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Batch extractive distillation separation method of methylal-methanol azeotropic mixture

A technology of azeotropic mixture and extractive distillation, which is applied in the direction of extractive distillation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of large equipment investment, low efficiency, unfavorable production, etc. The effect of flexibility and low equipment cost investment

Inactive Publication Date: 2012-08-08
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the extraction and rectification separation method of the methylal-methanol azeotropic system, the extractants mainly include salt-containing ethylene glycol, glycerin and N,N-dimethylformamide, but the energy consumption of these three extractants is relatively high. High, not conducive to production
Pressure swing rectification can separate the methylal-methanol azeotropic system, but the rectification tower needs to be pressurized, the energy consumption is high, the equipment investment is large, and the efficiency is low

Method used

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  • Batch extractive distillation separation method of methylal-methanol azeotropic mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Using a batch extraction and rectification device, put 500L of methylal-methanol azeotropic mixture (8.2% of methanol and 91.8% of methylal, both in mass percentage) into the heating kettle, the extraction agent selected for the test is propanol, and the heating kettle is turned on The heat source and the cold source of the condenser, after a period of reflux at the top of the extraction and rectification tower, the temperature of the top of the tower is stable, and the extraction agent is added. The feeding position of the extraction agent is near the top of the tower. , when the temperature at the top of the extractive distillation column is 41.3-43° C., the distillate starts to discharge the methylal content ≥ 99%, the reflux ratio is 3:1, and the discharge speed is 200 L / h. When the temperature at the top of the extractive distillation tower is 43-64°C, take out the transition section of methylal-methanol, and stop adding the extractant, the reflux ratio is 9:1, when...

Embodiment 2

[0013] A batch extraction and rectification device was adopted, and 500L of methylal-methanol azeotrope (wherein methanol 10%, methylal 90%, both in mass percent) was dropped into the heating kettle, and the selected extraction agent for the test was dimethyl sulfoxide. Turn on the heat source of the heating kettle and the cold source of the condenser. After the top of the extraction and rectification tower is refluxed for a period of time, the temperature at the top of the tower is stable, and the extraction agent is added. The feeding position of the extraction agent is near the top of the tower. Total reflux operation, when the temperature at the top of the extractive distillation column is 41.3-43°C, the distillate with a methylal content ≥ 99% starts to discharge, the reflux ratio is 2:1, and the discharge speed is 300L / h. When the temperature at the top of the extractive distillation column is 43-64°C, take out the transition section of methylal-methanol, and stop adding ...

Embodiment 3

[0015] The experimental device and operation method are the same as in Example 1, and isopropanol is used as the extractant.

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Abstract

Belonging to separation technologies of methylal-methanol azeotropic mixtures, the invention discloses a batch extractive distillation separation method of a methylal-methanol azeotropic mixture. The method takes propanol, isopropanol, butanol, tert-butyl alcohol, 1, 3-propylene glycol or dimethyl sulfoxide as the extracting agent. An extractive distillation tower are operated according to the operation conditions that, under normal pressure or reduced pressure, the extracting agent and an overhead product are in a mass ratio of 0.5:1-10:1, the feed temperature of the extracting agent is 20-40DEG C, and the extractive distillation tower top is controlled at different temperatures and reflux ratios, so that a methylal product, a methylal-methanol transition section I, a methanol product and a methanol-extracting agent transition section II can be obtained from the extractive distillation tower top respectively. When composition of the extracting agent of a heating kettle meets requirements, the extracting agent is pumped into a high storage tank, and feeding is conducted for next batch of extractive distillation separation. The method of the invention has the advantages of low cost of single-tower equipment, flexible operation, adoption of an extracting agent to destroy a methylal-methanol azeotropic system, and can obtain high purity methanol and methylal products.

Description

technical field [0001] The invention relates to a batch extraction and rectification separation method of a methylal-methanol azeotrope, which belongs to the separation technology of the methylal-methanol azeotrope. Background technique [0002] Extractive distillation is a special distillation separation technology, which is suitable for the separation of azeotropic systems. The purpose of separation is achieved by continuously adding extractant to the top of the rectification tower to change the relative volatility between the original components. Batch extractive distillation combines the advantages of batch distillation and extractive distillation. It is flexible in operation and can separate multiple components through one tower. The equipment investment is small, and it is suitable for the separation of azeotropic and near-boiling systems in small batches. The chemical structural formula of methylal is: CH 2 (OCH 3 ) 2 , is a good organic solvent. In industrial pro...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/58C07C29/84C07C31/04B01D3/40
Inventor 姜占坤孙国新袁美龙夏光明
Owner UNIV OF JINAN
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