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Method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis

A technology of ceftriaxone sodium and a purification method is applied in the field of recovery and purification of acetonitrile and devices used in the synthesis of ceftriaxone sodium, which can solve the problems of reaction influence and the like, and achieves reduced operating energy consumption, high safety factor and simple process. Effect

Active Publication Date: 2015-09-23
JIANGSU NINE HEAVEN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this process, extractant residues will be introduced into the acetonitrile waste liquid, and the residual extractant may have an impact on subsequent reactions

Method used

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  • Method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis
  • Method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis
  • Method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis

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Effect test

Embodiment 1

[0045] The recovery refining method of acetonitrile in ceftriaxone sodium synthesis, the device that adopts is as figure 1 As shown, the operation process includes the following steps: the acetonitrile waste liquid in the synthesis of ceftriaxone sodium is preheated by the preheater 1 and then enters the first rectification tower 2 for rectification and concentration. After concentration, the acetonitrile content is increased to 80 wt. %, the obtained acetonitrile distillate is transported to the neutralization tank 3, and the organic heavy components and part of the water are discharged from the bottom of the tower. In the neutralization tank 3, add a certain amount of lye to neutralize the acidic substances in the acetonitrile distillate. The neutralized acetonitrile distillate in the neutralization tank 3 is controlled flow rate to be 900 kg / h and sent to the second rectification column 4 for rectification and impurity removal, and the acetonitrile distillate is removed fr...

Embodiment 2

[0051] The recovery refining method of acetonitrile in ceftriaxone sodium synthesis, the device that adopts is as figure 1 As shown, the operation process comprises the following steps: the acetonitrile waste liquid in the synthesis of ceftriaxone sodium enters the first rectification tower 2 rectification and concentrates after the preheater 1 is preheated, and the acetonitrile content is respectively improved to 70, 75, 80, 84 wt.%, the obtained acetonitrile distillate is transported to the neutralization tank 3, and the organic heavy components and part of the water are discharged from the bottom of the tower. In the neutralization tank 3, add a certain amount of lye to neutralize the acidic substances in the acetonitrile distillate. The neutralized acetonitrile distillate control flow in the neutralization tank 3 is that 1500 kg / h is delivered to the second rectification column 4 for rectification and impurity removal, and the acetonitrile distillate is removed from the s...

Embodiment 3

[0057] The recovery refining method of acetonitrile in ceftriaxone sodium synthesis, the device that adopts is as figure 1 As shown, the operation process includes the following steps: the acetonitrile waste liquid in the synthesis of ceftriaxone sodium is preheated by the preheater 1 and then enters the first rectification tower 2 for rectification and concentration. After concentration, the acetonitrile content is respectively increased to 80 wt .% or so, the obtained acetonitrile distillate is transported to the neutralization tank 3, and the organic heavy components and part of the water are discharged from the bottom of the tower. In the neutralization tank 3, add a certain amount of lye to neutralize the acidic substances in the acetonitrile distillate. The neutralized acetonitrile distillate in the neutralization tank 3 is sent to the second rectifying tower 4 with 1500 kg / h for rectification and impurity removal. The top of the distillation tower is taken out, and th...

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Abstract

The invention relates to a method and device for recycling and refining acetonitrile in ceftriaxone sodium synthesis. The method includes the following steps: acetonitrile waste liquid in ceftriaxone sodium synthesis is fed into a first rectifying tower, and parts of water and heavy components are removed in a rectifying mode; rectified acetonitrile liquid is obtained after concentrating is carried out and fed into a neutralization tank for pH value adjustment; the neutralized rectified acetonitrile liquid is fed into a second rectifying tower for further impurity removing, the rectified acetonitrile liquid enters a pervaporation membrane separation unit after impurities are removed in the second rectifying tower, residual liquid in a kettle is returned to the first rectifying tower, and the acetonitrile in the residual liquid is recycled; the crude acetonitrile is obtained after the liquid is separated through the pervaporation membrane separation unit, water and a small amount of acetonitrile in a solution on the feed liquid side permeate a pervaporation membrane in a steam mode to obtain permeating liquid, the permeating liquid is condensed to be returned to the neutralization tank, and the acetonitrile in the permeating liquid is recycled; the crude acetonitrile obtained through the pervaporation membrane separation unit is fed into a third rectifying tower to be refined, the finished acetonitrile is obtained, acetonitrile-water azeotrope obtained after rectifying of the third rectifying tower is returned to the second rectifying tower, and the acetonitrile in the acetonitrile-water azeotrope is recycled.

Description

technical field [0001] The invention relates to a method and device for recovering and refining acetonitrile in the synthesis of ceftriaxone sodium, which belongs to the application field of pervaporation membranes. Background technique [0002] Ceftriaxone sodium is a broad-spectrum long-acting antibiotic launched by Swiss Roche Company in 1982. It has a small dosage, low toxicity and side effects, and has a large market share. It is the third-generation cephalosporin with broad-spectrum antibacterial activity. In actual production, when the crude product of ceftriaxone sodium is produced from the raw material 7-ACA, acetonitrile is used as a solvent for the reaction. After the reaction is over, the acetonitrile mother liquor produced is separated to obtain a certain quality index of reclaimed acetonitrile and is used again as a reaction solvent for recycling. In the production process, acetonitrile is inevitably mixed with water and other impurities to produce acetonitr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/34C07C255/03
Inventor 郭海超余从立顾学红庆祖森
Owner JIANGSU NINE HEAVEN HIGH TECH
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