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Method for preparing methyl-carbonate

A technology of dimethyl carbonate and carbon monoxide, which is applied in the field of gas-phase catalytic synthesis of dimethyl carbonate and its separation, can solve the problems of low catalyst activity, frequent regeneration, and fast deactivation, and achieve high product yield, convenient operation, and stability good sex effect

Inactive Publication Date: 2004-12-08
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The invention mainly solves the problems of low catalyst activity, fast deactivation, short life, frequent regeneration and the like in the prior art, and provides a gas-phase catalytic synthesis of dimethyl carbonate with high catalyst activity and good stability and its azeotropic distillation separation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0020] Weigh 1ml of PdCl prepared by equal volume impregnation method with a particle size of 20-40 mesh 2 -CuCl 2 -CH 3 COOK / a.c. The catalyst is mixed with 1ml of quartz sand of the same particle size as the catalyst, and placed in a tubular fixed-bed reactor with an inner diameter of 8mm. Carbon monoxide 8.02ml / min, oxygen 4.02ml / min and 2ml / h of methanol solution containing 10% dichloroethane are mixed and heated to 150℃ by a preheater and enter the reaction bed with a space velocity of 1800h -1 The feed composition: methanol 56.1%, carbon monoxide 27.1%, oxygen 13.6%, dichloroethane 3.2%, reaction temperature 160°C, reaction pressure 0.1Mpa. The reaction product was condensed into gas-liquid two phases. The methanol conversion rate was 18.16% and the space-time yield of dimethyl carbonate was 445.1g / l.cat.h as measured by gas chromatography analysis. The catalyst has stable activity during 150 hours of continuous operation.

example 2

[0022] Weigh 1ml of PdCl prepared by equal volume impregnation method with a particle size of 20-40 mesh 2 -CuCl 2 -CH 3 COOK / a.c. The catalyst is mixed with 1ml of quartz sand of the same particle size as the catalyst, and placed in a tubular fixed-bed reactor with an inner diameter of 8mm. 27.3ml / min of carbon monoxide, 10.2ml / min of oxygen and 8.0ml / h of methanol solution containing 10% dichloromethane are mixed and heated to 150℃ by a preheater, and enter the reaction bed with a space velocity of 6415h -1 , Feed composition: methanol 61.2%, carbon monoxide 25.1%, oxygen 9.4%, methylene chloride 4.3%, reaction temperature 160°C, reaction pressure 0.2Mpa. The reaction product was condensed into gas-liquid two phases. The methanol conversion rate was 10.9% and the space-time yield of dimethyl carbonate was 798g / l.cat.h as measured by gas chromatography analysis. The catalyst has stable activity during 150 hours of continuous operation.

example 3

[0024] Weigh 1ml of PdCl prepared by equal volume impregnation method with a particle size of 20-40 mesh 2 -CuCl 2 -CH 3 COOK / a.c. The catalyst is mixed with 1ml of quartz sand of the same particle size as the catalyst, and placed in a tubular fixed-bed reactor with an inner diameter of 8mm. Carbon monoxide 65.9ml / min, oxygen 13.2ml / min are mixed with 6ml / h of methanol solution containing 6% trichloroethylene and heated to 150℃ by a preheater, and enter the reaction bed with a space velocity of 7989h -1 , Feed composition: methanol 39.5%, carbon monoxide 49.4%, oxygen 9.9%, trichloroethylene 1.1%, reaction temperature 170°C, reaction pressure 0.3Mpa. The reaction product was condensed into gas-liquid two phases. The methanol conversion rate was 13.6% and the space-time yield of dimethyl carbonate was 781g / l.cat.h as measured by gas chromatography analysis. The catalyst has stable activity during 150 hours of continuous operation.

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Abstract

A process for preparing the dimethyl carbonate from Co, O2 and methanol features the gas-phase catalytic synthesis by adding the Cl-contained organic substance to said raw materials. Its separation method features the azeotropic rectification where the Cl-contained organic substance is used as azeotropic agent.

Description

Technical field [0001] The invention relates to a preparation method of dimethyl carbonate, and specifically relates to a gas-phase catalytic synthesis of dimethyl carbonate and a separation method thereof. Background technique [0002] Dimethyl carbonate is a new basic chemical raw material with low pollution and wide application in the past ten years. It can carry out methylation, carbonylation, methoxylation and carbonylmethylation reactions. It can replace the highly toxic dimethyl sulfate, phosgene and a variety of alcohols, phenols, amines, hydrazine and ester compounds to react, widely used in medicine, pesticides, dyes, fine chemical intermediates, chemicals for the electronics industry, Food additives, antioxidants, surfactants, solvent gasoline additives, etc. Its role has attracted more and more people's attention, and it is called a green raw material for organic compounding. [0003] The methanol oxidative carbonylation method is currently the most studied and most p...

Claims

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Application Information

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IPC IPC(8): C07C68/00C07C69/96
Inventor 王延吉王淑芳赵新强
Owner HEBEI UNIV OF TECH
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