the temperature of 95-100 DEG C, and oxidized crystallizing material is separated out by cooling, crystallizing and vacuum filtration; after that, the obtained oxidized crystallizing material is treated by hydrogenation reaction and esterification reaction, so that the amino-phenyl-beta-hydroxyethyl sulfone sulfate is obtained. The yield coefficient of the product reaches about 85%, and byproducts such as sodium chloride as well as three wastes which are waste acid, waste water and the like are less; as the quantity of the waste water is reduced to 1-2 t from 6-8 t produced by using the original product, the method reduces the production cost and is beneficial to promotion and application.

Description

1. Technical field: [0001] The invention relates to a production method of reactive dye intermediates, in particular to a production method of aminophenyl-β-hydroxyethyl sulfone sulfate. 2. Background technology: [0002] At present, the production process of p-aminophenyl-β-hydroxyethyl sulfone sulfate is synthesized by raw materials such as p-acetanilide, chlorosulfonic acid, sodium metabisulfite, sodium hydroxide, ethylene oxide, sulfuric acid, etc. The synthesis process includes Follow the steps below: [0003] A. Sulfonation process: first add the measured chlorosulfonic acid into the sulfonation kettle, then put the measured antipyretic ice into the sulfonation kettle for reaction (the design chlorosulfonic acid is excessive), and the sulfonation reaction is an exothermic reaction , When cooling, use ice brine below -10°C to cool down and control the temperature through the jacketed reactor to make the reaction go smoothly. A large amount of hydrogen chloride gas is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 苗建三李仲军任明安
Owner KAIFENG LONGXING CHEM
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