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Method for producing oxalic acid ester through CO gas phase coupling

A gas-phase coupling, oxalate ester technology, applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problem of low oxalate ester selectivity

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

[0009] The technical problem to be solved by the present invention is the low selectivity problem of oxalic acid ester that exists in the previous literature, and a kind of new CO gas-phase coupling production method of oxalic acid ester is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Use α-alumina as the carrier, all based on the weight of the carrier, prepared by the loading method, the catalyst A with a palladium content of 0.05% and the catalyst B with a palladium content of 0.8%, the loading ratio of the catalyst A and the catalyst B is 1:1, Load catalyst A and catalyst B in sequence in the composite bed reactor. Before use, both catalyst A and catalyst B are reduced with hydrogen at a temperature of 300°C for 4 hours. CO and methyl nitrite are used as raw materials. Among them, CO and nitrous acid The molar ratio of methyl ester is 1.2:1, the reaction temperature is 130°C, and the reaction volume space velocity is 2000 hours -1 , under the condition that the reaction pressure is -0.08MPa, the raw materials are successively contacted with catalyst A and catalyst B in the composite bed reactor, and the reaction is carried out. The reaction result is: the single-pass conversion rate of CO is 78.4%, and the selectivity of dimethyl oxalate is 99.2% ...

Embodiment 2

[0020] With α-alumina as the carrier, all based on the weight of the carrier, the palladium catalyst A with a palladium content of 0.08% and the palladium catalyst B with a palladium content of 0.15% are prepared by the loading method, and the loading ratio of the catalyst A and the catalyst B is 0.2:1 , the catalyst A and the catalyst B are sequentially loaded into the composite bed reactor, and the catalyst A and the catalyst B are reduced with hydrogen at a temperature of 300 ° C for 4 hours before use, and CO and methyl nitrite are used as raw materials, wherein CO and nitrous acid The molar ratio of methyl nitrate is 1.5: 1, the reaction temperature is 110°C, and the reaction volume space velocity is 800 hours -1 , under the condition that the reaction pressure is -0.05MPa, the raw materials are successively contacted with catalyst A and catalyst B in the composite bed reactor, and the reaction is carried out. The reaction result is: the conversion rate of CO per pass is 6...

Embodiment 3

[0022] With α-alumina as the carrier, all based on the weight of the carrier, the catalyst A with a palladium content of 0.08% and the palladium catalyst B with a palladium content of 0.2% are prepared by the loading method, and the loading ratio of the catalyst A and the catalyst B is 0.5: 1, Load catalyst A and catalyst B in sequence in the composite bed reactor. Before use, both catalyst A and catalyst B are reduced with hydrogen at a temperature of 300°C for 4 hours. CO and methyl nitrite are used as raw materials. Among them, CO and nitrous acid The molar ratio of methyl ester is 2: 1, at reaction temperature 140 ℃, reaction volume space velocity is 3000 hours -1 , under the condition that the reaction pressure is -0.02MPa, the raw materials are successively contacted with catalyst A and catalyst B in the composite bed reactor, and the reaction is carried out. The reaction result is: the single-pass conversion rate of CO is 45.2%, and the selectivity of dimethyl oxalate is...

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Abstract

The invention relates to a method for producing oxalic acid ester through CO gas phase coupling. The use of the method is aimed to mainly solving the technical problem of low selectivity of the target product in the prior art. A technical scheme is adopted as follows: the method comprises the steps of: taking mixture gas containing nitrite ester and CO as raw materials, and sequentially contacting the raw materials with catalysts A and B in a composite bed reactor under the conditions that the reaction temperature is 100-180 DEG C, the volumetric idle speed is 500-10,000 hour <1>, the reaction pressure is minus 0.08-1.5MPa, and reacting the nitrate ester with the CO in the raw materials to product the oxalic acid ester, wherein the catalysts A and B are both selected from palladium-containing catalysts, the palladium content in the catalyst A is lower than that in the catalyst B, and the weight filling proportion of the catalysts A and B is 0.1-5:1, thus better solving the problem of low selectivity of the target product in the prior art and being used for industrial production of increasing the oxalic acid ester.

Description

technical field [0001] The invention relates to a method for producing oxalate by gas-phase coupling of CO, in particular to a method for producing dimethyl oxalate or diethyl oxalate by coupling CO with methyl nitrite or ethyl nitrite. 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/36
Inventor 李斯琴刘俊涛李蕾张琳娜
Owner CHINA PETROLEUM & CHEM CORP
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