Method for preparing oxalic ester by CO coupling

A coupling technology for oxalate preparation and coupling, which is applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problem of high nitrite content. , poor security and other issues

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

[0010] The technical problem to be solved by the present invention is that there is a CO coupling oxalate ester system in the prior art, and the gas component entering the circulating compressor has high nitrite content and poor safety. A new CO coupling system is provided. oxalate method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Catalyst preparation:

[0028] Dissolve ferric nitrate in water, heat to 80 °C, and impregnate in 5 mm of α-Al by vacuum rotation 2 o 3 pellets, and then dried at 120°C for 4 hours. Dissolve potassium chloride and ammonium chloropalladate in water, adjust the solution with HCl to make the pH value about 4, then heat the solution to 80°C, impregnate it on the carrier again, and then dry it at 140°C for 4 hours, then Calcined at 450°C for 4 hours, then cooled to room temperature to obtain the desired catalyst, the weight composition of which is: 0.45% Pd+0.40% K+0.22% Fe / α-Al 2 o 3 .

[0029] Take by weighing 10 grams of the above-mentioned prepared catalyst, put into a tubular coupling reactor with a diameter of 18 millimeters, the pre-reaction catalyst is at 100 ml / min, the hydrogen molar content is 20%, and the nitrogen molar content is 80% under the condition, from The room temperature was raised to 300°C at a rate of 3°C / min, and after a constant temperature of ...

Embodiment 2

[0032] According to the same method as in Example 1, the weight composition is 0.17%Pd+0.12%Fe / α-Al 2 o 3 the required catalyst.

[0033] Take by weighing 10 grams of the above-mentioned prepared catalyst, put into a tubular coupling reactor with a diameter of 18 millimeters, the pre-reaction catalyst is at 100 ml / min, the hydrogen molar content is 20%, and the nitrogen molar content is 80% under the condition, from The room temperature was raised to 300°C at a rate of 3°C / min, and after a constant temperature of 3 hours, it was lowered to the reaction temperature and fed.

[0034] The gas containing CO and methyl nitrite first enters the coupling reactor to contact with the palladium-containing catalyst, and the reaction generates reaction effluent I containing nitrogen oxides, unreacted methyl nitrite, CO and dimethyl oxalate; After the effluent I is separated from gas and liquid, a liquid-phase reaction effluent II and a gas-phase reaction effluent III are obtained, and t...

Embodiment 3

[0036] According to the same method as in Example 1, the weight composition is 0.34%Pd+1.0%K+0.46%Mn / α-Al 2 o 3 the required catalyst.

[0037] Take by weighing 10 grams of the above-mentioned prepared catalyst, put into a tubular coupling reactor with a diameter of 18 millimeters, the pre-reaction catalyst is at 100 ml / min, the hydrogen molar content is 20%, and the nitrogen molar content is 80% under the condition, from The room temperature was raised to 300°C at a rate of 3°C / min, and after a constant temperature of 3 hours, it was lowered to the reaction temperature and fed.

[0038] The gas containing CO and methyl nitrite first enters the coupling reactor to contact with the palladium-containing catalyst, and the reaction generates reaction effluent I containing nitrogen oxides, unreacted methyl nitrite, CO and dimethyl oxalate; After the effluent I is separated from gas and liquid, a liquid-phase reaction effluent II and a gas-phase reaction effluent III are obtained,...

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Abstract

The invention relates to a method for preparing oxalic ester by CO coupling, by which the main technical problems that in a system for preparing the oxalic ester by CO coupling in the prior art, the content of nitrous acid ester in gas components entering a cyclic compressor is high and the safety is poor are solved. The invention has the technical scheme comprising the following steps: (a) firstly, gas containing CO and nitrous acid ester enters a coupling reactor to contact with a palladium catalyst and react to generate an effluent I; (b) after gas-liquid separation of the reaction effluent I, a liquid phase reaction effluent II and a gas phase reaction effluent III are obtained, and the effluent III contacts with a C1-C9 alcoholic solution in an absorption tower to obtain a liquid phase effluent IV and a gas phase effluent V; and (c) after further gas-liquid separation is carried out on the gas phase effluent V by a condenser for removing the nitrous acid ester, a gaseous effluentVI of which the content of nitrous acid ester is less than 50ppm is obtained, and the gaseous effluent VI reenters a compressing system. The technical scheme better solves the problems and can be used for industrial production of the 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 or ethyl 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 hete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/36B01J23/89B01J23/656
Inventor 刘俊涛宗弘元蒯骏王万民
Owner CHINA PETROLEUM & CHEM CORP
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