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A kind of method for extracting and rectifying separating acetonitrile and triethylamine

A technology of extractive distillation and extractive distillation tower, which is applied in the field of chemical separation and purification to achieve the effects of reducing pollution, high product purity and simple separation

Active Publication Date: 2018-06-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there is no report about the separation method of acetonitrile and triethylamine azeotropic system in the literature, so it is of great practical significance and industrial value to propose a method for separating acetonitrile and triethylamine that is environmentally friendly and easy to control

Method used

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  • A kind of method for extracting and rectifying separating acetonitrile and triethylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] In the extractive distillation tower equipped with 35 trays, the mixture of acetonitrile and triethylamine with a mass ratio of 8 and 2 enters from the 15th plate with a flow rate of 1000 kg / h, and the extractant ethylene glycol from the 10th plate The plate enters the tower, the flow is 2000kg / h, the operating pressure of the extractive distillation tower is 0.3atm, the reflux ratio is controlled to 4, acetonitrile is extracted from the top of the tower, and triethylamine and ethylene glycol are extracted from the bottom of the tower. The plates enter the solvent recovery tower equipped with 50 plates, the operating pressure is 0.3atm, the reflux ratio is controlled to 4, triethylamine is extracted from the top of the tower, and the ethylene glycol produced at the bottom of the tower is returned to the extractive distillation tower for recycling .

[0055] After separation: the purity of acetonitrile product reached 99.90wt%; the purity of triethylamine product reached 99...

Embodiment 2

[0057] In an extractive distillation tower equipped with 40 trays, the mixture of acetonitrile and triethylamine with a mass ratio of 7 and 3 enters from the 16th plate with a flow rate of 1000 kg / h, and the extractant ethylene glycol from the 11th plate The plate enters the tower, the flow rate is 1000kg / h, the operating pressure of the extractive distillation tower is 0.4atm, the reflux ratio is controlled to 5, acetonitrile is extracted from the top of the tower with a purity of 99.7wt%, and triethylamine and ethylene glycol are from the tower bottom After extraction, enter the solvent recovery tower equipped with 45 trays from the 19th plate, the operating pressure is 0.4atm, the reflux ratio is controlled to 4, the triethylamine is extracted from the top of the tower, and the ethylene glycol produced at the bottom of the tower is returned The extractive distillation tower is recycled.

[0058] After separation: the purity of acetonitrile product reaches 99.92wt%; the purity ...

Embodiment 3

[0060] In an extractive distillation tower equipped with 45 trays, the mixture of acetonitrile and triethylamine with a mass ratio of 7 and 3 enters from the 13th plate with a flow rate of 1000 kg / h and the extractant ethylene glycol from the 10th plate. The plate enters the tower, the flow is 3000kg / h, the operating pressure of the extractive distillation tower is 0.6atm, the reflux ratio is controlled to 4, acetonitrile is extracted from the top of the tower with a purity of 99.5wt%, and triethylamine and ethylene glycol are from the tower bottom After extraction, enter the solvent recovery tower equipped with 55 trays from the 21st plate, the operating pressure is 0.6atm, the reflux ratio is controlled to 5, the triethylamine is extracted from the top of the tower, and the ethylene glycol produced at the bottom of the tower is returned The extractive distillation tower is recycled.

[0061] After separation: the purity of acetonitrile product reached 99.84wt%; the purity of tr...

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Abstract

The invention relates to a method for separating an acetonitrile and triethylamine azeotropic mixture by extractive distillation. An extractive distillation column and a solvent recovery tower adopt negative pressure operation; the acetonitrile and triethylamine mixture are introduced from the upper middle part of the extractive distillation column; ethylene glycol as an extractant is introduced from the upper part of the column; after the extractive distillation column, acetonitrile is extracted from the top of the extractive distillation column; the extractant and triethylamine are extracted from the bottom of the extractive distillation column and introduced from the upper middle part of the recovery tower; the triethylamine is extracted from the top of the solvent recovery tower; and the extractant ethylene glycol is extracted from the bottom of the recovery tower for recycling. The negative pressure operation adopted by the invention can reduce the heat load of the reboiler, and reduce the energy consumption for operation; the extractant ethylene glycol can significantly improve the relative volatility of acetonitrile and triethylamine; and the recovery rate is as high as 99.9%.

Description

【Technical Field】 [0001] The invention belongs to the field of chemical separation and purification, and relates to a method for separating an azeotropic mixture of acetonitrile and triethylamine. Further, it relates to an extraction distillation tower using an ethylene glycol extractant, and then a solvent recovery tower to extract the concentrate. Distillation separation method of azeotropic mixture of acetonitrile and triethylamine. 【Background technique】 [0002] Acetonitrile, also known as methyl nitrile, is a colorless and transparent liquid, very volatile, and has a special smell similar to ether. Acetonitrile is an excellent solvent that can dissolve a variety of organic, inorganic and gaseous substances. Acetonitrile can undergo typical nitrile reactions and is used to prepare many typical nitrogen-containing compounds. It is an important organic intermediate. [0003] Triethylamine is a kind of amine organic compound. It is a colorless and transparent liquid with a stro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/03C07C253/34C07C211/05C07C209/86
CPCC07C209/86C07C253/34C07C211/05C07C255/03
Inventor 王英龙贺炜赵婷然李敏文桂林朱兆友
Owner QINGDAO UNIV OF SCI & TECH