Method for separating dichloromethane, triethylamine and water

A technology of dichloromethane and triethylamine, which is applied in the field of separation of dichloromethane, triethylamine and water, and can solve the problems of flammability, unreported separation method and toxicity of triethylamine

Active Publication Date: 2014-10-08
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Triethylamine is flammable, explosive, toxic and highly irritating
At present, there is no report about the separation method of the three mixtures of dichloromethane, triethylamine and water

Method used

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  • Method for separating dichloromethane, triethylamine and water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The raw material liquid 5 contains 65% of dichloromethane (mass fraction, the same below), 30% of triethylamine and 5% of water, and the temperature is 20°C. The raw material liquid 5 is first sent into the first phase separation tank 1 under normal pressure. The temperature of the first phase separation tank 1 is 10° C., and the pressure is 101.325 kPa. The stream separated from the upper layer feed liquid of the first phase separation tank 1 is sent to the rectification tower 2, the stream temperature is 20°C, the number of trays in the rectification tower 2 is 24, and the 12th tray from the rectification tower 2 Feed, the top of the tower is the total condenser 4. The total reflux operation is carried out until the top temperature of the rectification tower 2 is 37.4°C, and the extraction starts when the temperature of the bottom of the tower is about 88.0°C, and the reflux ratio is 0.4. In the bottom liquid of rectification tower 2, through chromatographic separat...

Embodiment 2

[0033] The raw material liquid 5 contains 65% of dichloromethane (mass fraction, the same below), 30% of triethylamine and 5% of water, and the temperature is 22°C. The raw material liquid 5 is first sent into the first phase separation tank 1 under normal pressure. The temperature of the first phase separation tank 1 is 25° C., and the pressure is 101.325 kPa. The stream separated from the upper layer feed liquid of the first phase separation tank 1 is sent to the rectification tower 2, the stream temperature is 25°C, the number of trays in the rectification tower 2 is 24, and the 12th tray from the rectification tower 2 Feed, the top of the tower is the total condenser 4. The total reflux operation is carried out until the top temperature of the rectification tower 2 is 37.4°C, and the extraction starts when the temperature of the bottom of the tower is about 88.6°C, and the reflux ratio is 0.3. In the bottom liquid of rectification tower 2, through chromatographic separat...

Embodiment 3

[0035] The raw material liquid 5 contains 65% of dichloromethane (mass fraction, the same below), 30% of triethylamine and 5% of water, and the temperature is 25°C. The raw material liquid 5 is first sent into the first phase separation tank 1 under normal pressure. The temperature of the first phase separation tank 1 is 35° C., and the pressure is 101.325 kPa. The stream separated from the upper layer feed liquid of the first phase separation tank 1 is sent to the rectification tower 2, the stream temperature is 35°C, the number of trays in the rectification tower 2 is 24, and the 12th tray from the rectification tower 2 Feed, the top of the tower is the total condenser 4. The total reflux operation is carried out until the top temperature of the rectification tower 2 is 37.5°C, and the extraction starts when the temperature of the bottom of the tower is about 88.6°C, and the reflux ratio is 1.0. In the bottom liquid of rectification tower 2, through chromatographic separat...

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Abstract

The invention relates to a method for separating dichloromethane, triethylamine and water. The method comprises the following steps of firstly feeding feed liquor containing dichloromethane, triethylamine and water into a first phase splitting tank; feeding material flow separated out from upper-layer feed liquor of the first phase splitting tank into a rectifying tower, carrying out normal-pressure rectifying operation, keeping a tower-top temperature at 37-38 DEG C, keeping a tower-kettle temperature at 88-89 DEG C, extracting triehylamine from the tower kettle; feeding tower-top extracting liquor of the rectifying tower into a second phase splitting tank, thereby obtaining dichloromethane from the upper-liquid feed liquor of the second phase splitting tank and obtaining water from the material flow separated out from the lower-layer feed liquor of the second phase splitting tank. The method disclosed by the invention can effectively separate a mixture of dichloromethane, triethylamine and water to obtain 99.6% dichloromethane and 99.9% triethylamine.

Description

technical field [0001] The invention relates to a method for separating dichloromethane, triethylamine and water using a rectification tower. Background technique [0002] Rectification is a distillation method that uses reflux to separate liquid mixtures with high purity. It is the most widely used liquid mixture separation operation in industry, and is widely used in petroleum, chemical, light industry, food, metallurgy, pharmaceutical and other fields. [0003] Dichloromethane is a colorless liquid with the advantages of strong solvency and low toxicity. Dichloromethane is mainly used in film production and medicine in China. It is mostly used as a reaction medium in the pharmaceutical industry, and can also be used as a solvent in film production. Triethylamine is flammable, explosive, toxic and highly irritating. In industry, it is mainly used as solvent, curing agent, catalyst, etc. The solvent waste liquid in the pharmaceutical industry often contains dichlorometh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/38C07C17/383C07C19/03C07C209/86C07C211/05
Inventor 李春利王洪海耿海腾余迎新王荣良
Owner HEBEI UNIV OF TECH
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