Preparation method of p-aminophenyl-beta-ethoxyl sulphone sulphate

A technology of p-aminophenyl and hydroxyethyl sulfone, applied in the field of preparation of p-aminophenyl-β-hydroxyethyl sulfone sulfate, to achieve the effects of reducing the discharge of three wastes, being conducive to environmental protection, and reducing the amount of use

Inactive Publication Date: 2014-03-12
XINXIANG RUICHENG TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved in the present invention is: in order to overcome the defect that the invention patent of application number 200910064706.3 produces p-aminophenyl-β-hydroxyethyl sulfone sulfate, the present invention provides a new p-aminophenyl-β- The preparation method of hydroxyethyl sulfone sulfate, utilize preparation method of the pre

Method used

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  • Preparation method of p-aminophenyl-beta-ethoxyl sulphone sulphate

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Experimental program
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Embodiment 1

[0036] a. First add N,N-dimethylformamide solvent into the reaction kettle, then add p-nitrochlorobenzene and mercaptoethanol to fully dissolve and mix well, then slowly add sodium hydroxide to control the amount of sodium hydroxide After 4 hours of addition, the molar ratio of p-nitrochlorobenzene, mercaptoethanol, N,N-dimethylformamide and sodium hydroxide is 1:1.2:1.5:1; Control the temperature at 70±2°C, react for 4.0 hours under this temperature condition, and obtain the reaction product after the reaction is completed; filter the obtained reaction product through a filter pool at a temperature of <40°C, remove the solid NaCl, and obtain the filtrate. The filtrate was distilled under reduced pressure at 80-120mmHg and 130-140°C for 1.5h to distill off water and N,N-dimethylformamide to obtain p-nitrophenyl-β-hydroxyethyl sulfide;

[0037] b. Add the p-nitrophenyl-β-hydroxyethyl sulfide and sodium tungstate catalyst obtained in step a into the oxidation kettle, and slowly ...

Embodiment 2

[0043] In step a: control the addition of sodium hydroxide for 3.5 hours, and the molar ratio of the addition amount of p-nitrochlorobenzene, mercaptoethanol, N,N-dimethylformamide and sodium hydroxide is 1:1.1:1.6 : 1; after the addition of sodium hydroxide, the temperature is controlled to be 75±2°C, and the reaction is carried out at this temperature for 3.5h;

[0044] In step b: the molar ratio between hydrogen peroxide and p-nitrophenyl-β-hydroxyethyl sulfide is 1.05:1, and the addition of sodium tungstate catalyst accounts for 0.3% of the mass of sulfide; during the process of adding hydrogen peroxide, the temperature is controlled at 80-85°C, and the continuous addition time of hydrogen peroxide is 4h; after adding hydrogen peroxide, react at 95-100°C for 2h;

[0045] In step c: repeatedly washing the oxidized crystal material obtained in step b with methanol having a concentration of 20-30% by mass;

[0046] In step d: the mass ratio between the oxidized crystallizati...

Embodiment 3

[0049] In step a: control the addition of sodium hydroxide for 3 hours, the molar ratio of the addition amount of p-nitrochlorobenzene, mercaptoethanol, N,N-dimethylformamide and sodium hydroxide is 1:1.15:2.0: 1. After adding sodium hydroxide, control the temperature to 78-80°C, and react at this temperature for 3 hours; carry out vacuum distillation of the obtained filtrate at 120-150mmHg, 120-130°C for 1.5h;

[0050] In step b: the molar ratio between hydrogen peroxide and p-nitrophenyl-β-hydroxyethyl sulfide is 1.1:1, and the amount of sodium tungstate catalyst added accounts for 0.1% of the mass of sulfide; during the process of adding hydrogen peroxide, the temperature is controlled at 95±2°C, and the continuous addition time of hydrogen peroxide is 5h; after adding hydrogen peroxide, react at 95-100°C for 3h;

[0051] In step c: repeatedly washing the oxidized crystal material obtained in step b with methanol having a concentration of 60-70% by mass;

[0052] In step d...

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Abstract

The invention discloses a preparation method of p-aminophenyl-beta-ethoxyl sulphone sulphate. The preparation method comprises the following steps of: adding p-aminophenyl and mercaptoethanol into an N, N-dimethyl formamide solvent to dissolve, and adding NaOH to carry out reaction; filtering, distilling under reduced pressure to obtain p-aminophenyl-beta-ethoxyl thioether after reaction; adding the p-aminophenyl-beta-ethoxyl thioether and a catalyst into an oxidization kettle, adding hydrogen peroxide to carry out reaction, and cooling and separating out an oxidized and crystallized material after the reaction; washing the oxidized and crystallized material, adding water and a palladium-carbon catalyst after washing to carry out hydrogenation reaction, thus obtaining an hydrogenation product and water after the reaction; adding pure sulfuric acid to carry out esterification reaction, and crushing the obtained product to obtain the p-aminophenyl-beta-ethoxyl sulphone sulphate. In the preparation method disclosed by the invention, dosage of the adopted hydrogen peroxide and the palladium-carbon catalyst is less, especially, dosage of the palladium-carbon catalyst is greatly reduced, so that production cost is greatly lowered; and moreover, output of three wastes is lower, yield is higher, economical benefits and social benefits are remarkable.

Description

technical field [0001] The invention relates to a production method of reactive dye intermediates, in particular to a preparation method of p-aminophenyl-β-hydroxyethyl sulfone sulfate. Background technique [0002] At present, the production method of p-aminophenyl-beta-hydroxyethyl sulfone sulfate is to adopt raw materials such as p-acetanilide, chlorosulfonic acid, sodium pyrosulfite, sodium hydroxide, ethylene oxide, sulfuric acid to synthesize, and its synthesis includes The following steps: [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 (excess chlorosulfonic acid), the sulfonation reaction is an exothermic reaction, When cooling, use ice-salt water 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 produced during the reactio...

Claims

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Application Information

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IPC IPC(8): C07C317/36C07C315/04
Inventor 任龙飞张成立
Owner XINXIANG RUICHENG TECH DEV
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