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Method for producing oxalate by coupling carbon monoxide(CO)

An oxalate ester and coupling technology, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of low selectivity of oxalate ester and low utilization rate of nitrite ester, so as to avoid thermal or catalytic decomposition , the effect of good technical effect

Inactive Publication Date: 2011-10-19
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • 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 of oxalate and the low utilization rate of nitrite in the previous literature, and a new method for producing oxalate by CO coupling is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Using CO and methyl nitrite as raw materials, wherein the molar ratio of CO and methyl nitrite is 1.2:1, palladium-supported alumina is used as a catalyst, and the weight content of metal palladium is 1.5% based on the weight of the carrier. The CO and methyl nitrite raw materials first enter the crystallizer, remove water and alcohol at a temperature of -20°C, and the obtained effluent I enters a coupling reactor at a reaction temperature of 120°C and a reaction pressure of -0.05MPa. Airspeed is 1000 hours -1 Contact with a palladium-containing catalyst under certain conditions to generate a reaction effluent containing dimethyl oxalate. The reaction results are: the single-pass conversion rate of CO is 62.3%, and the selectivity of dimethyl oxalate is 98.2%.

Embodiment 2

[0022] Using CO and methyl nitrite as raw materials, wherein the molar ratio of CO to methyl nitrite is 1.5:1, palladium-supported alumina is used as a catalyst, and the weight content of metal palladium is 0.5% based on the weight of the carrier. The CO and methyl nitrite raw materials first enter the crystallizer, remove water and alcohol at a temperature of -10°C, and the obtained effluent I enters the coupling reactor at a reaction temperature of 130°C and a reaction pressure of 0.05MPa. Speed ​​is 2000 hours -1 Contacting with a palladium-containing catalyst under certain conditions produces a reaction effluent containing dimethyl oxalate, and the reaction results are: the single-pass conversion rate of CO is 55.4%, and the selectivity of dimethyl oxalate is 97.9%.

Embodiment 3

[0024] Using CO and ethyl nitrite as raw materials, wherein the molar ratio of CO to ethyl nitrite is 1:1, palladium-loaded ZSM-5 molecular sieve is used as catalyst (Si / Al molar ratio is 550:1), and the carrier weight As a benchmark, the weight content of metal palladium is 0.8%, CO and ethyl nitrite raw materials first enter the cooler, remove water and alcohol under the condition of temperature-8 ° C, and the effluent I obtained enters the coupling reactor and reacts The temperature is 140°C, the reaction pressure is 0.1MPa, and the reaction space velocity is 3000 hours -1 Contact with a palladium-containing catalyst under certain conditions to generate a reaction effluent containing diethyl oxalate. The reaction results are: the single-pass conversion rate of CO is 66.4%, and the selectivity of diethyl oxalate is 99.1%.

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Abstract

The invention relates to a method for producing oxalate by coupling CO, and mainly aims to solve the technical problem of low selectivity of target products in the prior art. The method comprises the following steps of: a, introducing a raw material mixture containing nitrite and CO into a raw material purifier, removing water and alcohol at the temperature of between 30 DEG C below zero and 10 DEG C to obtain effluent I; and b, introducing the purified effluent I into a coupling reactor, and contacting a palladium-contained catalyst at the reaction temperature of between 100 and 160 DEG C and the reaction space velocity of between 500 and 6,000 hour<-1> under the reaction pressure of between -0.09 and 1.5 MPa to obtain reaction effluent containing oxalate, wherein the raw material purifier used in the step a is a crystallizer or a cooler. The technical scheme solves the technical problem of low selectivity of the target products; and the method can be applied to the industrial production of increasing the yield of the oxalate.

Description

technical field [0001] The invention relates to a method for producing oxalate by CO coupling, in particular to a method for CO coupling with methyl nitrite or ethyl nitrite to produce dimethyl oxalate or diethyl oxalate. 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 heterocyclic compounds. It ...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36
Inventor 杨为民刘俊涛孙凤侠蒯骏
Owner CHINA PETROLEUM & CHEM CORP
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