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Method for preparing oxalate by using CO gaseous phase process

An oxalate, gas phase method, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of nitrogen oxides or nitrite utilization. low rate 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 the low technical problem of nitrogen oxide or nitrite utilization rate existing in the literature in the past, and a kind of new method for preparing oxalate by CO gas phase method is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The mixture of nitrogen oxides from ammonia oxidation, ethanol and air first enters reactor I, producing effluent I containing ethyl nitrite; this effluent is separated to give non-condensable gas (containing N 2 and Ar) the effluent III of effluent II and ethyl nitrite; the effluent III of ethyl nitrite enters the coupling reactor I with the first stream of CO gas, contacts with catalyst I, and reacts to generate diethyl oxalate liquid phase Effluent IV and NO-containing gas phase effluent V; NO-containing gas phase effluent V enters reactor II for oxidative esterification with methanol and oxygen to generate effluent VI containing methyl nitrite, which is obtained after separation The methyl nitrite effluent VII and the second CO gas enter the coupling reactor II, contact with the catalyst II, and react to generate dimethyl oxalate effluent VIII and the NO-containing gas phase effluent IX; the NO-containing gas phase effluent IX and the The NO gas phase effluent V is ...

Embodiment 2

[0028] According to the flow process of embodiment 1, just wherein the molar ratio of the second strand of CO gas and the first strand of CO gas is 100:1; Catalyst I and catalyst II are all selected from palladium as the active component, and its weight composition is: 0.30% Pd+0.2%Bi+0.02%Fe / α-Al 2 o 3 . Reactor I and Reactor II are filled with alumina, C 2 ~C 4 The alkanol is selected from ethanol, and the operating conditions in the reactor I are: the reaction temperature is 70°C, the reaction pressure is 0.5MPa, and the reaction contact time is 150 seconds; the operating conditions in the reactor II are: the reaction temperature is 45°C, and the reaction The pressure is 0.4MPa, the reaction contact time is 30 seconds, the molar ratio of NO, methanol and oxygen in the NO-containing gas phase effluent V is 1:20:0.15; the operating conditions of the coupling reactor I are: the reaction temperature is 150°C , the reaction contact time is 40 seconds, the reaction pressure i...

Embodiment 3

[0030] According to the flow process of embodiment 1, just wherein the molar ratio of the second stream of CO gas and the first stream of CO gas is 150: 1; Catalyst I weight composition is 0.30%Pd+0.2%Bi+0.02%Fe / α-Al 2 o 3 , the weight composition of Catalyst II is 0.6%Pd+0.2%Cu+0.08%Fe / α-Al 2 o 3 . Reactor I and Reactor II are filled with 5A molecular sieves, C 2 ~C 4 The alkanol is selected from n-butanol, and the operating conditions in the reactor I are: the reaction temperature is 50°C, the reaction pressure is -0.02MPa, and the reaction contact time is 30 seconds; the operating conditions in the reactor II are: the reaction temperature is 60 ℃, the reaction pressure is 0.2MPa, the reaction contact time is 10 seconds, the molar ratio of NO, methanol and oxygen in the NO-containing gas phase effluent V is 1:15:0.20; the operating conditions of the coupling reactor I are: reaction temperature The reaction temperature is 130°C, the reaction contact time is 5 seconds, th...

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Abstract

The invention relates to a method for preparing oxalate by using a CO gaseous phase process, which mainly solves the technical problem of low utilization rate of nitric oxides or nitrite in the prior art. The method comprises the following steps of: a, enabling a nitric oxide mixture, C2-C4 alkane alcohol and air to enter a reactor 1 to generate an effluent I containing C2-C4 alkyl nitrite; separating the effluent to obtain a non-condensable gas effluent II and a non-condensable gas effluent III; b, enabling the effluent III and a first path of CO gas to enter a coupling reactor I to generate an oxalate liquid phase effluent IV and an NO-containing gas phase effluent V; c, enabling the effluent V and methane and oxygen to enter a reactor II to generate an effluent VI containing methyl nitrite, separating to obtain a methyl nitrite effluent VII and then enabling the methyl nitrite effluent VII and a second path of CO gas to enter a coupling reactor II to react to obtain a dimethyl oxalate effluent VIII and an NO-containing gas phase effluent IX; d, returning the effluent IX to be mixed with the effluent V for circular use; and e, separating the dimethyl oxalate effluent VIII to obtain a dimethyl oxalate product I. The technical scheme for obtaining the oxalate product II by separating the oxalate liquid phase effluent IV better solves the problem and can be used in the industrialized production for preparing the oxalate by using the CO gas phase process.

Description

technical field [0001] The present invention relates to a method for preparing oxalate by CO gas phase method, especially about CO coupling to prepare dimethyl oxalate, co-produce diethyl oxalate, dipropyl oxalate or dibutyl oxalate, greatly reduce nitrogen oxides Or a method for preparing oxalate by CO gas phase method that consumes 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 ...

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 谢在库刘俊涛孙凤侠王万民
Owner CHINA PETROLEUM & CHEM CORP
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