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Method for preparing high-purity 4-hydroxyethyl piperazine ethane sulfonic acid

A technology of hydroxyethylpiperazine ethanesulfonic acid and hydroxyethylpiperazine is applied in the field of preparation of high-purity 4-hydroxyethylpiperazine ethanesulfonic acid, and can solve environmental pollution, consumption of large acids and bases, and high cost problem, to achieve the effect of simple operation process, low purification cost and simple process

Active Publication Date: 2015-07-29
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem that this method exists is: (1) produces a large amount of difficult-to-handle saline waste water in the production process, and environmental pollution is serious; (2) ion-exchange resin needs repeated regeneration, consumes a large amount of acid and alkali; (3) obtains the product The purity is not high enough, and further separation and purification are needed; (4) the purification amount per unit mass of ion exchange resin is low, and the life is short, so the cost is high

Method used

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  • Method for preparing high-purity 4-hydroxyethyl piperazine ethane sulfonic acid
  • Method for preparing high-purity 4-hydroxyethyl piperazine ethane sulfonic acid
  • Method for preparing high-purity 4-hydroxyethyl piperazine ethane sulfonic acid

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Experimental program
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Effect test

Embodiment 1

[0048] Add 131.5g N-hydroxyethylpiperazine (purity: 99%, about 1mol) and 30% (mass concentration) sodium vinylsulfonate aqueous solution (containing 1.05mol sodium vinylsulfonate) into 1000mL four Addition reaction was carried out under sufficient stirring; first reacted at 60°C for 1.0 hour, then gradually heated to boiling reflux (about 100-120°C, depending on the composition of the reaction solution), and continued to react for 2.0 hours; then , cooling to obtain a reaction mother liquor containing 4-hydroxyethylpiperazine sodium ethanesulfonate. Through high-performance liquid chromatography analysis, the calculated yield of sodium 4-hydroxyethylpiperazineethanesulfonate was 95.2%.

Embodiment 2

[0050] Add 1 mol N-hydroxyethylpiperazine and 35% (mass concentration) sodium vinyl sulfonate aqueous solution (containing 1.15 mol sodium vinyl sulfonate) into a 1000 mL four-necked flask with a reflux tube, and add them under sufficient stirring. reaction; first react at 50°C for 2.0 hours, then gradually increase the temperature to boil and reflux, and continue to react for 3.0 hours; then, cool down to obtain a reaction mother liquor containing sodium 4-hydroxyethylpiperazineethanesulfonate. Through high performance liquid chromatography analysis, the calculated yield of sodium 4-hydroxyethylpiperazineethanesulfonate was 96.4%.

Embodiment 3

[0052] Add 1mol N-hydroxyethylpiperazine and 30% (mass concentration) vinylsulfonic acid aqueous solution (containing 1.00mol vinylsulfonic acid) into a 1000mL four-necked flask with a reflux tube, and then slowly dropwise add Aqueous sodium hydroxide solution (mass concentration is 30%, containing 1.1mol sodium hydroxide); then react at 40°C for 2.0 hours, then gradually heat up and boil to reflux, and continue to react for 1.5 hours; then, cool down to obtain 4-hydroxyethyl Reaction mother liquor of sodium piperazine ethanesulfonate. Through high-performance liquid chromatography analysis, the calculated yield of sodium 4-hydroxyethylpiperazineethanesulfonate was 87.7%.

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Abstract

The invention belongs to the technical field of organic matter preparation, and particularly relates to a method for preparing high-purity 4-hydroxyethyl piperazine ethane sulfonic acid. The method comprises the following steps: carrying out addition reaction on vinylsulfonic acid or vinyl sulfonate and N-hydroxyethyl piperazine to prepare 4-hydroxyethylpiperazine ethane sulfonate; converting the 4-hydroxyethylpiperazine ethane sulfonate into 4-hydroxyethylpiperazine ethane sulfonic acid and corresponding salts of an acidifier by adopting the acidifier, thus obtaining acidifying mother liquor; then crystallizing to remove the corresponding salts of the acidifier to obtain processed acidifying mother liquor; adding soluble barium salt or calcium salt to the processed acidifying mother liquor to remove residual sulfate radicals, and carrying out evaporative concentration to obtain a primary purified product of the 4-hydroxyethylpiperazine ethane sulfonic acid; finally, washing the primary purified product by adopting small molecular weight alcohol and drying to obtain the high-purity 4-hydroxyethylpiperazine ethane sulfonic acid. The 4-hydroxyethylpiperazine ethane sulfonic acid prepared by the method disclosed by the invention is high in purity, simple and convenient in operation process, environment-friendly in production process, low in purification cost, high in yield and suitable for industrial batch production.

Description

technical field [0001] The invention belongs to the technical field of organic matter preparation, in particular to a method for preparing high-purity 4-hydroxyethylpiperazineethanesulfonic acid. Background technique [0002] 4-Hydroxyethylpiperazineethanesulfonic acid (HEPES) is a hydrogen ion buffer, which has good buffering capacity in the pH range of 6.8-8.2, and can control a constant pH for a long time. The use concentration is about 10-50mmol / L, and the general culture medium contains 20mmol / L HEPES to have a good buffer capacity. [0003] HEPES can be used in cell culture medium, such as the patent application number CN00109662.1 and the patent application number CN201010610401.0 using HEPES as the composition of cell culture medium, effectively obtaining a simple, high stability, good culture effect Cell culture system; HEPES can also be used as a buffer solution, such as the patent application number CN201210171396.7 using HEPES as a buffer for detecting hypochlor...

Claims

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Application Information

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IPC IPC(8): C07D295/088
CPCC07D295/088
Inventor 崔洪友王建刚朱丽伟刘然升杨涌王杨
Owner SHANDONG UNIV OF TECH
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