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Method for producing oxalic ester by gas phase CO coupling

A gas-phase coupling, oxalate technology, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalysts, etc. The problems of low space-time yield of ester and low oxygen removal rate of raw materials can achieve the effect of fast reaction rate, reduced stability and complete reaction

Active Publication Date: 2011-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is that the raw material oxygen removal rate that exists in the past literature is low, the technical problem that target product selectivity is low and oxalic acid ester space-time yield rate is low, a kind of new CO gas phase coupling production oxalic acid is provided Ester method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022]The CO gas raw material containing oxygen first enters the deoxidation reactor with NO gas, and contacts with the ZSM-5 molecular sieve catalyst with a Si / Al molar ratio of 20:1. The oxygen in the raw material reacts with NO to form NO 2 , the gaseous phase effluent I of unreacted NO and CO; The gaseous phase effluent I and methyl nitrite enter in the coupling reactor, and contain palladium catalyst (its weight composition is: 0.45%Pd+0.40%K+0.22%Fe / α-Al 2 o 3 ) contact, the reaction generates effluent II containing dimethyl oxalate; the effluent II of dimethyl oxalate obtains dimethyl oxalate product and gas phase effluent III containing nitrogen oxides after separation; wherein, the CO gas containing oxygen The volume concentration of oxygen in the raw material is 8%, and the operating conditions of the deoxygenation reactor are: the reaction temperature is 20°C, the reaction pressure is -0.05MPa, the residence time is 30 seconds, the molar ratio of NO to oxygen in t...

Embodiment 2

[0024] The CO gas raw material containing oxygen first enters the deoxidation reactor with NO gas, and contacts with the ZSM-5 molecular sieve catalyst with a Si / Al molar ratio of 100:1. The oxygen in the raw material reacts with NO to generate NO gas 2 , gas phase effluent I of unreacted NO and CO; gas phase effluent I and methyl nitrite enter in the coupling reactor, and contain palladium catalyst (its weight is composed of: 0.17%Pd+0.12%Fe / α-Al 2 o 3 ) contact, the reaction generates effluent II containing dimethyl oxalate; the effluent II of dimethyl oxalate obtains dimethyl oxalate product and gas phase effluent III containing nitrogen oxides after separation; wherein, the CO gas containing oxygen The volume concentration of oxygen in the raw material is 5%, and the operating conditions of the deoxidation reactor are: the reaction temperature is 50° C., the reaction pressure is 0.01 MPa, the residence time is 20 seconds, and the molar ratio of NO to oxygen in the CO gas r...

Embodiment 3

[0026] The CO gas raw material containing oxygen first enters the deoxidation reactor with NO gas, and contacts with the ZSM-5 molecular sieve catalyst with a Si / Al molar ratio of 200:1. The oxygen in the raw material reacts with NO to form NO 2 , the gas phase effluent I of unreacted NO and CO; the gas phase effluent I and methyl nitrite enter in the coupling reactor, and contain palladium catalyst (its weight composition is: 0.34%Pd+1.0%K+0.46%Mn / α-Al 2 o 3 ) contact, the reaction generates effluent II containing dimethyl oxalate; the effluent II of dimethyl oxalate obtains dimethyl oxalate product and gas phase effluent III containing nitrogen oxides after separation; wherein, the CO gas containing oxygen The volume concentration of oxygen in the raw material is 1%, and the operating conditions of the deoxygenation reactor are: the reaction temperature is 80° C., the reaction pressure is 0.2 MPa, the residence time is 30 seconds, and the molar ratio of NO to oxygen in the...

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Abstract

The invention relates to a method for producing oxalic ester by gas phase CO coupling, which mainly solves the technical problems of low oxygen removal rate of raw materials, low selectivity of target products and low space-time yield of the oxalic ester in the prior art. The method comprises the following steps: (a) firstly, a CO gas raw material containing oxygen and NO gas enter a deoxidizing reactor and contact with a molecular sieve catalyst, and the oxygen in the raw material reacts with the NO to generate a gas phase effluent I containing NO2, unreacted NO and CO; (b) the gas phase effluent I and nitrous acid ester enter a coupling reactor and contact with a palladium-containing catalyst to react to generate an effluent II containing the oxalic ester; and (c) the effluent II of the oxalic ester is separated to obtain the oxalic ester product and a gas phase effluent III containing nitrogen oxides, wherein the mol ratio of the NO to oxygen in the CO gas raw material containing the oxygen in the step (a) is 4-100:1. By using the technical scheme, the problems are better solved and the method can be used for the industrial production for increasing the yield of the oxalic ester.

Description

technical field [0001] The present invention relates to a kind of CO gas-phase coupling production method of oxalate ester, especially about the CO raw material that contains oxygen reacts with NO to remove oxygen first and then is coupled with methyl nitrite or ethyl nitrite to produce dimethyl oxalate or Diethyl oxalate method. 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 ...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J23/89B01J23/656B01J23/63
Inventor 谢在库刘俊涛王万民孙凤侠
Owner CHINA PETROLEUM & CHEM CORP
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