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Method for synthesizing ethyl methyl carbonate in one-step and co-producing ethylene glycol from ethylene oxide

A technology of ethyl methyl carbonate and ethylene oxide, which is applied in the field of synthesizing ethyl methyl carbonate, can solve the problems of high energy consumption, low conversion rate of reactants and product selectivity, increased operating costs, etc., and achieves a clean reaction process Effect

Inactive Publication Date: 2018-06-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

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 ethyl methyl carbonate in one-step and co-producing ethylene glycol from ethylene oxide
  • Method for synthesizing ethyl methyl carbonate in one-step and co-producing ethylene glycol from ethylene oxide
  • Method for synthesizing ethyl methyl carbonate in one-step and co-producing ethylene glycol from ethylene oxide

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preparation example Construction

[0061] 1. Preparation method of mesoporous molecular sieve carrier:

[0062] 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:

[0063] 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.

[0064] 2) Desiliconization: Add the M-S-DAl carrier prepared in pro...

Embodiment 1

[0098] In the still of 50L slurry bed reactor, reaction pressure 10MPa, reaction raw material ethylene oxide: carbon dioxide: methyl alcohol: ethanol=1:1:3:2, drop into each 1.2kg of the basic catalyst that above-mentioned preparation method obtains respectively, react The total volume of the solution is 40 L. The reaction was mechanically stirred at a reaction temperature of 100°C. After 10 hours of reaction, samples were taken for chromatographic analysis and calculation. The conversion rate of raw materials and product selectivity are shown in Table 1.

[0099] Table 1 Effects of different types of catalysts on feedstock conversion and product selectivity

[0100]

[0101] The conversion of ethylene oxide and carbon dioxide was essentially the same under all reaction conditions, therefore, the conversion of ethylene oxide, CO 2 The conversion rate also represents the CO 2 and ethylene oxide conversion, product selectivity in terms of CO 2 base calculation. In additio...

Embodiment 2

[0103] In a fixed-bed reactor, the effects of different reaction pressures on the conversion of raw materials and product selectivity were explored. Load 15%BaO-5%CaO-3%La in a fixed bed 2 o 3 / Cs-meso-EMT catalyst 50 g, the molar ratio of ethylene oxide to carbon dioxide is 1:1, and the constant flow pump is used to pump methanol and ethanol into the reactor according to the molar ratio of 3:2, and the space velocity is 5 h -1 , the reaction pressure is shown in the table, the reaction temperature is 100°C, and it is stabilized for 500 h. After stabilization, samples are taken for chromatographic analysis and calculation. The conversion rate of raw materials and product selectivity are shown in Table 2.

[0104] Table 2 Effects of Different Reaction Pressures on Raw Material Conversion Rate and Product Selectivity

[0105]

[0106] As can be seen from Table 2, with 15%BaO-5%CaO-3%La 2 o 3 When / Cs-meso-EMT was used as the catalyst, the conversion of reactants and produ...

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Abstract

The invention discloses a method for synthesizing ethyl methyl carbonate in one step and co-producing ethylene glycol from ethylene oxide, and relates to methods for synthesizing ethyl methyl carbonate. The method is characterized in that a high-efficiency alkaline catalyst with a composite pore structure is used for one-step synthesis of ethyl methyl carbonate from ethylene oxide, carbon dioxide,methanol and ethanol. The obtained crude product of the reation contains dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate and ethylene glycol, wherein the selectivity of methyl ethyl carbonate can reach up to 70% at maximum, byproducts of dimethyl carbonate and diethyl carbonate can be directly isolated as products, or can be recycled to react continuously to form ethyl methyl carbonate, and the byproduct ethylene glycol as a bulk raw material can be separated through simple distillation. The entire reaction process is clean, efficient, non-polluting and free of generating any waste. When the molar ratio of ethylene oxide: carbon dioxide: methanol: ethanol is 1:1:3:2, the reaction pressure is 5 MPa, the reaction temperature is 100 DEG C, and the space velocity is 5 h<-1>, thecatalyst does not lose activity after being used for 5000 h, and the stability is better.

Description

technical field [0001] The invention relates to a method for synthesizing ethyl methyl carbonate, in particular to a method for synthesizing ethyl methyl carbonate in one step from ethylene oxide and co-producing ethylene glycol. 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...

Claims

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Application Information

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IPC IPC(8): C07C68/04C07C69/96C07C29/00C07C31/20B01J29/70B01J35/10B01J37/08B01J37/30
CPCC07C29/00C07C68/04B01J29/7069B01J37/088B01J37/30B01J2229/18B01J35/60C07C69/96C07C31/202Y02P20/52Y02P20/141
Inventor 石磊姚杰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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