Method for preparing oxalate coupling reaction of CO

A technology of oxalate and nitrite, applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problem of low selectivity of oxalate, and achieve the effect of good technical effect

Active Publication Date: 2009-07-08
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 problem of low selectivity of oxalate in the previous literature, providing a new CO coupling method for preparing oxalate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Using CO and methyl nitrite as raw materials, methyl nitrite is divided into two raw materials, the first methyl nitrite and the second methyl nitrite, which enter the first reactor and the second reactor in turn, in which CO The mol ratio with the first strand and the second strand methyl nitrite sum is 1.2: 1, and the mol ratio of the first strand methyl nitrite and the second strand methyl nitrite is 0.5: 1, reactor I and reaction Palladium catalyst I and palladium catalyst II are respectively loaded in the device II, wherein both palladium catalyst I and palladium catalyst II are based on alumina, and the weight content of palladium is 0.5% based on the carrier. The ester raw material first enters the first reactor to contact with palladium catalyst I, and reacts to generate reaction effluent I. The reaction effluent I and the second methyl nitrite raw material enter the second reactor to contact with the palladium catalyst II, and the reaction generates the reactio...

Embodiment 2

[0021]Using CO and methyl nitrite as raw materials, methyl nitrite is divided into two raw materials, the first and the second, and enter the first reactor and the second reactor in turn, wherein, CO and the first methyl nitrite The mol ratio of the sum of methyl nitrite and the second strand is 1.5: 1, and the mol ratio of the first strand of methyl nitrite and the second strand of methyl nitrite is 3: 1, respectively in the reactor I and the reactor II Loading palladium catalyst I and palladium catalyst II, wherein palladium catalyst I is carrier with silicon oxide, and palladium catalyst II is carrier with aluminum oxide, with carrier as benchmark, the weight content of catalyst I palladium is 1.5%, the weight content of catalyst II palladium is 1%, CO and the first methyl nitrite raw material first enter the first reactor to contact with palladium catalyst I, and react to generate reaction effluent I. The reaction effluent I and the second methyl nitrite raw material enter...

Embodiment 3

[0023] Using CO and ethyl nitrite as raw materials, ethyl nitrite is divided into two raw materials, the first ethyl nitrite and the second ethyl nitrite, and they enter the first reactor and the second reactor in turn, wherein, CO The molar ratio with the sum of the first unit of ethyl nitrite and the second unit of ethyl nitrite is 1: 1, and the molar ratio of the first unit of ethyl nitrite and the second unit of ethyl nitrite is 5: 1, and the reaction Load palladium catalyst I and palladium catalyst II in device I and reactor II respectively, wherein palladium catalyst I is carrier with ZSM-5 molecular sieve, and its Si / Al molar ratio is 300: 1, and palladium catalyst II is carrier with alumina, with Carrier is a benchmark, the weight content of catalyst I palladium is 0.6%, the weight content of catalyst II palladium is 3%, CO and the first strand of ethyl nitrite raw material first enter the first reactor to contact with palladium catalyst I, and the reaction generates re...

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PUM

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Abstract

The invention relates to a method for preparing oxalic ester by CO coupling, which mainly solves the problems of low selectivity of target products in the prior art. The method adopts a technical proposal that: the method comprises the following steps that: (a) a first spout of raw materials of gases containing nitrous acid ester and CO enter a first reaction area first to contact a palladium-containing catalyst I to generate a first spout of reaction effluent containing the oxalic ester; and (b) gaseous phase components subjected to the gas-liquid separation or not subjected to separation of the first spout of the reaction effluent and a second spout of gases containing the nitrous acid ester directly enter at least one second reaction area and are contacted with a palladium-containing catalyst II to generate a second spout of reaction effluent containing the oxalic ester, wherein the mol ratio of the first spout of gases containing the nitrous acid ester to the second spout of the gases containing the nitrous acid ester is 0.1-10:1, and the mol ratio of the CO to the sum of the first spout of the nitrous acid ester and the second spout of the nitrous acid ester is 1-3:1. The method solves the problems well and can be used in industrial production for increasing the yield 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 preparing dimethyl oxalate or diethyl oxalate by coupling CO 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 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. I...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36
Inventor 刘俊涛朱志焱王万民
Owner CHINA PETROLEUM & CHEM CORP
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