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Method for synthesizing carbonic acid symmetric ester in one step with ethylene carbonate and alcohols

A technology of ethylene carbonate and carbonic acid, which is applied in the field of synthesizing symmetrical carbonate esters, can solve the problems of high energy consumption, low conversion rate of reactants and product selectivity, increased operating costs, etc., and achieves the effect of clean reaction process

Inactive Publication Date: 2018-05-18
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
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Problems solved by technology

[0027] At present, in all above-mentioned synthesis methods of ethyl methyl carbonate, the transesterification method is mainly used as the mainstream synthetic route, but the raw material dimethyl carbonate of the transesterification method needs to be synthesized through methanol transesterification of ethylene carbonate or propylene carbonate, while ethylene carbonate Esters need to be prepared by the reaction of ethylene oxide and carbon dioxide, and propylene carbonate needs to be prepared by the reaction of propylene oxide and carbon dioxide. The above reaction route needs to be carried out in stages. The process consumes a lot of energy and increases operating costs

Method used

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  • Method for synthesizing carbonic acid symmetric ester in one step with ethylene carbonate and alcohols
  • Method for synthesizing carbonic acid symmetric ester in one step with ethylene carbonate and alcohols
  • Method for synthesizing carbonic acid symmetric ester in one step with ethylene carbonate and alcohols

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preparation example Construction

[0063] 1. Preparation method of mesoporous molecular sieve carrier:

[0064] In the present invention, orderly acid-base treatment is carried out on different carriers, and finally the molecular sieve carrier with the compound pore structure of mesoporous and micropores is prepared by high-temperature roasting. The purpose of the acid treatment is to remove the Al in the molecular sieve framework, so as to realize pore formation. The main function of the alkali treatment is to remove the Si in the molecular sieve framework to make the molecular sieve form a mesoporous structure. The preparation process includes the following steps:

[0065] 1) Dealumination: Add a certain mass of M-S carrier to a certain volume of acidic solution with a concentration of 0.11 mol / L, then stir and reflux in an oil bath at 100°C for 6 h, then filter, wash, and dry at 120°C for 8 h. The dealuminated M-S-DAl carrier is obtained.

[0066] 2) Desiliconization: Add the M-S-DAl carrier prepared in pro...

Embodiment 1

[0100] In the still of 50L slurry bed reactor, reaction pressure 2MPa, reaction raw material ethylene carbonate: methyl alcohol=1:3, drop into each 1.2 kg of the basic catalyst that above-mentioned preparation method obtains respectively, the total volume of reaction solution is 40 L. The reaction was carried out with mechanical stirring, and the reaction temperature was 100°C. After 10 hours of reaction, samples were taken for chromatographic analysis and calculation. The conversion rate of raw materials and the yield of products are shown in Table 1.

[0101] Table 1 The influence of different types of catalysts on the conversion rate of raw materials and product yield

[0102]

[0103] The reaction is catalyzed by a basic catalyst, and the reaction product is a single dimethyl carbonate and ethylene glycol. In addition to the generation of dimethyl carbonate (DMC) in the above table, a large amount of ethylene glycol is generated. Since ethylene glycol is derived from et...

Embodiment 2

[0105] In a 50L slurry bed reactor, the reaction pressure is 2MPa, the reaction raw material ethylene carbonate: various alcohols = 1:3, put in 15%CaO-5%Cr 2 o 3 -3%La 2 o 3 / Zn-meso-Y catalyst 1.2kg, the total volume of the reaction solution is 40 L. The reaction was mechanically stirred, the reaction temperature was 100°C, and after 10 hours of reaction, samples were taken for chromatographic analysis and calculation.

[0106] The influence of table 2 different alcohols on raw material conversion rate, product yield

[0107]

[0108] It can be seen from Table 2 that when different alcohols are used as reaction raw materials to synthesize symmetrical carbonate esters, the reaction results are quite different. As the R group becomes more complex, the conversion rate of ROH gradually decreases, and the yield of symmetrical carbonate esters also gradually decreases. . The reason is that as the R group becomes more complex, the steric hindrance of ROH becomes larger, and ...

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Abstract

The invention relates to a method for synthesizing carbonic acid symmetric ester in one step with ethylene carbonate and alcohols, in particular to a method for synthesizing the carbonic acid symmetric ester. A high-efficiency alkaline catalyst of a composite pore structure is used for preparing synthesizing the carbonic acid symmetric ester in one step with ethylene carbonate and various alcoholssuch as ROH and diols, ethylene glycol, diethylene glycol, polyol and the like. A crude product obtained through a reaction only contains the carbonic acid symmetric ester and ethylene glycol. The conversion rate of the ethylene carbonate can reach 95% at most. The byproduct ethylene glycol serving as a bulk raw material can be separated through simple distillation. The whole reaction process isclean, efficient, free of pollution and free of waste. The molar ratio of the ethylene carbonate to various alcohols is 1:3, the reaction pressure is 5 MPa, the reaction temperature is 100 DEG C, theair speed is 5 h<-1>, and after being used for 5000 h, the catalyst is still active and good in stability.

Description

technical field [0001] The invention relates to a method for synthesizing symmetrical carbonate esters, in particular to a method for synthesizing symmetrical carbonate esters in one step from ethylene carbonate and alcohols. Background technique [0002] Methyl Ethyl Carbonate (MEC for short), molecular formula: C 4 h 8 o 3 , colorless transparent liquid, density 1.01 g / mL, melting point -55 ° C, boiling point 107 ° C, flammable, can be mixed with organic solvents such as alcohols, ketones, esters in any proportion, is an excellent solvent, ethyl methyl carbonate is due to Its molecular structure has methyl and ethyl groups at the same time, so it has the characteristics of dimethyl carbonate and diethyl carbonate, and can be used as some special organic synthesis reagents, and it is also a solvent for special fragrances. [0003] Due to the low viscosity, large dielectric constant and strong solubility of lithium salts, ethyl methyl carbonate is an excellent lithium-ion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96C07C29/00C07C29/80C07C31/20B01J29/03B01J23/10B01J29/04B01J29/70B01J29/08B01J29/40B01J35/10B01J37/02B01J37/03
CPCC07C29/00C07C29/80C07C68/065B01J23/002B01J23/10B01J29/0308B01J29/04B01J29/041B01J29/045B01J29/084B01J29/405B01J29/7007B01J29/7876B01J37/0201B01J37/035B01J35/647C07C69/96C07C31/202Y02P20/52
Inventor 石磊陈飞
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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