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Adsorption process for removing low content water from tetrahydrofuran-methanol mixed solvent during production of statin drugs

A technology of tetrahydrofuran and mixed solvents, which is applied in the field of low-content water adsorption method and its device, can solve the problems of high-efficiency application in the chemical industry, low adsorption performance, poor exchange degree, etc., to improve the reuse rate, reduce pollution and Effects of destroying and reducing waste discharge

Active Publication Date: 2015-06-03
JIANGSU ALPHA PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, molecular sieves sold on the market generally have problems such as low adsorption performance, poor exchange rate, and easy breakage during the heating and cooling process, which affects their efficient application in the chemical industry.

Method used

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  • Adsorption process for removing low content water from tetrahydrofuran-methanol mixed solvent during production of statin drugs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] There is a batch of solvents, the composition of which is 61.5% methanol, 35% THF, 3% water, and the rest are solvents with high boiling point impurities. Add caustic soda in a proportion of 6% (mass ratio), stir and filter to remove solid impurities, and then Enter the rectification tower at a rate of 300kg / hr to remove heavy component impurities and further concentrate, and the obtained mixed solution containing only methanol-tetrahydrofuran-water enters the adsorption tower. Control the adsorption temperature of the adsorption tower below 60°C, and control the overall liquid phase residence time for 3 hours to obtain a tetrahydrofuran-methanol product with a water content below 500ppm at the top of the tower.

[0025] Sampling is continued on the outlet pipeline at the top of the tower. When the moisture content of the product exceeds the standard, the liquid phase feed is closed, the nitrogen / air pipeline at the top of the tower is opened, and the liquid phase materi...

Embodiment 2

[0029] There is a batch of solvents, the composition of which is 31.6% methanol, 67.2% THF, 1% water, and the rest are solvents with high boiling point impurities. Add caustic soda in a proportion of 6% (mass ratio), stir and filter to remove solid impurities, and then Enter the rectification tower at a rate of 300kg / hr to remove heavy component impurities and further concentrate, and the obtained mixed solution containing only methanol-tetrahydrofuran-water enters the adsorption tower. Control the adsorption temperature of the adsorption tower below 60°C, and control the overall liquid phase residence time for 1 hr to obtain a tetrahydrofuran-methanol product with a water content below 500ppm at the top of the tower. Sampling is continued on the outlet pipeline at the top of the tower. When the moisture content of the product exceeds the standard, the liquid phase feed is closed, the nitrogen / air pipeline at the top of the tower is opened, and the liquid phase material remaini...

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Abstract

The invention discloses an adsorption process for removing low content water from a tetrahydrofuran-methanol mixed solvent during production of statin drugs. The process includes: taking an adsorption tower as core separation equipment, using a 4A modified zeolite molecular sieve, introducing a mixed solvent containing only methanol-tetrahydrofuran into the adsorption tower, taking the 4A modified zeolite sieve as an adsorbent, performing an adsorption treatment at 20-60DEG C, thus obtaining a tetrahydrofuran-methanol product with a water content of less than 500ppm. Specifically, the mixed solvent has a water content of 0.1-3wt%. The process provided in the invention adopts the adsorption tower and combines the adsorbent for recycling, can remove water from the solvent, and can decrease the content of water in the solvent to less than 500ppm so as to obtain a high purity product. And the product can be recycled in a drug synthesis process, thus greatly improving the usage rate and economic benefits of the tetrahydrofuran solvent and reducing waste emission.

Description

technical field [0001] The invention belongs to the field of solvent separation, and in particular relates to an adsorption method and a device for removing low-content water in tetrahydrofuran-methanol mixed solvents in the production process of statin drugs. Background technique [0002] In the production process of statin drugs, solvents such as tetrahydrofuran and methanol are usually used in large quantities, resulting in mixed waste liquid of solvents. During use, the solvent will be mixed with water due to hydrolysis and other steps, which cannot meet the solvent circulation requirements for the production of statins. Therefore, the recycled solvent needs to be refined and dehydrated before it can be recycled. But under normal temperature and pressure, water will form azeotrope with tetrahydrofuran, and tetrahydrofuran accounts for 95% in the azeotropic composition, and water accounts for about 5%, and it is difficult to remove moisture by using conventional rectific...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/08C07C31/04C07C29/76B01J20/16B01J20/30
Inventor 漆志文张弛尹晓龙陈立芳叶银梅徐春涛徐雪峰
Owner JIANGSU ALPHA PHARM CO LTD