A kind of preparation method of p-aminobenzene-beta-hydroxyethyl sulfone sulfate

A technology of hydroxyethyl sulfone and p-aminobenzene, which is applied in the field of preparation of p-aminobenzene-β-hydroxyethyl sulfone sulfate, can solve the problems of product quality and yield gap, and achieve increased yield and product quality , to achieve the effect of cost control

Active Publication Date: 2019-06-28
新乡市锦源化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The production history of para-ester in my country has been more than 50 years. Although the production process has been improved in recent years, the product quality and yield still have a large gap compared with foreign products.

Method used

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  • A kind of preparation method of p-aminobenzene-beta-hydroxyethyl sulfone sulfate
  • A kind of preparation method of p-aminobenzene-beta-hydroxyethyl sulfone sulfate
  • A kind of preparation method of p-aminobenzene-beta-hydroxyethyl sulfone sulfate

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preparation example Construction

[0037] Specifically, the steps of the preparation method of the present invention are as follows:

[0038] After reducing p-nitrochlorobenzene, it reacts and condenses with chloroethanol, then after the acylation reaction, catalyzes oxidation, and finally esterifies to obtain p-aminobenzene-β-hydroxyethyl sulfone sulfate;

[0039] By increasing the steps of the acylation reaction, the intermediate product can be made more stable, thereby further improving the quality of the product.

[0040] Preferably, the method steps of the present invention are as follows:

[0041] (i) Add water in p-nitrochlorobenzene, preferably, the mass ratio of p-nitrochlorobenzene and water is 50:100~110, more preferably, the mass ratio of p-nitrochlorobenzene and water is 50: 110;

[0042] Then, heat up and stir, and preferably heat up to 101-102°C;

[0043] Then, drop sodium sulfide solution, preferably, the mass percent of sodium sulfide solution used is 20~25%; More preferably, the mass percen...

Embodiment 1

[0080] (i) Add 50g of p-nitrochlorobenzene in the reaction kettle, then add 110g of water, stir and heat up to 101-102°C, start to add 60g of sodium sulfide solution (22%) dropwise, and the dropping time is controlled at 2-3 hours , after the dropwise addition is completed, the temperature of the reaction solution is controlled at 104-105°C;

[0081] Continue the reaction for 10 hours, then change the reflux device to a distillation device, distill out the by-product (a small amount of p-chloroaniline) at 106-108°C until the distillate is colorless, cool the reaction liquid to 5°C and filter, and collect the filtrate;

[0082] (ii) Move the filtrate obtained in step (i) into a reactor, add 80 g of chloroethanol (40%) at room temperature (cooled in a water bath) and stir for 1 hour, slowly add 40 mL of 36% hydrochloric acid, and stir for another 1 hour, and the reaction ends;

[0083] Pour the reaction solution into a 1000mL separatory funnel and let it stand for layering to se...

Embodiment 2

[0088] Prepare p-aminobenzene-β-hydroxyethyl sulfone sulfate with reference to the method of Example 1, wherein, in the step (i) of Example 2, the amount of water is 80g.

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Abstract

The invention provides a preparation method of p-aminobenzene-beta-hydroxyethylsulfone sulfate. In the preparation method, parachloronitrobenzene is used as a raw material, and is subjected to reaction steps of reduction, condensation, acylation, catalytic oxidation, esterification and the like, and therefore, the p-aminobenzene-beta-hydroxyethylsulfone sulfate which is high in yield and high in quality can be prepared.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of p-aminobenzene-β-hydroxyethyl sulfone sulfate. Background technique [0002] Since the advent of reactive dyes, they have developed into important dyes for cellulose fiber applications. With the development and progress of synthetic technology, the research on reactive dyes has also made great progress, and has developed from early chlorinated triazines and homogenized triazines to reactive dyes containing vinylsulfone groups and halogenated pyrimidines, especially It is p-, m-β-hydroxyethylsulfate. Since β-hydroxyethylsulfate is a temporary water-soluble group, it can not only improve the solubility of dyes when they are applied, but also contain hydroxyethylsulfate during dyeing. Reactive dyes have low affinity to fibers and can achieve level dyeing effect; react with fibers to form dye-fiber ether bonds, which have good acid resistance and thermal stab...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/04C07C317/40
CPCC07C315/02C07C315/04C07C319/02C07C319/14C07C319/20C07C317/40C07C323/41C07C323/34
Inventor 樊明伟魏艳军蔡红新王元徐周庆闫玲玲
Owner 新乡市锦源化工有限公司
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