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Combined method for extracting piperazine

A combined, piperazine technology, applied in the field of combined extraction of piperazine, can solve the problems of light yellow color of piperazine, high energy consumption, many by-products, etc.

Inactive Publication Date: 2015-12-23
WUXI QIAOYANG MACHINERY MFG
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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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Inject the piperazine reaction liquid into the distillation tower, open the steam generator at the bottom of the tower, send water vapor with a temperature of 200-250°C from the bottom of the tower into the distillation tower, and send the piperazine reaction liquid into the distillation tower from the liquid inlet at the top of the tower Inside, the water vapor at the bottom of the tower heats the mixed liquid at the top of the tower, the temperature at the top of the tower is 140-155°C, the reflux ratio of the distillation tower is 2, the steam condensate is collected in the top reflux device, and the condensate is pumped into the supercritical Extraction tower, the extraction agent is glycerol, the operating pressure is 12-25MPa, the extraction temperature is 147-149°C, and the fraction piperazine is extracted to obtain the piperazine product; the piperazine reaction liquid is obtained by ethylenediamine and ammonia Reaction solution obtained by preparing piperazine. ...

Embodiment 2

[0011] Inject the piperazine reaction liquid into the distillation tower, open the steam generator at the bottom of the tower, send water vapor with a temperature of 200-250°C from the bottom of the tower into the distillation tower, and send the piperazine reaction liquid into the distillation tower from the liquid inlet at the top of the tower Inside, the water vapor at the bottom of the tower heats the mixed liquid at the top of the tower, the temperature at the top of the tower is 140-155°C, the reflux ratio of the distillation tower is 4, the steam condensate is collected in the top reflux device, and the condensate is pumped into the supercritical Extraction tower, the extraction agent is glycerol, the operating pressure is 12-25MPa, the extraction temperature is 147-149°C, and the fraction piperazine is extracted to obtain the piperazine product; the piperazine reaction liquid is obtained by ethylenediamine and ammonia Reaction solution obtained by preparing piperazine. ...

Embodiment 3

[0013] Inject the piperazine reaction liquid into the distillation tower, open the steam generator at the bottom of the tower, send water vapor with a temperature of 200-250°C from the bottom of the tower into the distillation tower, and send the piperazine reaction liquid into the distillation tower from the liquid inlet at the top of the tower Inside, the water vapor at the bottom of the tower heats the mixed liquid at the top of the tower in countercurrent, the temperature at the top of the tower is 140-155°C, the reflux ratio of the distillation tower is 5, the steam condensate is collected in the top reflux device, and the condensate is pumped into the supercritical Extraction tower, the extraction agent is glycerol, the operating pressure is 12-25MPa, the extraction temperature is 147-149°C, and the fraction piperazine is extracted to obtain the piperazine product; the piperazine reaction liquid is obtained by ethylenediamine and ammonia Reaction solution obtained by prep...

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PUM

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Abstract

The present invention discloses a combined method for extracting piperazine. The method comprises the steps of: pouring a piperazine reaction solution into a distillation column; opening a steam generator at the bottom; feeding water vapor at the temperature of 200-250 DEG C from the column bottom; sending the piperazine reaction solution from a liquid inlet on the top of the distillation column; conducting countercurrent heating on the mixed solution on column top by water vapor at the column bottom, wherein the column top temperature is 140-155 DEG C, and a reflux ratio of the distillation column is 2.5-12; collecting steam condensate in a reflux device at the column top; pumping the condensate into a supercritical extraction tower; extracting a fraction piperazine under the conditions of an extraction agent of glycerin, operating pressure of 12-25 MPa and extraction temperature of 147-149 DEG C, so as to obtain the piperazine product. The piperazine reaction solution is obtained from the reaction of ethylenediamine with ammonia for preparing piperazine. The preparation method of piperazine has the advantages of high separation efficiency, high product purity and pure white color of the product.

Description

technical field [0001] The invention relates to a combined method for extracting piperazine. Background technique [0002] Piperazine is an important intermediate required by industries such as medicine, pesticides, dyes, etc. The main raw material of Shaxing. At the same time, it can also be used in synthetic resins, synthetic fibers, and the production of surfactants, etc. [0003] The raw materials for synthesizing piperazine can be amino compounds such as aminoethanol, ethylenediamine, diethylenetriamine, etc. Therefore, according to different raw materials, piperazine has multiple synthetic routes, and the main synthetic processes include dichloroethane method, ethanolamine method, The ethylenediamine method, wherein the ethanolamine method and the ethylenediamine method are a kind of relatively advanced synthesis technology generally adopted at home and abroad. There are many by-products in the reaction solution of the synthetic product, and the boiling point is sim...

Claims

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Application Information

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IPC IPC(8): C07D295/023C07D295/027
CPCC07D295/023C07D295/027Y02P20/54
Inventor 沈秋
Owner WUXI QIAOYANG MACHINERY MFG