Method for continuous extraction rectification separation of azeotrope of dimethyl carbonate and methanol

A dimethyl carbonate and separation method technology, applied in the field of continuous extraction, rectification and separation of dimethyl carbonate and methanol, can solve the problem that the extractant cannot be continuously operated, and achieve stable continuous separation process, stable properties, and improved stability Effect

Active Publication Date: 2019-03-05
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0006] In order to solve the problem that the ionic liquid existing in the azeotrope separation of dimethyl carbonate and methanol cannot operate continuously as an extractant, th

Method used

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  • Method for continuous extraction rectification separation of azeotrope of dimethyl carbonate and methanol
  • Method for continuous extraction rectification separation of azeotrope of dimethyl carbonate and methanol

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Embodiment 1

[0025] Such as figure 2 The extractive distillation process shown. The extractive distillation column has 30 theoretical plates (the number of plates is counted from top to bottom), and the mixed extractant contains 30wt% triethylene glycol dimethyl ether and 70wt% 1-hexyl-3-methylimidazole hexafluorophosphate ([hmim][PF 6 ]) add from the 4th tray, total flow is 7kg / h, the mixture of raw material dimethyl carbonate and methyl alcohol adds from the 27th tray, dimethyl carbonate content is 30wt%, methanol content is 70wt%, total The flow rate is 1kg / h, and the molar solvent ratio of the extractant to the raw material is 1.1 at this time. The extractive distillation tower is operated under normal pressure, the top of the tower is fully condensed, the reflux ratio is 1.6, the output at the top of the tower is 0.7kg / h, 99.89wt% of methanol can be obtained, and the temperature of the top of the extractive distillation tower is 64°C. The temperature of the tower kettle is 185°C. ...

Embodiment 2

[0027] Such as figure 2 The extractive distillation process shown. The extractive distillation column has 35 theoretical plates (the number of plates is counted from top to bottom), and the mixed extractant contains 20wt% triethylene glycol dimethyl ether and 80wt% 1-hexyl-3-methylimidazole hexafluorophosphate ([hmim][PF 6 ]) add from the 4th tray, flow rate is 6.5kg / h, the mixture of raw material dimethyl carbonate and methyl alcohol adds from the 30th tray, dimethyl carbonate content is 30wt%, methanol content is 70wt%, total The flow rate is 1kg / h, and the molar solvent ratio of the extractant to the raw material is 0.95 at this time. The extractive distillation tower operates under normal pressure, the top of the tower is fully condensed, the reflux ratio is 1.5, the output of the tower top is 0.7kg / h, 99.93wt% of methanol can be obtained, and the temperature of the top of the extractive distillation tower is 64°C. The temperature of the tower kettle was 196°C. The pr...

Embodiment 3

[0029] Such as figure 2 The extractive distillation process shown. The extractive distillation column has 40 theoretical plates (the number of plates is counted from top to bottom), and the mixed extractant contains 50wt% triethylene glycol dimethyl ether and 50wt% 1-butyl-3-methylimidazole hexafluorophosphoric acid salt([bmim][PF 6 ]) add from the 4th tray, total flow is 9kg / h, the mixture of raw material dimethyl carbonate and methyl alcohol adds from the 36th tray, dimethyl carbonate content is 30wt%, methanol content is 70wt%, total The flow rate is 1kg / h, and the molar solvent ratio of the extractant to the raw material is 1.57. The extractive distillation tower is operated under normal pressure, the top of the tower is fully condensed, the reflux ratio is 3, the output at the top of the tower is 0.7kg / h, 99.7wt% of methanol can be obtained, and the temperature of the top of the extractive distillation tower is 64°C. The temperature of the tower kettle is 170°C. The pr...

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Abstract

The invention discloses a method for continuous extraction rectification separation of an azeotrope of dimethyl carbonate and methanol. The invention relates to the method for separating dimethyl carbonate and methanol, and mainly solves a problem that operation of apparatus is not stable in a continuous production process when an ionic liquid is used as an extracting agent. The separation methodis extraction rectification, and a mixed extraction agent is adopted in extraction rectification, wherein one of the mixed extracting agents is an ionic liquid with anions of hexafluorophosphate radicals, and the mixed extraction agent is one selected from diethylene glycol dimethyl ether, triethylene glycol dimethyl ether or tetraethylene glycol dimethyl ether. The separation method can be used to realize continuous separation of dimethyl carbonate and methanol, product quality and running stability of the apparatus are stable, and the method can be applied to an industrial production process.

Description

technical field [0001] The present invention relates to a kind of separation method of dimethyl carbonate and methanol, specifically, relate to a kind of continuous extraction rectification separation method of dimethyl carbonate and methanol. Background technique [0002] Dimethyl carbonate (DMC) is an environmentally friendly chemical intermediate widely used in reactions such as methylation, carbonylation, carbonylmethylation and methoxylation, and is known as the "new cornerstone" of organic synthesis today . In industry, transesterification is usually used to produce dimethyl carbonate. During the production process, dimethyl carbonate and methanol form an azeotrope, which is difficult to separate by ordinary distillation methods. [0003] In recent years, technologies such as extractive distillation, pressurized distillation, azeotropic distillation and membrane separation have been used to produce high-purity dimethyl carbonate. Compared with the latter three proces...

Claims

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Application Information

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IPC IPC(8): C07C68/08C07C69/96C07C29/84C07C31/04
CPCC07C29/84C07C68/08C07C69/96C07C31/04
Inventor 李骏杨为民何文军
Owner CHINA PETROLEUM & CHEM CORP
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