Method for synthesizing EMC (Ethylmethyl Carbonate) through homogeneously precipitating solid base catalyst

A solid base catalyst, methyl ethyl carbonate technology, applied in the preparation of organic carbonate, chemical instruments and methods, catalyst activation/preparation and other directions, can solve the problems of polluted products, product difficulties, long reaction period and other problems, and achieve component distribution The effect of uniformity, high production efficiency and large grain size

Inactive Publication Date: 2019-03-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the catalyst used in it can be recycled repeatedly, because its catalyst is a chloride-type Lewis acid, it is difficult to separate. On the other hand, the use of a chlorine-containing catalyst will cause organic chlorine impurities to be mixed into the product. product presents difficulties
[0006] CN1394847A discloses supported metal oxides loaded on alumina, including SnO 2 / Al 2 o 3 , Ga 2 o 3 / Al 2 o 3 , MoO 3 al 2 o 3 , ZrO 2 / Al 2 o 3 , TiO 2 / Al 2 o 3 and V 2 o 5 / Al 2 O, reacted at normal pressure and 104°C for 10 hours, the highest EMC yield was 43.6%, the quality of the catalyst in this patent accounted for 8.4% of the total weight of the reaction raw materials, the amount of catalyst was large and the product yield was not high
[0009] In summary, the catalysts that have been reported have problems such as low product yield, difficult recovery, polluted products, large amount of catalyst, harsh requirements for raw materials, and long reaction cycle.

Method used

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  • Method for synthesizing EMC (Ethylmethyl Carbonate) through homogeneously precipitating solid base catalyst
  • Method for synthesizing EMC (Ethylmethyl Carbonate) through homogeneously precipitating solid base catalyst
  • Method for synthesizing EMC (Ethylmethyl Carbonate) through homogeneously precipitating solid base catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] In a three-necked flask, 45 g of dimethyl carbonate and 59 g of diethyl carbonate were charged, the molar ratio of the two was 1:1, and the homemade 20% Ca / SiO 2 (1#), 20% Mg / SiO 2 (2#), 20% Fe / SiO 2 (3#), 20% Cs / SiO 2 (4#), 20% Zn / SiO 2 (5#), 20% Cu / SiO 2 (6#), 20% Ba / SiO 2 (7#), 20% K / SiO2 2 (8#), 20% Ag / SiO 2 (9#), 20% Mn / SiO 2 (10#), 20% Au / SiO 2(11#), 20% Mg / Al 2 o 3 -SiO 2 (12#), 20% Mg / TiO 2 -SiO 2 (13#), 20%Mg / ZrO 2 -SiO 2 (14#), 10% Mg-10% Fe / Al 2 o 3 -SiO 2 (15#), 10% Mg-10% Cs / Al 2 o 3 -SiO 2 (16#), 10%Zn-10%Cu / Al 2 o 3 -SiO 2 (17#), 10% Ba-10% K / Al 2 o 3 -SiO 2 (18#), 10% Mn-10% Ag / Al 2 o 3 -SiO 2 (19#), 10% Mg-10% Cs / Al 2 o 3 -TiO 2 -SiO 2 (20#), 7.5% Ca-7.5% Mg-5% Cs / Al 2 o 3 -SiO 2 (21#), 7.5% Mg-7.5% Ca-5% La / Al 2 o 3 -SiO 2 (22#), 7.5% Ca-7.5% Cs-5% Mn / Al 2 o 3 -SiO 2 (23#), 7.5% Mg-7.5% Cs-5% Mn / Al 2 o 3 -TiO 2 -SiO 2 (24#), 7.5% Mg-7.5% Cs-5% Mn / Al 2 o 3 -ZrO 2 -SiO 2 (25#) Catalyst Each catalyst, the ...

Embodiment 2

[0066] In the fixed bed reactor, the mass ratios of homemade carrier, metal salt solution and urea are 1:0.2:1 (26#), 1:0.2:5 (23#), 1:0.2:10 ( 27#), 1:0.4:5 (28#), 1:0.6:5 ​​(29#) of 7.5% Ca-7.5% Cs-5% Mn / Al 2 o 3 -SiO 2 Catalysts were 50 g each (the source of the active components was the same as 23#), and the amount of deionized water in the preparation process was 15 times the mass of the raw materials; the temperature of the oil bath was gradually heated from room temperature to 90 °C, and the retention time was 6 h, and the aging time of the catalyst was 3 h; the amount of catalyst washing solvent was 10 times that of the catalyst, the drying temperature was 80 °C, and the drying time was 6 h; the catalyst was roasted at 500 °C, and the roasting time was 3 h; Diethyl ester is pumped into the reactor according to the molar ratio of 1:1, under normal pressure conditions, the reaction temperature is 150 °C, and the mass space velocity of raw materials is 20 h -1 After 10...

Embodiment 3

[0071] In the fixed-bed reactor, the self-made 7.5%Ca-7.5%Cs-5%Mn / Al with roasting temperatures of 400, 450, 500, 600, and 800°C were loaded respectively. 2 o 3 -SiO 2 Each catalyst is 50 g (the source of the active component is the same as 23#), in which the mass ratio of carrier, metal salt solution, and urea is 1:0.2:5, and the amount of deionized water in the preparation process is 15 times the mass of the raw material; the oil bath temperature Gradually heated from room temperature to 90°C, the holding time was 6 h, the catalyst aging time was 3 h; the amount of catalyst washing solvent was 10 times that of the catalyst, the drying temperature was 80°C, and the drying time was 6 h; the catalyst roasting time was 3 h ; Use a constant flow pump to pump dimethyl carbonate and diethyl carbonate into the reactor according to the molar ratio of 1:1, under normal pressure conditions, the reaction temperature is 150 ° C, and the mass space velocity of raw materials is 20 h -1 A...

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Abstract

The invention discloses a method for synthesizing EMC (Ethylmethyl Carbonate) through homogeneously precipitating a solid base catalyst, and relates to a method for synthesizing the EMC. A mesoporous-microporous composite solid catalyst simultaneously having a strong base active center and an L acid catalysis center can be prepared through a homogenous precipitation method, and the homogenous precipitation method can be used for efficiently synthesizing the EMC from dimethyl carbonate and diethyl carbonate. A urea hydrolysis method is adopted for preparing a composite carrier and supported alkaline or acidic metalloid oxide, and a single solution or a mixed salt solution of several of metal nitrate, sulfate and hydrochloride is used as a source of an active component for preparing a supported metal catalyst; in kettle reaction, the catalyst after reaction can be repeatedly utilized again through simple filtering, and higher activity of the catalyst still can be kept after the catalystis repeatedly used for many times; the active center of the supported metal catalyst prepared by adopting the urea hydrolysis method is high in dispersion degree and good in crystallinity degree. Compared an impregnation method or a coprecipitation method, the prepared catalyst is higher in catalysis efficiency and better in stability.

Description

technical field [0001] The invention relates to a method for synthesizing ethyl methyl carbonate, in particular to a method for homogeneously depositing a solid base catalyst for synthesizing ethyl methyl carbonate. Background technique [0002] Ethylmethyl carbonate (EMC for short), molecular formula C 4 h 8 o 3 , with a molecular weight of 104.1, a colorless transparent liquid with a slightly pungent odor. Melting point -55°C, boiling point 109°C, insoluble in water, soluble in alcohol, ether and other organic solvents, it is an asymmetric carbonate. Because it contains both methyl and ethyl groups and has the characteristics of dimethyl carbonate and diethyl carbonate, EMC is also a solvent for special fragrances and intermediates, and has a wide range of uses. Ethyl methyl carbonate can be used as a good electrolyte for lithium-ion batteries. EMC has a large dielectric constant, low viscosity, strong solubility for lithium salts, and good low-temperature performance....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96B01J23/34B01J37/03
CPCB01J23/002B01J23/34B01J37/031C07C68/06C07C69/96
Inventor 石磊范家麒叶青刘铭钰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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