Recovery and separation method for solvent containing tetrahydrofuran-carbinol system

A technology of tetrahydrofuran and methanol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large solvent loss and the like

Inactive Publication Date: 2013-02-06
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the extractive distillation with pentane as the extractant avoids the disadvantages of benzene extractive distillation, the low boiling point of pentane (36.1°C) requires pressurized operation, and it is easy to vaporize at room temperature, so the solvent loss is relatively large

Method used

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  • Recovery and separation method for solvent containing tetrahydrofuran-carbinol system

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Experimental program
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Embodiment 1

[0022] There is a solvent composed of 20% methanol, 25% tetrahydrofuran, 54% water, and the rest are high-boiling impurities, which are added to the pretreatment tower at a rate of 200kg / hr. The number of plates in the pretreatment tower is 15, and the reflux ratio is 1.5 , The recovery rate at the top of the tower is 0.9 (relative to the feed), and the flow rate obtained is about 100kg / hr, and the mixed solution containing methanol-tetrahydrofuran-water enters the extractive distillation column. The number of plates in the extractive distillation column is 40, and the extraction agent ethylene glycol is added to the upper part of the column at a solvent ratio of 1:2 (solvent amount: extraction dose, mass ratio), and the reflux ratio is controlled to be 1-1.5, and the extraction at the top of the column is controlled. The ratio is 0.20-0.25 (relative to the feed), and the tower pressure is controlled at 1.5 atmospheres, so that a tetrahydrofuran product with a purity of more th...

Embodiment 2

[0024] There is a solvent composed of 10% methanol, 30% tetrahydrofuran, 59% n-heptane, and all the other high-boiling impurities, which are added to the pretreatment tower at a rate of 200kg / hr. The number of pretreatment tower plates is 17, and the reflux The ratio is 2.5, the recovery rate at the top of the tower is 0.4 (relative to the feed), and the flow rate is about 80kg / hr. The mixed solution containing methanol-tetrahydrofuran enters the extractive distillation tower, and the n-heptane product is obtained in the tower reactor. The number of plates in the extractive distillation column is 40, and the extraction agent ethylene glycol is added to the upper part of the column at a solvent ratio of 1:1.5 (solvent amount: extraction amount, mass ratio), and the reflux ratio is controlled to be 1-1.5, and the extraction at the top of the column is controlled. The ratio is 0.25-0.3 (relative to the feed), and the tower pressure is controlled at 1.5 atmospheres, so that a tetra...

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Abstract

The invention relates to an extraction, rectification and separation method and an extraction, rectification and separation process for a solvent containing a tetrahydrofuran-carbinol system which take ethylene glycol as an extractions solvent, and take tetrahydrofuran and carbinol as products. In the drug synthesis process in the pharmaceutical industry, a great quantity of solvents containing the tetrahydrofuran, the carbinol and the like are used, and a mixed liquid waste is generated. Under the normal temperature and normal pressure, the boiling temperatures of the tetrahydrofuran and the carbinol are extremely similar (the boiling temperature of the tetrahydrofuran is 65.4 DEG C and the boiling temperature of the carbinol is 64.8 DEG C), so that the tetrahydrofuran and the carbinol are difficult to separate by adopting a common rectification operation. In addition, the tetrahydrofuran and the carbinol are good in intersolubility and can be well dissolved with great majority of organic or inorganic solvents so as to be incapable of being separated by an extraction operation. According to the method and the process, the waste solvent containing the tetrahydrofuran-carbinol system can be recovered by adopting an extraction and rectification manner, meanwhile, an extracting agent is recycled, so that the obtained tetrahydrofuran and carbinol products are high in purity, impurities are few, the recovered solvent can be recycled in the drug synthesis process, further not only is the cost of pharmacy process reduced, and also the pollution of the waste solvent to the environment is alleviated greatly.

Description

technical field [0001] The present invention relates to a waste solvent recovery method and process using ethylene glycol as the extraction agent and high-purity tetrahydrofuran and methanol as the products, especially a kind of extraction agent ethylene glycol circulates inside the system and uses extraction and rectification as the main means A waste solvent recovery method containing tetrahydrofuran-methanol system, and a process route using the method. Background technique [0002] Extractive distillation is to add an extractant to the mixture system, which has similar polarity to one or several substances in the system. The difference in the relative volatilities of the substances makes separation possible. [0003] The choice of extractant has a great influence on the operating conditions and the quality of the product. Usually, in addition to considering the difficulty and completeness of the separation, process issues and economic issues are also considered when se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/08C07C31/04C07C29/84
Inventor 漆志文张弛
Owner EAST CHINA UNIV OF SCI & TECH
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