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Method for preparing oxalate by coupling reaction of CO in gaseous phase

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

Active Publication Date: 2009-07-08
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 of oxalic acid ester in the previous literature, the low technical problem of single-pass conversion rate, and a new CO gas-phase coupling production method for oxalic acid ester is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The mixture of CO and methyl nitrite is used as the raw material, and the molar ratio of CO and methyl nitrite is 1.2:1. The raw material enters from the middle of the reaction separation tower and contacts with the palladium-containing catalyst supported by alumina. Standard, the weight content of palladium is 0.5%, is 110 ℃ at reaction temperature, and reaction contact time is 0.5 second, and reaction pressure is under the condition of 0.08MPa, and reaction generates the stream containing oxalate, while reacting, reaction separation tower The gas-liquid separation is carried out at the same time, the oxalate product is obtained at the bottom of the tower, and the gas phase effluent containing unreacted nitrite and CO is obtained at the top of the tower. The reaction results are as follows: the single pass conversion rate of CO is 68.9%, and the selectivity of dimethyl oxalate is 98.5%.

Embodiment 2

[0018] The mixture of CO and methyl nitrite is used as the raw material, wherein the molar ratio of CO and methyl nitrite is 1.5:1. The raw material enters from the bottom of the reaction separation tower and contacts with the palladium-containing catalyst supported by alumina. Standard, the weight content of palladium is 0.8%, is 140 ℃ at temperature of reaction, and the reaction contact time is 1.5 seconds, and reaction pressure is under the condition of 0.2MPa, and reaction generates the stream containing oxalate, while reacting, reaction separation tower The gas-liquid separation is carried out at the same time, the oxalate product is obtained at the bottom of the tower, and the gas phase effluent containing unreacted nitrite and CO is obtained at the top of the tower. The reaction results are as follows: the single-pass conversion rate of CO is 57.9%, and the selectivity of dimethyl oxalate is 98.9%.

Embodiment 3

[0020] The mixture of CO and methyl nitrite is used as the raw material, wherein the molar ratio of CO and ethyl nitrite is 1:1. The raw material enters from the bottom of the reaction separation tower and contacts with the palladium-containing catalyst supported by ZSM-5 molecular sieve. Carrier is a benchmark, and the weight content of palladium is 1.2%. At reaction temperature, it is 100 ℃, and the reaction contact time is 3 seconds, and reaction pressure is under the condition of 0.5MPa, and reaction generates the stream that contains oxalate, while reacting, reacting The gas-liquid separation is carried out in the separation tower at the same time, the oxalate product is obtained at the bottom of the tower, and the gas phase effluent containing unreacted nitrite and CO is obtained at the top of the tower. The reaction results are as follows: the single pass conversion rate of CO is 75.9%, and the selectivity of diethyl oxalate is 99.2%.

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Abstract

The invention relates to a method for producing oxalic ester by CO gaseous phase coupling, which mainly solves the problems of low selectivity of target products and low single-pass conversion in the prior art. The method adopts a technical proposal that raw materials of nitrous acid ester-containing gas and CO are introduced into a reacting-separating tower and are contacted with palladium-containing catalysts under the condition that the temperature is between 60 and 160 DEG C, the reaction contact time is between 0.5 and 6 seconds, and the reaction pressure is between 0.05 and 1.5 MPa, a gas-liquid mixture containing oxalic ester is generated after the reaction; meanwhile, gas-liquid separation is performed in the reacting-separating tower, an oxalic ester product is obtained at the bottom of the tower, and gaseous phase effluenst containing unreacted nitrous acid ester and CO are obtained at the top of the tower. The method solves the problems well and can be used in industrial production for increasing the yield of the oxalic 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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IPC IPC(8): C07C69/36C07C67/36
Inventor 刘俊涛朱志焱王万民李蕾
Owner CHINA PETROLEUM & CHEM CORP
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