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Carbon Monoxide Vapor Phase Synthesis of Oxalate Catalyst

A carbon monoxide, gas phase synthesis technology, applied in the direction of carbon monoxide or formate reaction preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of oxalate conversion rate of nitrite Low yield, low catalyst activity and other problems, to achieve the effect of improving utilization rate and catalytic activity, good dispersion and high adsorption ratio

Active Publication Date: 2018-07-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that there is low catalyst activity in the prior art, and the problems of low conversion rate of nitrite and low space-time yield of oxalate in the process of gas-phase synthesis of oxalate by carbon monoxide provide a new gas-phase synthesis of oxalate by carbon monoxide Ester catalyst

Method used

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  • Carbon Monoxide Vapor Phase Synthesis of Oxalate Catalyst
  • Carbon Monoxide Vapor Phase Synthesis of Oxalate Catalyst
  • Carbon Monoxide Vapor Phase Synthesis of Oxalate Catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 60 g of the alumina support calcined at 1100° C. for 4 hours. Dissolve 0.3 g of palladium chloride in 30 ml of deionized water containing 0.1% fatty alcohol polyoxyethylene ether phosphate, add sodium carbonate after dissolving to adjust the pH to 4.0 to obtain impregnation solution I. Slowly add the impregnating solution I into the carrier, and turn the carrier to make the solution impregnate evenly, so as to prepare the catalyst precursor. The catalyst precursor is aged in the air for 20 hours, then dried at 80°C, then roasted in a muffle furnace at 450°C, and then placed in a reactor where the temperature is programmed to rise to 300°C and reduced by hydrogen for 8 hours to obtain carbon monoxide gas-phase synthesis of oxalate Catalyst cat-1A.

[0031] See Table 1 for the palladium dispersion, palladium grain average particle size, and carbon monoxide adsorption test results of the analytical test catalyst.

Embodiment 2

[0033] Take 60 g of the alumina support calcined at 1100° C. for 4 hours. Dissolve 0.3 g of palladium chloride in 30 ml of deionized water containing 0.1% fatty alcohol polyoxyethylene ether phosphate, add sodium carbonate after dissolving to adjust the pH to 2.0 to obtain impregnation solution I. Slowly add the impregnating solution I into the carrier, and turn the carrier to make the solution impregnate evenly, so as to prepare the catalyst precursor. The catalyst precursor is aged in the air for 20 hours, then dried at 80°C, then roasted in a muffle furnace at 450°C, and then placed in a reactor where the temperature is programmed to rise to 300°C and reduced by hydrogen for 8 hours to obtain carbon monoxide gas-phase synthesis of oxalate Catalyst cat-2A.

[0034] See Table 1 for the palladium dispersion, palladium grain average particle size, and carbon monoxide adsorption test results of the analytical test catalyst.

Embodiment 3

[0036] Take 60 g of the alumina support calcined at 1100° C. for 4 hours. Dissolve 0.3 g of palladium chloride in 30 ml of deionized water containing 0.01% fatty alcohol polyoxyethylene ether phosphate, add sodium carbonate after dissolving to adjust the pH to 4 to obtain impregnation solution I. Slowly add the impregnating solution I into the carrier, and turn the carrier to make the solution impregnate evenly, so as to prepare the catalyst precursor. The catalyst precursor is aged in the air for 20 hours, then dried at 80°C, then roasted in a muffle furnace at 450°C, and then placed in a reactor where the temperature is programmed to rise to 300°C and reduced by hydrogen for 8 hours to obtain carbon monoxide gas-phase synthesis of oxalate Catalyst cat-3A.

[0037] See Table 1 for the palladium dispersion, palladium grain average particle size, and carbon monoxide adsorption test results of the analytical test catalyst.

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Abstract

The invention relates to a catalyst for gas-phase synthesis of oxalate from carbon monoxide. The technical problems to overcome are that catalysts in the prior art is low in activity, and the conversion ratio of nitrite and the space-time yield of oxalate are low in a process of gas-phase synthesis of oxalate from carbon monoxide. According to a technical scheme, at least one of aluminum oxide, silica or a molecular sieve is adopted as a carrier, the carrier is loaded with 0.03-3 wt% of an active component that is palladium and 0-3 wt% of at least one auxiliary agent selected from barium, magnesium, lanthanum, nickel, copper, samarium, calcium, zirconium, cerium, titanium, zinc and cerium, and the ratio of bridged absorption and linear absorption of the carbon monoxide by the palladium is 0.5-5. The problems are overcome by adoption of the technical scheme. The catalyst can be used for industrial gas-phase synthesis of oxalate from carbon monoxide.

Description

technical field [0001] The invention relates to a catalyst for gas-phase synthesis of oxalate from carbon monoxide, in particular to a catalyst for gas-phase synthesis of dimethyl oxalate or diethyl oxalate from carbon monoxide. Background technique [0002] Oxalate is an important organic chemical raw material, which is widely used in fine chemical industry to prepare various dyes, medicines, solvents, extractants and various intermediates. In addition, hydrogenation of oxalate can produce ethylene glycol, a very important chemical raw material, and this route can replace the current method of producing ethylene glycol by the petroleum route with high cost. [0003] Traditional oxalate production routes include starch nitric acid oxidation method, cellulose alkali fusion method, sodium formate method, ethylene glycol one-step oxidation method, propylene oxidation method and oxalate alcohol esterification reaction method, but the above-mentioned traditional processes have hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J23/63B01J23/89B01J23/58B01J29/74C07C69/36C07C67/36
Inventor 龚海燕刘俊涛刘国强
Owner CHINA PETROLEUM & CHEM CORP