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Method for producing oxalic ester by CO coupling

An oxalate ester and coupling technology, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of low single-pass conversion rate of raw materials and low selectivity of oxalate ester

Active Publication Date: 2011-10-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is the low selectivity of oxalate esters and the low conversion rate of raw materials in the previous literature, and a new CO coupling production method for oxalate esters is provided.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025]Using CO and methyl nitrite as raw materials, wherein the molar ratio of CO and methyl nitrite is 1.2:1, the high-gravity rotating bed reactor is loaded with palladium-loaded alumina catalyst, based on the carrier, the weight content of palladium Both are 1.5%. CO and methyl nitrite raw materials enter the rotary bed reactor to contact with the catalyst. At a reaction temperature of 100°C, the reaction pressure is -0.01MPa; The result of the reaction is: the single pass conversion rate of CO is 62.3%, and the selectivity of dimethyl oxalate is 97.2%.

Embodiment 2

[0027] Using CO and methyl nitrite as raw materials, wherein the molar ratio of CO to methyl nitrite is 1.5:1, the high-gravity rotating bed reactor is loaded with palladium-loaded alumina catalyst, based on the carrier, the weight content of palladium Both are 0.5%, CO and methyl nitrite raw materials enter the rotating bed reactor to contact with the catalyst, at a reaction temperature of 150°C, and a reaction pressure of -0.06MPa; under the condition of the rotating speed of the rotor of the high gravity rotating bed reactor being 2000rpm, its The result of the reaction is: the single-pass conversion rate of CO is 55.4%, and the selectivity of dimethyl oxalate is 97.9%.

Embodiment 3

[0029] Using CO and ethyl nitrite as raw materials, wherein the molar ratio of CO to ethyl nitrite is 1:1, a palladium-loaded ZSM-5 molecular sieve catalyst (Si / Al molar ratio of 150 : 1), taking the carrier as a benchmark, the weight content of palladium is 0.8%, CO and ethyl nitrite raw materials enter the rotating bed reactor to contact with the catalyst, at the reaction temperature of 120 ° C, the reaction pressure is -0.02MPa; Under the condition that the rotating speed of the rotor of the bed reactor is 5000 rpm, the reaction result is as follows: the single-pass conversion rate of CO is 66.4%, and the selectivity of diethyl oxalate is 98.1%.

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PUM

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Abstract

The invention relates a method for producing oxalic ester by CO coupling, mainly solving the technical problems of low objective product selectivity and low conversion per pass in the prior art. According to the technical scheme of the method, a raw material mixture containing nitrous acid ester and CO is in contact with a catalyst containing palladium under the conditions that the reaction temperature is 80 to 160 DEG C and the reaction pressure is 0.09 to 1.5MPa, then a reaction effluent containing oxalic ester is generated, wherein the catalyst containing palladium is fixed on a rotor of asuper gravity rotating bed reactor, the molar ratio of CO to nitrous acid ester in the raw material is (1-5):1. The problems are solved better by using the technical scheme of the method disclosed bythe invention. The method disclosed by the invention can be used in the industrial production of increase production of oxalic ester.

Description

technical field [0001] The invention relates to a method for coupling CO to produce oxalate, in particular to a method for coupling CO with methyl nitrite or ethyl nitrite to produce dimethyl oxalate or diethyl oxalate. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in the fine chemical industry to produce 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 compounds. It ca...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36
Inventor 刘俊涛张惠明孙凤侠
Owner CHINA PETROLEUM & CHEM CORP
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