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Method for refining piperazine

A piperazine and rectifying column technology, which is applied in the field of refining piperazine, can solve the problems of light yellow color of piperazine, many by-products, affecting use, etc., and achieve the effects of pure white product color, improved production efficiency, and high separation efficiency.

Active Publication Date: 2011-04-06
山西玉龙格兰特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many by-products in the reaction solution of the synthetic product, and the boiling point is similar to that of piperazine, so that the purification of piperazine requires a large number of theoretical plates or a high reflux ratio, which consumes a lot of energy, and the produced piperazine is light yellow in color. Affect the use, some manufacturers adopt recrystallization method, the process is relatively backward, and most of the obtained piperazine contains crystal water

Method used

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  • Method for refining piperazine
  • Method for refining piperazine

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 1000g of piperazine reaction liquid prepared from ethanolamine and ammonia to the bottom of the rectification tower for temperature rise and separation. The reaction liquid in the bottom of the bottom is heated to a temperature of 130°C, the reflux ratio is controlled at 0.2:1, and the fraction at 100°C is collected. 75g of water, continue to heat to 140°C, control the reflux ratio to 2:1, collect 105g of ethylenediamine fraction at 119°C, continue to heat to 160°C, and when the thermometer shows that it reaches 140°C, use a micropump to pump the extractant from the rectification tower The upper extractant inlet is poured into the rectification column, the extractant is ethylene glycol, the reflux ratio is controlled at 3:1, and the ratio of the mass of the extractant added per minute to the mass of piperazine produced per minute is 0.05:1. 641g of piperazine was collected at 148°C, and the purity of piperazine was 99.2% as detected by gas chromatography. The residu...

Embodiment 2

[0019] Add 1000g of piperazine reaction solution prepared from ethanolamine and ammonia to the bottom of the rectification tower for temperature rise and separation. The reaction solution in the bottom of the tower is heated to a temperature of 140°C, the reflux ratio is controlled at 1:1, and 70g of distillate water at 100°C is collected. , continue heating to 150°C, control the reflux ratio to 5:1, collect 110g of distillate ethylenediamine at 119°C, continue heating to 160-170°C, and when the thermometer shows 140°C, use a micropump to pump the extractant from the rectification tower The upper extraction agent inlet is poured into the rectification column, the extraction agent is glycerol, the reflux ratio is controlled at 5:1, and the ratio of the mass of the extraction agent added per minute to the mass of piperazine produced per minute is 0.2:1. The fraction piperazine at 148°C was collected to obtain 640 g of piperazine. The purity of piperazine detected by gas chromatog...

Embodiment 3

[0021] Add 1000g of piperazine reaction solution prepared from ethanolamine and ammonia to the bottom of the rectification tower for temperature rise and separation. The reaction solution in the bottom of the tower is heated to a temperature of 135°C, the reflux ratio is controlled at 0.5:1, and 72g of distillate water at 100°C is collected , continue heating to 145°C, control the reflux ratio to 3:1, collect 108g of distillate ethylenediamine at 119°C, continue heating to 165°C, and when the thermometer shows 140°C, use a micropump to pump the extractant from the upper part of the rectification tower The inlet of the extractant is poured into the rectification column, the extractant is 1,5-pentanediol, the reflux ratio is controlled at 4:1, and the ratio of the mass of the extractant added per minute to the mass of piperazine produced per minute is 0.1: 1. Collect 646g of piperazine at 148°C, and the purity of piperazine detected by gas chromatography is 99.1%. The residual m...

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Abstract

The invention discloses a method for refining piperazine, which comprises the following steps of: adding piperazine reaction liquid in a tower of a rectifying column for heating separation; heating the reaction liquid in the tower to 130 DEG C-140 DEG C, controlling the reflux ratio to be 0.2-1:1, collecting 100 DEG C fractional water; continuing to heat to 140 DEG C -150 DEG C, controlling reflux ratio to be 2-5:1, collecting 119 DEG C fractional ethylene diamine; continuing to heat to 160 DEG C -170 DEG C, pumping an extraction agent into the rectifying column from an extraction agent inlet at the upper part of the rectifying column by using a microinfusion pump when the scale of a thermometer shows 140 DEG C, wherein the extraction agent is one of dihydric alcohol or triatomic alcohol of C2-C5; and controlling the reflux ratio to be 3-5:1, controlling the ratio of addition mass of the extraction agent per minute to extraction mass of piperazine per minute to be 0.05-0.2:1, and collecting 148 DEG C fractional piperazine which is pure piperazine. The method can improve the purity of the product and the separation efficiency and also can greatly reduce production cost since the extraction agent can be reused after being separated simply.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of fine chemicals, and specifically relates to a method for refining piperazine from a reaction liquid after synthesizing piperazine with ethylenediamine or ethanolamine and ammonia as raw materials. Background technique [0002] Piperazine, also known as hexahydropiperazine, is an important fine organic chemical intermediate in the pharmaceutical industry, from which piperazine phosphate, piperazine sulfate, norfloxacin, pipemidic acid, quinolones, rifampicin, etc. can be synthesized: piperazine Zinc is also widely used in synthetic resins, synthetic fibers, surfactants, antioxidants, preservatives, stabilizers, vulcanization accelerators, textile printing and dyeing auxiliaries, corrosion inhibitors, defoamers, cosmetic emulsifiers and coatings and other fields. [0003] The raw materials for synthesizing piperazine can be amino compounds such as aminoethanol, ethylenediamine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/027C07D295/023
Inventor 王伟吕剑杨建明赵锋伟郝志军曾纪珺淡保松
Owner 山西玉龙格兰特化工有限公司
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