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A kind of separation method of n-methylpiperazine and n-ethylpiperazine

A technology of methylpiperazine and ethylpiperazine, which is applied in the field of separation and purification of fine chemicals, can solve the problems of failure to meet the separation requirements and difficulty in meeting the separation requirements, and achieve the effect of solvent recycling and simple operation process

Active Publication Date: 2016-01-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] N-methylpiperazine and N-ethylpiperazine form near-boilers, and it is difficult to reach separation requirements by ordinary rectification. The inventor adopts a rectification tower to carry out N-methylpiperazine and N-ethylpiperazine Separation, the number of theoretical plates in the rectification tower is 20 plates, the reflux ratio is 5:1, and the purity of N-methylpiperazine at the top of the tower is about 70%, which does not meet the separation requirements

Method used

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  • A kind of separation method of n-methylpiperazine and n-ethylpiperazine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Crude material N-methylpiperazine and N-ethylpiperazine are pumped into the azeotrope column B3 with the crude product feed pump B2, and the feed position is at 10 theoretical plates, and the azeotrope feed pump B1 is used to feed the azeotrope The boiling agent is injected into the azeotropic column B3, the entrainer is toluene, the feed position is 10 theoretical plates, the mass ratio of the entrainer to the crude material is 1:1, and the number of theoretical plates of the azeotropic column is not less than 30 theoretical trays, the reflux ratio is 0.1:1, the operating pressure is 0.1atm, N-ethylpiperazine is extracted from the tower kettle by the N-ethylpiperazine product pump B4, and filled after being cooled by the condenser B5. The top material of the azeotropic tower is separated by the phase separator B6, the upper entrainer is circulated back to the azeotrope tower through the entrainer circulation pump B7, and the crude N-methylpiperazine in the lower layer i...

Embodiment 2

[0018] The same operation as in Example 1, the crude feed position is the 13th theoretical plate, the entrainer is m-xylene, the feed position is the 13th theoretical plate, the quality of the entrainer and the crude The ratio is 3:1, the number of theoretical plates of the azeotropic column is 35 theoretical plates, the reflux ratio is 4:1, the operating pressure is 0.5 atm, and the feeding position of the N-methylpiperazine crude product in the lower layer of the phase separator is 12 At the theoretical plate, the theoretical plate number of the purification tower is 25 theoretical plates, the reflux ratio is 2:1, and the operating pressure is 0.5 atm. The purity of N-methylpiperazine and N-ethylpiperazine determined by gas chromatography was 99.6% and 99.3%, respectively.

Embodiment 3

[0020] The same operation as in Example 1, the crude feed position is the 15th theoretical plate, the entrainer is mesitylene, the feed position is the 15th theoretical plate, the quality of the entrainer and the crude The ratio is 1:1, the number of theoretical plates of the azeotropic column is 30 theoretical plates, the reflux ratio is 0.1:1, the operating pressure is 1 atm, and the feeding position of the N-methylpiperazine crude product in the lower layer of the phase separator is 15 theoretical plates At the tray, the number of theoretical trays in the purification tower is 30 theoretical trays, the reflux ratio is 0.1:1, and the operating pressure is 1 atm. The purity of N-methylpiperazine and N-ethylpiperazine determined by gas chromatography was 99.8% and 99.8%, respectively.

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Abstract

The invention discloses a N-methyl piperazine and N-ethyl piperazine separation method; an azeotropic agent is used for separation of N-methyl piperazine and N-ethyl piperazine in an azeotrope tower, the N-ethyl piperazine is collected in the tower kettle; a N-methyl piperazine azeotrope is collected at the tower top, after phase separation, an upper liquid is cycled back to the azeotrope tower, a lower liquid enters into a solvent recovery tower, and after separation, the N-methyl piperazine is collected from the tower kettle. The separation method has the advantages of simple process and reusable extractant, and is used for the separation of the N-methyl piperazine and the N-ethyl piperazine.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of fine chemicals, and relates to a method for separating N-methylpiperazine and N-ethylpiperazine. Background technique [0002] N-methylpiperazine and N-ethylpiperazine are important derivatives of piperazine. N-methylpiperazine is an important intermediate, which is widely used in medicine, surfactant, synthetic fiber and so on. N-methylpiperazine is an intermediate of the new generation of broad-spectrum antibacterial drugs ofloxacin and clozapine. It is also used in the synthesis of dyes and insecticides, and is also widely used in polymer materials such as plastics and rubber. N-ethylpiperazine is mainly used in the synthesis of enrofloxacin, dyes and plant protection agents, etc. It is also widely used in polymer industries such as plastics and rubber. It can also be used as a human insecticide and antibiotic. Raw materials for repelling roundworms and burning worms. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/023C07D295/03
CPCC07D295/023C07D295/03
Inventor 王伟吕剑毛伟张振华马辉王为强李亚妮杨建明赵峰伟
Owner XIAN MODERN CHEM RES INST
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