Method for producing oxalate through carbon monoxide coupling

An oxalate ester and coupling 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 esters existing in the previous literature, and a new method for producing oxalate esters by CO coupling is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve praseodymium oxalate in water, heat to 70°C, and impregnate in Al with an average particle diameter of 50 microns under vacuum rotation 2 o 3 pellets, and then dried at 120°C for 6 hours. Dissolve a certain amount of palladium nitrate in water, adjust the solution with nitric acid to make the pH value about 4, then heat the solution to 80°C, impregnate it on the carrier again, and then dry it at 140°C for 8 hours, then dry it at 450°C in air Calcined in the atmosphere for 4 hours, and reduced in the hydrogen atmosphere at 400°C for 2 hours to obtain catalyst A with a composition of 0.17%Pd+0.28%Pr / Al 2 o 3 . Take by weighing 500 grams of the catalyst that makes, pack in the fluidized-bed reactor, then take CO and methyl nitrite as raw material, wherein, the mol ratio of CO and methyl nitrite is 1.2: 1, at reaction temperature 130°C, the reaction volume space velocity is 2000 hours -1 , under the condition that the reaction pressure is -0.08MPa, the raw mat...

Embodiment 2

[0026] Dissolve praseodymium nitrate in water, heat to 80°C, and impregnate in Al with an average particle diameter of 60 microns under vacuum rotation 2 o 3 pellets, and then dried at 120°C for 4 hours. Dissolve ammonium chloropalladate in water, adjust the solution with nitric acid so that its pH value is about 4, then heat the solution to 80°C, impregnate it on the carrier again, then dry it at 140°C for 4 hours, then dry it at 450°C in an air atmosphere Medium calcination for 4 hours, and reduction in hydrogen atmosphere at 400°C for 2 hours to obtain catalyst B with a composition of 0.45% Pd+0.40% Pr / Al 2 o 3 . Take by weighing 500 grams of the catalyst that makes, pack in the fluidized-bed reactor, then take CO and methyl nitrite as raw material, wherein, the mol ratio of CO and methyl nitrite is 1.5: 1, at reaction temperature 110°C, the reaction volume space velocity is 800 hours -1, under the condition that the reaction pressure is -0.05MPa, the raw material is c...

Embodiment 3

[0028] Dissolve bismuth nitrate in water and vacuum impregnate Al with an average particle diameter of 100 μm 2 o 3 On the pellets, dry at 140°C for 4 hours. Dissolve palladium nitrate in ethanol solution, impregnate on the carrier again, dry at 140°C for 4 hours, then bake in air atmosphere at 450°C for 4 hours, reduce in hydrogen atmosphere at 300°C for 4 hours, and then cool to room temperature in nitrogen atmosphere , to obtain catalyst C, the composition is 0.01%Pd+1%Bi / Al 2 o 3 . Take by weighing 500 grams of the catalyst that makes, pack in the fluidized-bed reactor, be raw material then with CO and methyl nitrite, wherein, the mol ratio of CO and methyl nitrite is 2: 1, at reaction temperature 140 ℃, the reaction volume space velocity is 3000 hours -1 , under the condition that the reaction pressure is -0.02MPa, the raw material is contacted with the catalyst, and the reaction is carried out. The reaction result is: the conversion rate of CO per pass is 45.2%, and...

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Abstract

The invention relates to a method for producing oxalate through carbon monoxide coupling, 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, also adopts a fluidized bed reactor, and comprises the step that 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, the raw material is in contact with a palladium-containing precious metal catalyst in which lanthanum, praseodymium or bismuth is selected as the additive, so as to react to produce oxalate, wherein a catalyst carrier is spherical aluminum oxide with the average particle diameter of 20-300 microns. 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 that produces oxalate by CO coupling, especially about adopting fluidized bed reactor to produce dimethyl oxalate or diethyl oxalate by CO coupling with methyl nitrite or ethyl nitrite method. 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 al...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J23/63B01J23/644
Inventor 刘俊涛孙凤侠蒯骏
Owner CHINA PETROLEUM & CHEM CORP
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