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Method for producing oxalic ester by CO coupling

An oxalate and coupling technology, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalysts, etc. Problems such as low utilization rate of nitrate and low space-time yield

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 the low selectivity of oxalic acid ester, low space-time yield and low technical problem of nitrite utilization rate in the previous literature, and a new CO coupling production method for oxalic acid ester is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] CO coupling catalyst preparation:

[0025] 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 nitrate and palladium nitrate in water respectively, adjust the solution with HCl to make the pH value about 4, then heat the solution to 80°C, and continue to immerse in 5 mm of α-Al 2 o 3 Then dry at 140°C for 4 hours, then bake at 450°C for 4 hours, and drop to room temperature to obtain the desired catalyst, whose weight composition is: 0.45%Pd+0.40%K+0.22%Fe / α-Al 2 o 3 .

[0026] CO and methyl nitrite first enter the coupling reactor to contact with the palladium-containing catalyst, and react to generate reaction effluent I containing nitrogen oxides and dimethyl oxalate; after the reaction effluent I is separated, dimethyl oxalate is obtained. Reaction effluent II and gas phase reaction effluent III containing nitrogen oxides; gas phase reaction ef...

Embodiment 2

[0029] According to the various steps and conditions of Example 1, the weight composition is as follows: 0.30%Pd+0.2%Bi+0.02%Fe / α-Al 2 o 3 palladium-containing catalyst.

[0030] CO and methyl nitrite first enter the coupling reactor to contact with the palladium-containing catalyst, and react to generate reaction effluent I containing nitrogen oxides and dimethyl oxalate; after the reaction effluent I is separated, dimethyl oxalate is obtained. Reaction effluent II and gas phase reaction effluent III containing nitrogen oxides; gas phase reaction effluent III containing nitrogen oxides and O 2 And methanol, after entering the regeneration reactor to react, generate the effluent IV containing methyl nitrite and methanol; the effluent IV containing methyl nitrite and methanol enters the water washing tower to contact with water, and the methyl nitrite is desorbed from the methanol solution , to obtain gas-phase effluent V and liquid-phase effluent VI containing methyl nitrite...

Embodiment 3

[0033] According to the various steps and conditions of Example 1, the weight composition is as follows: 0.6%Pd+0.2%Cu+0.08%Fe / α-Al 2 o 3 palladium-containing catalyst.

[0034] CO and methyl nitrite first enter the coupling reactor to contact with the palladium-containing catalyst, and react to generate reaction effluent I containing nitrogen oxides and dimethyl oxalate; after the reaction effluent I is separated, dimethyl oxalate is obtained. Reaction effluent II and gas phase reaction effluent III containing nitrogen oxides; gas phase reaction effluent III containing nitrogen oxides and O 2 And methanol, after entering the regeneration reactor to react, generate the effluent IV containing methyl nitrite and methanol; the effluent IV containing methyl nitrite and methanol enters the water washing tower to contact with water, and the methyl nitrite is desorbed from the methanol solution , to obtain gas-phase effluent V and liquid-phase effluent VI containing methyl nitrite;...

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PUM

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Abstract

The invention relates to a method for producing oxalic ester by CO coupling, by which the main technical problems of low selectivity, low space-time yield and low oxalic ester utilization rate in producing the oxalic ester by CO coupling in the prior art cen be solved. The invention has the technical scheme comprising the following steps: (a) firstly, CO and nitrous acid ester enter a coupling reactor to contact with a palladium catalyst and react to generate a reaction effluent I containing nitrogen oxide and the oxalic ester; (b) after the reaction effluent I is separated, a reaction effluent II containing the oxalic ester and a gas phase reaction effluent III containing the nitrogen oxide are obtained; (c) the reaction effluent III and O2 and C1-C4 monohydric alcohols enter a regeneration reactor and react to generate an effluent IV; (d) the effluent IV enters a water scrubbing tower and contacts with water to obtain a gas phase effluent V containing the nitrous acid ester and a liquid phase effluent VI; and (e) the gas phase effluent V containing the nitrous acid ester from the step (d) is dried and then returned to the coupling reactor for cycle use. 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 coupling CO to produce oxalate, in particular to a method for producing dimethyl oxalate or diethyl oxalate by reacting CO with 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 heterocyclic compounds. It ca...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J23/89B01J23/656
Inventor 刘俊涛杨为民王万民蒯骏
Owner CHINA PETROLEUM & CHEM CORP
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