Separation method of azeotrope of dimethyl carbonate and methanol

A technology of dimethyl carbonate and a separation method, which is applied in the field of continuous extraction, rectification and separation of dimethyl carbonate and methanol, can solve the problems such as the inability of continuous operation of the extractant, and achieves stable continuous separation process, lower use threshold, and mutual solubility. Good results

Active Publication Date: 2019-03-05
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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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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  • Separation method of azeotrope of dimethyl carbonate and methanol
  • Separation method of azeotrope of dimethyl carbonate and methanol

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Experimental program
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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-ethyl-3-methylimidazole bistrifluoro Methanesulfonylimide salt ([emim][NTf 2 ]) add from the 4th tray, total flow is 8kg / 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 1.06 at this moment. The extractive distillation tower is operated under normal pressure, the top of the tower is fully condensed, the reflux ratio is 1.4, the output at the top of the tower is 0.7kg / h, 99.8wt% of methanol can be obtained, and the temperature of the top of the extractive distillation tower is 64°C. The temperature of the t...

Embodiment 2

[0027] 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-ethyl-3-methylimidazole bistrifluoro Methanesulfonylimide salt ([emim][NTf 2 ]) 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 0.93 at this moment. The extractive distillation tower operates under normal pressure, the top of the tower is fully condensed, the reflux ratio is 1.4, the output at the top of the tower is 0.7kg / h, 99.6wt% of methanol can be obtained, and the temperature of the top of the extractive distillation tower is 64°C. The temperature of the towe...

Embodiment 3

[0029] 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-ethyl-3-methylimidazole bistrifluoro Methanesulfonylimide salt ([emim][NTf 2 ]) add from the 4th tray, total flow is 10kg / 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 0.93 at this time. The extractive distillation tower operates under normal pressure, the top of the tower is fully condensed, the reflux ratio is 1.23, the output at the top of the tower is 0.7kg / h, 99.92wt% of methanol can be obtained, and the temperature of the top of the extractive distillation tower is 64°C. The temperature in the botto...

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Abstract

The invention provides a separation method of an azeotrope of dimethyl carbonate and methanol. The invention relates to a separation method of dimethyl carbonate and methanol, and mainly solves the problem of unstable operation of a device in a continuous production process using ionic liquid as an extractant. The separation method is extractive distillation, the extractive distillation adopts a mixed extractant, wherein one component of the mixed extractant is ionic liquid with an anion of bistrifluoromethanesulfonimide radical, and the other component of the mixed extractant is one of diethylene glycol dimethyl ether, triethylene glycol dimethyl ether or tetraethylene glycol dimethyl ether. The separation method can realize the continuous separation of dimethyl carbonate and methanol. The product quality and the device operation are stable. The separation method can be used in the 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): C07C67/54C07C69/96C07C29/84C07C31/04C07C27/32
CPCC07C29/84C07C67/54C07C69/96C07C31/04
Inventor 李骏何文军戈军伟王嘉华
Owner CHINA PETROLEUM & CHEM CORP
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