Method for producing oxalate through gas-phase reaction of carbon monoxide

A gas-phase reaction, oxalate ester technology, applied in chemical instruments and methods, carbon monoxide or formate reaction preparation, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of low selectivity of oxalate , to achieve a good technical effect

Active Publication Date: 2012-08-29
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 problem of oxalate ester that exists in previous literature, and a kind of new method of producing oxalate ester by CO gas phase reaction is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 100 grams of α-Al 2 o 3 Carrier, by 0.1wt% Pd+0.3wt% Ga / α-Al 2 o 3 content preparation catalyst, its steps are as follows: select palladium nitrate and gallium nitrate, prepare impregnating solution according to the loading capacity of Pd and gallium, in order to prevent metal ion hydrolysis to generate hydroxide or oxide precipitation, add a small amount of nitric acid in impregnating solution, make The pH of the impregnation solution is 0.8, and the specific surface area is 8 square meters per gram of α-Al 2 o 3 The carrier is immersed in the prepared mixed impregnation solution for a period of time, then taken out and placed in the air to dry, dry, and bake in air, nitrogen or argon atmosphere to make Pd-Ga / α-Al 2 o 3 Catalyst A, before use, catalyst A was reduced with hydrogen at a temperature of 300°C for 4 hours, and then CO and methyl nitrite were used as raw materials, wherein the molar ratio of CO to methyl nitrite was 1.2:1, and the reaction tempera...

Embodiment 2

[0028] Weigh 100 grams of α-Al 2 o 3 Carrier, by 0.3wt% Pd+0.8wt% Ga / α-Al 2 o 3content preparation catalyst, its steps are as follows: select palladium nitrate and gallium nitrate, prepare impregnating solution according to the loading capacity of Pd and gallium, in order to prevent metal ion hydrolysis to generate hydroxide or oxide precipitation, add a small amount of nitric acid in impregnating solution, make The pH of the impregnation solution is 6, and the specific surface area is 5 square meters per gram of α-Al 2 o 3 The carrier is immersed in the prepared mixed impregnation solution for a period of time, then taken out and placed in the air to dry, dry, and bake in air, nitrogen or argon atmosphere to make Pd-Ga / α-Al 2 o 3 Catalyst B and Catalyst B were all reduced with hydrogen at a temperature of 300°C for 4 hours before use, and then CO and methyl nitrite were used as raw materials, wherein the molar ratio of CO to methyl nitrite was 1.5:1, and the reaction tem...

Embodiment 3

[0030] Weigh 100 grams of α-Al 2 o 3 Carrier, according to 0.8wt%Pd+2.5wt%Ga / α-Al 2 o 3 content preparation catalyst, its steps are as follows: select palladium chloride and gallium nitrate, prepare impregnating solution according to the load capacity of Pd and gallium, in order to prevent the hydrolysis of metal ion to generate hydroxide or oxide precipitation, add a small amount of nitric acid in impregnating solution, Make the PH of the impregnating solution=3, the specific surface area is 30 square meters / gram α-Al 2 o 3 The carrier is immersed in the prepared mixed impregnation solution for a period of time, then taken out and placed in the air to dry, dry, and bake in air, nitrogen or argon atmosphere to make Pd-Ga / α-Al 2 o 3 Catalyst C and Catalyst C were all reduced with hydrogen at a temperature of 300°C for 4 hours before use, and then CO and methyl nitrite were used as raw materials, wherein the molar ratio of CO to methyl nitrite was 2:1, and at a reaction tem...

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Abstract

The invention relates to a method for producing oxalate through gas-phase reaction of carbon monoxide, and mainly solves the technical problem in the prior art that the target product is low in selectivity. The method adopts a mixed gas containing both nitrous acid ester and carbon monoxide as the raw material, and comprises the step that the raw material is in contact with a precious metal catalyst to produce oxalate under the conditions that the reaction temperature is 100-180 DEG C, the hourly space velocity is 500-10,000 hours <-1> and the reaction pressure is -0.08-1.5MPa, wherein the precious metal catalyst selects palladium as the active component, at least one of gallium or germanium as the additive and at least one of aluminum oxide, silicon oxide or molecular sieve as the carrier. By adopting the technical scheme, the problem is better solved and the method provided by the invention can be used for industrial increase production of oxalate.

Description

technical field [0001] The present invention relates to a kind of method of producing oxalate by CO gas-phase reaction, especially about the method for producing dimethyl oxalate or diethyl oxalate by CO coupling 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/36B01J23/62B01J29/44
Inventor 刘俊涛李斯琴孙凤侠
Owner CHINA PETROLEUM & CHEM CORP
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