Semi-continuous reaction distillation process for producing carbonic ester

A reactive distillation and semi-continuous technology, applied in the carbonate field, can solve the problems of difficulty for new entrants to enter the linear carbonate market, increase in impurity generation and equipment costs, and high threshold for capital investment, so as to reduce equipment investment and operating costs, reduce Equipment investment cost, high efficiency

Pending Publication Date: 2021-09-17
张文进 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This will increase the generation of impurities and equipment costs, the capital investment

Method used

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  • Semi-continuous reaction distillation process for producing carbonic ester
  • Semi-continuous reaction distillation process for producing carbonic ester
  • Semi-continuous reaction distillation process for producing carbonic ester

Examples

Experimental program
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Effect test

Example

[0047] Example 1: Production of high purity from DEC and EMC DMC

[0048] like figure 1 Shown, a conventional batch distillation system, which is characterized by a distillation kettle equipped with a stirrer, and used as a reactor. This reactor is built with a molar ratio of 1: 1 ethanol and DMC. Sodium (dissolved in methanol) is used as a catalyst in methanol. Steps are as follows:

[0049] (1) The reactor was heated to the reaction temperature of 65-85 deg.] C. The distillation column is operated at total reflux until the temperature at the top of the column reaches 63.5 ℃ (DMC- methanol azeotrope temperature under atmospheric pressure). Then continue to 3: 1 reflux ratio of distillation of the reaction and adjusting the reaction temperature, so that the overhead temperature was controlled at about 63.5 ℃.

[0050] (2) When the reaction temperature began to rise, the flow rate begins to decrease overhead, the start fresh DMC feed is pumped into the reactor. DMC flow control in ...

Example

[0062] Example 2. image 3 , A conventional batch distillation apparatus used in Example 1 into a semi-continuous embodiment of the distillation apparatus. Add a circulation pump to pump the mixture into the reaction tower or the reactor vapor space, thereby enhancing the reactive distillation of heat and mass transfer. Heat exchange may be added to the circulation loop to increase the heating / cooling capacity, but according to the characteristics and other design parameters of the device response, this heat exchanger is optional.

[0063] Cycle entry point may be any point in the distillation column. By introducing the reaction mixture in the column, the column having a stripping and thus rectification section, and therefore may be used as the column batch column continuous distillation column 13, thereby increasing the efficiency of the tower. In a typical batch distillation operation, only the column having a rectification section without a stripping section. The distillation ...

Example

[0077] Example 3 Preparation carbonate from ethylene carbonate (EC) dimethyl carbonate (DMC)

[0078] like Image 6 Shown, a reactive distillation column to enable the EC industrial grade methanol and the reaction to produce industrial DMC. The sodium methoxide catalyst while still. The reactive distillation system adds a cycle, it enters the upper section of the reaction column, as Image 6 Indicated. The procedure is similar to Example 2 of this system.

[0079] (1) was added to the reactor in a molar ratio of 1: EC 2 and methanol. Sodium methoxide catalyst is added to accelerate the reaction. It was heated to 65-80 ℃, so that the distillation column in total reflux state. When the overhead temperature reached 63.5 deg.] C, changed to 3: 1 reflux ratio operation, the overhead product withdrawn (i.e., DMC / MeOH azeotrope).

[0080] (2) When the overhead temperature began to drop and the flow rate decrease start fresh methanol introduced into the reactor loop. Fresh methanol is pre...

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Abstract

The invention relates to the technical field of carbonic ester, in particular to a semi-continuous reaction distillation process for producing carbonic ester, which comprises the following steps of: adding one or more reactants into a reactor or a distillation tower in the reaction distillation process by using intermittent distillation equipment or improved continuous distillation equipment, so as to completely convert the other reactant; then conducting distilling, distilling out light impurities from the top of the tower, completely retaining the residual light impurities in the distillation tower above the reaction kettle, and sending the reacted mixture without light components from the distillation kettle (reactor) to another set of distillation unit for separation, or feeding the materials into a storage tank firstly and then conducting rectification and separation by using the same set of reaction distillation equipment to produce high-purity DMC, EMC and DEC. The process maximizes the conversion of one or more reactants so as to avoid the formation of azeotropes.

Description

technical field [0001] The invention relates to the technical field of carbonates, in particular to a semi-continuous reactive distillation process for producing carbonates. Background technique [0002] Organic carbonates, such as ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC) and diethyl carbonate (DEC), have been produced industrially for many years. Among them, ethylene carbonate and propylene carbonate generate 1,2 through the reaction of CO2 and ethylene oxide (EO) in the presence of a catalyst. [0003] [0004] Dialkyl carbonates, such as DMC, EMC and DEC, are usually produced by the transesterification of EC or PC with methanol or ethanol3 or mixtures of methanol and ethanol, the by-product of which is ethylene glycol (EG) or propylene glycol (PG). These dialkyl carbonates can also be prepared by transesterification of a carbonate with an alcohol. The following are some examples of transesterification ...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06C07C68/065C07C68/08C07D317/36
CPCC07C68/06C07C68/065C07C68/08C07D317/36C07C69/96Y02P20/10
Inventor 张文进耿昆仑
Owner 张文进
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