Method for producing oxalic ester with CO coupling

A coupling technology for producing oxalate and coupling, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of low selectivity of oxalate and low conversion rate of CO per pass, and achieve high selectivity , catalytic selectivity and activity improvement, and the effect of reducing cycle energy consumption

Active Publication Date: 2009-07-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is the problem of low oxalate selectivity an...

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] CO and methyl nitrite are used as raw materials I, and the molar ratio of CO and methyl nitrite is 1.2:1. The raw materials first enter the coupling reactor and contact with the palladium-containing catalyst, and the reaction generates unreacted nitrous acid containing nitrogen oxides. The reaction effluent I of methyl ester, CO and dimethyl oxalate; after the reaction effluent I is separated by gas and liquid, the liquid phase reaction effluent II and the gas phase reaction effluent III are obtained, and the gas phase reaction effluent III, O 2 and methanol as the raw material II, and the raw material II enters the regeneration reactor for reaction to generate a gas effluent IV containing methyl nitrite, and the gas effluent IV returns to the coupling reactor to continue the reaction; the liquid phase reaction effluent II is obtained after separation Dimethyl oxalate product. Among them, the reaction conditions of the coupling reactor: the reaction temperature is 90°C,...

Embodiment 2

[0019] CO and methyl nitrite are used as raw materials I, and the molar ratio of CO and methyl nitrite is 1:1. The raw materials first enter the coupling reactor and contact with the palladium-containing catalyst, and the reaction generates unreacted nitrous acid containing nitrogen oxides. Reaction effluent I of methyl ester, CO and dimethyl oxalate ester; after gas-liquid separation of reaction effluent I, liquid-phase reaction effluent II and gas-phase reaction effluent III are obtained, and gas-phase reaction effluent III, O 2 and methanol as the raw material II, and the raw material II enters the regeneration reactor for reaction to generate a gas effluent IV containing methyl nitrite, and the gas effluent IV returns to the coupling reactor to continue the reaction; the liquid phase reaction effluent II is obtained after separation Dimethyl oxalate product. Among them, the reaction conditions of the coupling reactor: the reaction temperature is 120°C, the reaction contact...

Embodiment 3

[0021] CO and ethyl nitrite are used as raw materials I, and the molar ratio of CO and ethyl nitrite is 3:1. The raw materials first enter the coupling reactor and contact with the palladium-containing catalyst, and the reaction generates unreacted nitrous acid containing nitrogen oxides. The reaction effluent I of ethyl ester, CO and diethyl oxalate; after the reaction effluent I is separated by gas and liquid, the liquid phase reaction effluent II and the gas phase reaction effluent III are obtained, and the gas phase reaction effluent III, O 2 and ethanol as the raw material II, the raw material II enters the regeneration reactor for reaction, and generates a gas effluent IV containing ethyl nitrite, and the gas effluent IV returns to the coupling reactor to continue the reaction; the liquid phase reaction effluent II is obtained after separation Diethyl oxalate product. Among them, the reaction conditions of the coupling reactor: the reaction temperature is 130 ° C, the re...

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Abstract

The invention relates to a method for producing oxalic ester by CO coupling, which mainly solves the problems of the prior art such as low selectivity and low CO single pass conversion in producing the oxalic ester by CO coupling. In the invention, firstly CO and nitrite ester are put into a coupling reactor and then contacted with a catalyst containing Pd; liquid phase reaction effluent II and gas phase reaction effluent III are obtained from effluent I through gas-liquid separation; the gas phase reaction effluent III, O2 and monohydric alcohol of C1-C4 are taken as raw material and put into a regeneration reactor for reaction to generate gas effluent IV containing nitrite ester; the gas effluent IV returns to the coupling reactor for continuous reaction and the mol ratio of nitrogen oxide:O2:monohydric alcohol of C1-C4 is 1:0.3-0.5:1-1.5. The technical proposal of obtaining the oxalic ester product by separating the liquid phase reaction effluent II better solves the problem and can be applicable to the industrial production of oxalic ester.

Description

technical field [0001] The invention relates to a method for preparing oxalate by CO coupling, in particular to a method for producing dimethyl oxalate or diethyl oxalate by reacting CO with methyl nitrite in a gas phase method. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in the fine chemical industry to prepare various dyes, medicines, important solvents, extractants and various intermediates. In the 21st century, oxalate, as a degradable and environmentally friendly engineering plastic monomer, has received extensive international attention. In addition, oxalic acid can be obtained by normal pressure hydrolysis of oxalate, and oxalamide can be obtained by normal pressure ammonia solution. Oxalate can also be used as a solvent to produce pharmaceutical and dye intermediates, etc., such as various condensation reactions with fatty acid esters, cyclohexylacetophenone, amino alcohols, and many heterocyclic compound...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36
Inventor 杨为民刘俊涛孙凤侠王万民
Owner CHINA PETROLEUM & CHEM CORP
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