Double-rectifying-tower series separation and purification method for recovery of methyl tert-butyl ether-tetrahydrofuran in waste liquid in statins synthesis process

A technology for synthesizing methyl tert-butyl ether and drugs, which is applied in the field of separation and purification of double rectification towers in series, and can solve problems such as solvent waste, economic waste, and environmental pollution

Active Publication Date: 2014-04-09
JIANGSU ALPHA PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In waste solvents, methyl tert-butyl ether and tetrahydrofuran account for a relatively large proportion of solvents, accounting for about 50%-80%. If they are discharged, it will not only cause great pollution to the environment, but also cause economic waste.
However, due to the complexity of the system and numerous azeotropes, high-purity methyl tert-buty

Method used

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  • Double-rectifying-tower series separation and purification method for recovery of methyl tert-butyl ether-tetrahydrofuran in waste liquid in statins synthesis process

Examples

Experimental program
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Effect test

Embodiment 1

[0023] There is a batch of process raw materials, its composition is isoprene 12.3%, methyl tert-butyl ether 51.2%, tetrahydrofuran 17.6%, tert-butyl acetate 18.4%, also contains 0.5% impurities, moisture content 2%. It was added to the I tower at a rate of 0.95 L / h, the reflux ratio was controlled to 2-4, the tower top temperature was controlled to 35° C., and the operating pressure of the whole tower was normal pressure. Through the above operations, a mixed solution of isoprene and water with relatively high purity can be obtained at the top of the tower, and high-purity isoprene can be obtained after layering. The composition of the tower kettle discharge liquid is 3.2% isoprene, 54.2% methyl tert-butyl ether, 20.5% tetrahydrofuran, 21.6% tert-butyl acetate, and the rest are impurities. The discharge from tower I of tower I enters from the middle and lower part of tower II, the feed rate is 0.36L / h, the reflux ratio is controlled at 0.3-1.0, the temperature at the top of t...

Embodiment 2

[0025]There is a batch of process raw materials, the composition of which is 16.5% of isoprene, 48.2% of methyl tert-butyl ether, 16.7% of tetrahydrofuran, 17.8% of tert-butyl acetate, and contains 0.8% of impurities, and the water content is 1.8%. It was added to the I tower at a rate of 0.95 L / h, the reflux ratio was controlled to 2-4, the tower top temperature was controlled to 35° C., and the operating pressure of the whole tower was normal pressure. Through the above operations, a mixed solution of isoprene and water with relatively high purity can be obtained at the top of the tower, and high-purity isoprene can be obtained after layering. The composition of the tower kettle discharge liquid is 3.7% of isoprene, 51.6% of methyl tert-butyl ether, 21.6% of tetrahydrofuran, 22.3% of tert-butyl acetate, and the rest are impurities. The discharge from tower I of tower I enters from the middle and lower part of tower II, the feed rate is 0.36L / h, the reflux ratio is controlled...

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Abstract

The invention discloses a double-rectifying-tower series separation and purification method for recovery of methyl tert-butyl ether-tetrahydrofuran in waste liquid of a statins synthesis process, the method is as follows: leading the waste liquid of the statins synthesis process into a packed tower I, controlling the tower top temperature at 30-40 DEG C for distillation treatment to obtain an isoprene and water mixture from the tower top, and then obtaining isoprene by further layering treatment; leading a tower kettle discharging liquid of the packed tower I into a packed tower II, and controlling the tower top temperature at 50-65 DEG C for distillation treatment to obtain an methyl tert-butyl ether-tetrahydrofuran mixed solvent from the tower top of the packed tower II. According to the method, two packed distillation towers are in series for operation, the separation operation process is low in energy consumption and simple in process, and can improve the recovery rate of the solvent methyl tert-butyl ether-tetrahydrofuran, the economic benefit can be improved, and at the same time the environmental pollution and destruction can be reduced.

Description

technical field [0001] The invention belongs to the field of chemical waste liquids, and in particular relates to a double rectification column series separation and purification process aimed at recovering methyl tert-butyl ether-tetrahydrofuran from waste liquids in the synthesis process of statins. Background technique [0002] In the preparation process of statins, a large amount of solvents such as isoprene, methyl tert-butyl ether, tetrahydrofuran and tert-butyl acetate need to be used, so a large amount of mixed waste liquid of solvents is generated. At normal temperature and pressure, isoprene, methyl tert-butyl ether and tetrahydrofuran are all very volatile substances (boiling points: isoprene is 34°C, methyl tert-butyl ether is 55.2°C, tetrahydrofuran is 65.4 ℃), where methyl tert-butyl ether and tetrahydrofuran will form the lowest azeotrope with the water in the solution, and isoprene will also form the lowest azeotrope with the water in the solution, and will f...

Claims

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Application Information

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IPC IPC(8): B01D3/14B01D3/42
Inventor 漆志文张弛秦磊叶银梅陈立芳尹晓龙徐雪峰
Owner JIANGSU ALPHA PHARM CO LTD
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