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Method for preparing ethyl methyl carbonate through ester exchange method

A technology of ethyl methyl carbonate and dimethyl carbonate, applied in the field of preparing chemical raw materials

Inactive Publication Date: 2017-12-15
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0027] In summary, the catalyzers mentioned above all have certain defects in the process of catalyzing dimethyl carbonate and ethanol transesterification to synthesize ethyl methyl carbonate

Method used

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  • Method for preparing ethyl methyl carbonate through ester exchange method
  • Method for preparing ethyl methyl carbonate through ester exchange method
  • Method for preparing ethyl methyl carbonate through ester exchange method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] The prepared Al with composite pore structure 2 o 3 -SiO 2 200 g of the carrier was placed in a muffle furnace and calcined at 500 °C for 4 hours to remove Al 2 o 3 -SiO 2 Adsorbed water; take 0.75 mol (192 g) Mg(NO 3 ) 2 ·6H 2 O, 0.10 mol (21.4 g) MgCl 2 ·6H 2 O was dissolved in 1000 mL deionized water, and the prepared mixed solution of magnesium nitrate and magnesium chloride was impregnated into the calcined Al 2 o 3 -SiO 2 In the carrier channel; the impregnated catalyst precursor was dried in an oven at 120 °C for 10 h; the dried catalyst precursor was calcined in a muffle furnace at 600 °C for 4 h to obtain a MgO loading of 15 % wt and a MgCl loading A supported catalyst with composite pore structure 15% MgO-5% MgCl in the amount of 5% wt 2 / Al 2 o 3 -SiO 2 .

[0070] The catalyst support was replaced by SiO 2 -SiO 2 、Al 2 o 3 -SiO 2 , SiO 2 -Al 2 o 3 、Al 2 o 3 -Al 2 o 3 , single macroporous SiO 2 , single small hole SiO 2 , using a ...

Embodiment 2

[0076] The prepared Al with composite pore structure 2 o 3 -SiO 2 200 g of the carrier was placed in a muffle furnace and calcined at 500 °C for 4 hours to remove Al 2 o 3 -SiO 2 Adsorbed water; take 0.75 mol (192 g) Mg(NO 3 ) 2 ·6H 2 O, 0.10 mol (21.4 g) MgCl 2 ·6H 2 O, 0.025 mol (8.42g) La(NO 3 ) 3 ·H 2 O was dissolved in 1000 mL deionized water, and the prepared mixed solution of magnesium nitrate, magnesium chloride and lanthanum nitrate was impregnated into the calcined Al 2 o 3 -SiO 2 In the carrier channel; the impregnated catalyst precursor was dried in an oven at 120 °C for 10 h; the dried catalyst precursor was calcined in a muffle furnace at 600 °C for 4 h to obtain a MgO loading of 15% wt, MgCl 2 With a loading of 5% wt, La 2 o 3 Supported catalyst 15%MgO-5%MgCl ​​with multi-active centers and composite pore structure with a loading of 2% wt 2 -2%La 2 o 3 / Al 2 o 3 -SiO 2 .

[0077] In the fixed-bed reactor, load 50 g of the catalyst prepared...

Embodiment 3

[0082] In the fixed-bed reactor, 50 g of catalysts prepared in Example 2 were loaded, and dimethyl carbonate and ethanol were pumped into the reactor according to the molar ratio of 1:1 by using a constant flow pump, and the space velocity was 10 respectively. h -1 、20 h -1 、30 h -1 、40 h -1 and 50h -1 , normal pressure, the reaction temperature was 200°C, and it was stabilized for 500 h. After stabilization at different space velocities, samples were taken for chromatographic analysis and calculation. The conversion rate of raw materials, product selectivity and product yield are shown in Table 3.

[0083] Table 3 Effects of different space velocities on raw material conversion, product selectivity and product yield

[0084]

[0085] As can be seen from Table 3, with the increase of space velocity, the conversion rate of raw materials and the yield of ethyl methyl carbonate decreased gradually. The smaller the mass space velocity, the longer the residence time of the ...

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Abstract

The invention provides a method for preparing ethyl methyl carbonate through an ester exchange method, and relates to a method for preparing a chemical raw material. A first catalyst prepared by the method simultaneously has macropore and micropore structures, wherein the macropores can obviously improve the mass transfer effect; and the micropores can obviously improve the specific surface area of a carrier and simultaneously improve the dispersity of active centers. Meanwhile, the prepared first catalyst simultaneously has an alkali active center and a Lewis acid catalytic active center. The prepared 15%MgO-5%MgCl2-2%La2O3 / Al2O3-SiO2 is used in a dimethyl carbonate and ethanol ester exchange fixed bed continuous reaction; when the reaction temperature is 200 DEG C and the space velocity is 30h<-1>, the catalyst is not inactivated after 5000h of continuous reaction, the dimethyl carbonate conversion rate can be kept at 70%, the ethanol conversion rate can be kept at 80%, and the yield of the product ethyl methyl carbonate is 56%; and after the reaction, the catalyst can be reused through simple filtration treatment, and the activity of the catalyst can still be kept unchanged after the catalyst is reused for multiple times.

Description

technical field [0001] The invention relates to a method for preparing chemical raw materials, in particular to a method for preparing ethyl methyl carbonate by transesterification. 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 battery electrolyte solvent, which can impr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/06C07C69/96B01J27/10B01J35/10
CPCC07C68/06B01J27/10B01J35/394B01J35/61C07C69/96
Inventor 张志刚陈飞姚杰石磊王吉宇王玉鑫
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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