Method for one-step synthesis of ethyl methyl carbonate from propylene oxide and co-production of 1,2-propanediol

A technology for methyl ethyl carbonate and propylene oxide, applied in the field of synthesizing methyl ethyl carbonate, can solve the problems of high energy consumption, increased operating cost, low reactant conversion rate and product selectivity, etc.

Inactive Publication Date: 2018-06-15
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 one-step synthesis of ethyl methyl carbonate from propylene oxide and co-production of 1,2-propanediol
  • Method for one-step synthesis of ethyl methyl carbonate from propylene oxide and co-production of 1,2-propanediol
  • Method for one-step synthesis of ethyl methyl carbonate from propylene oxide and co-production of 1,2-propanediol

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preparation example Construction

[0062] 1. Preparation method of mesoporous molecular sieve carrier:

[0063] 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:

[0064] 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.

[0065] 2) Desiliconization: Add the M-S-DAl carrier prepared in pro...

Embodiment 1

[0099] In the still of 50L slurry bed reactor, reaction pressure 10MPa, reaction raw material propylene oxide: carbon dioxide: methyl alcohol: ethanol=1:1:3:2, drop into each 1.2kg of basic catalyst that above-mentioned preparation method obtains respectively, reaction solution The total volume 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.

[0100]

[0101] The propylene oxide and carbon dioxide conversions were essentially the same under all reaction conditions, therefore, the propylene oxide conversion, CO 2 The conversion rate also represents the CO 2 and propylene oxide conversion, product selectivity in terms of CO 2 base calculation. In addition to the generation of propylene carbonate (PC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC) and diethy...

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. 50 g of 15%BaO-5%Al2O3-3%La2O3 / Cs-meso-EMT catalyst was loaded into the fixed bed, the molar ratio of propylene oxide to carbon dioxide was 1:1, and the methanol and ethanol were mixed according to the molar ratio of 3 :2 ratio pumped into the reactor with a space velocity of 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]

[0105] As can be seen from Table 2, with 15%BaO-5%Al 2 o 3 -3%La 2 o 3 When / Cs-meso-EMT was used as the catalyst, the conversion of reactants and product selectivity increased with the increase of reaction pressure. When the reaction pressure reaches 5MPa ...

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Abstract

The invention relates to a method for synthesizing ethyl methyl carbonate, and concretely relates to a method for one-step synthesis of ethyl methyl carbonate from propylene oxide and co-production of1,2-propanediol. An efficient alkaline catalyst having a compopsite pore structure is used in the one-step reaction of the propylene oxide, carbon dioxide, methanol and ethanol for synthesizing the ethyl methyl carbonate. A crude product obtained through the reaction contains dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate and 1,2-propanediol, wherein the ethyl methyl carbonate selectivity reaches up to 70%. Byproducts dimethyl carbonate and diethyl carbonate can be directly separated as products, also can be recycled, and are continuously reacted to generate the ethyl methyl carbonate, and the product 1,2-propanediol can be separated through simple distillation as a popular raw material. The method has the advantages of cleanness, high efficiency, no pollution and no wastesin the whole reaction process. The catalyst is not inactive after being used at a molar ratio of the propylene oxide to the carbon dioxide to the methanol to the ethanol of 1:1:3:2 under a reaction pressure of 5 MPa at a reaction temperature of 100 DEG C under an air speed of 5 h<-1> for 5000 h, and has a good stability.

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 from propylene oxide in one step and co-producing 1,2-propanediol. 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 lithiu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/04C07C31/20C07C29/128
CPCC07C29/128C07C68/04C07C31/205C07C69/96Y02P20/141
Inventor 石磊于悦
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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