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Tetrahydrofuran-methanol system-contained solvent recovering and separating method

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: 2018-04-13
南京科慧化工技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Tetrahydrofuran-methanol system-contained solvent recovering and separating method

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Experimental program
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Effect test

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 1:6 (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 1:5 (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 0.25-0.3 (relative to the feed), and the tower pressure is controlled at 1.5 atmospheres, so that a tetrahydr...

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Abstract

The invention relates to a method and process for solvent extraction, rectification and separation of a tetrahydrofuran-methanol system using ethylene glycol as an extraction agent and tetrahydrofuran and methanol as products. Generally, pharmaceutical companies use a large amount of solvents such as tetrahydrofuran and methanol in the production process of pharmaceutical products, resulting in mixed waste liquid of solvents. Under normal temperature and pressure, the boiling points of tetrahydrofuran and methanol are very close (65.4°C for tetrahydrofuran and 64.8°C for methanol), so it is difficult to separate them by general rectification. In addition, tetrahydrofuran and methanol have good mutual solubility, and can be well miscible with most organic or inorganic solvents, so it is impossible to separate them by extraction. The present invention adopts the way of extraction and rectification to recover the waste solvent containing tetrahydrofuran and methanol system, and at the same time, the extractant is recycled, and the obtained tetrahydrofuran and methanol products have high purity and less impurities, and can be used for solvent recycling in pharmaceutical companies. It not only reduces the cost of the pharmaceutical process, but also greatly reduces the pollution of the waste solvent to the environment.

Description

technical field [0001] The present invention relates to a kind of waste solvent recovery method and technology that take ethylene glycol (EG) as extraction agent, take high-purity tetrahydrofuran and methanol as products, especially a kind of extraction agent ethylene glycol (EG) circulates inside the system, with A waste solvent recovery method containing tetrahydrofuran-methanol system with extraction and rectification as the main means, 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 al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/08C07C29/84C07C31/04
CPCC07D307/08C07C29/84C07C31/04
Inventor 张弛
Owner 南京科慧化工技术服务有限公司
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