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Method for carbon monoxide gas phase synthesis of oxalate

A carbon monoxide, gas phase synthesis technology, applied in the direction of carbon monoxide or formate reaction preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve the active component Pd dispersion and crystallite content Low, low space-time yield of synthetic oxalate, etc., to achieve the effect of improving catalytic activity and improving utilization rate

Active Publication Date: 2014-10-22
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that active component Pd dispersity and crystallite content in prior art catalyst are low, cause the problem of low space-time yield of synthetic oxalic acid ester, provide a kind of new carbon monoxide vapor phase synthetic oxalic acid ester method

Method used

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  • Method for carbon monoxide gas phase synthesis of oxalate
  • Method for carbon monoxide gas phase synthesis of oxalate
  • Method for carbon monoxide gas phase synthesis of oxalate

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Take 60 g of the alumina support calcined at 1100° C. for 4 hours. Prepare 50 ml of a solution containing 0.03 mol / L palladium chloride and 0.05 mol / L lanthanum nitrate, adjust the pH to 4.0 with 10% (weight) sodium carbonate, and add 1 g tartaric acid 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 was aged in air for 20 hours, dried at 80°C, and then calcined in a muffle furnace at 450°C to obtain the catalyst cat-1A for gas-phase synthesis of oxalate from carbon monoxide.

[0038] Get 40g and make catalyst and pack in reaction tube, feed hydrogen volume space velocity and be 500 hours -1 , the temperature was programmed to 200°C for 6 hours for reduction. Then at a reaction temperature of 140°C, a reaction pressure of 0.2 MPa, a molar ratio of CO to methyl nitrite of 1.5, and a volumetric space velo...

Embodiment 2~8

[0041] According to the preparation method of [Example 1], the catalyst cat-2~8A was prepared only by changing the palladium content of the catalyst, the type and content of the auxiliary agent. See Table 1 for the weight percentage composition of each component of the catalyst and the microcrystalline content and dispersion of palladium, and see Table 2 for the synthesis reaction conditions.

[0042]

Embodiment 9~12

[0044] Use the catalyzer of [embodiment 1], just change the condition of synthetic reaction. See Table 1 for the weight percentage composition of each component of the catalyst and the microcrystalline content and dispersion of palladium, and see Table 2 for the synthesis reaction conditions.

[0045]

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Abstract

The invention relates to a method for carbon monoxide gas phase synthesis of oxalate, and mainly solves the problem of low space time yield of oxalate due to the low dispersion of an active component Pd crystal grain and low microcrystal content in catalysts in the prior art. The method is characterized in that carbon monoxide and a nitrite ester raw material contact with a catalyst under coupling reaction conditions; the catalyst comprises 0.03-3wt% of at least one selected from metallic palladium or palladium oxides, 0.01-3wt% of at least one selected from rare earth elements or rare earth element oxides and 94-99.96wt% of an alumina carrier; the average particle size of metal palladium or palladium oxide crystal grains in the catalyst is 3-12nm; and the dispersity of palladium is greater than 20%.

Description

technical field [0001] The invention relates to a method for synthesizing oxalate in gas phase from carbon monoxide, in particular to a method for synthesizing dimethyl oxalate or diethyl oxalate. 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 high cost and energy consumption. ...

Claims

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Application Information

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IPC IPC(8): C07C69/36C07C67/36B01J23/63
CPCB01J23/002B01J23/63B01J2523/00C07C67/36C07C69/36B01J2523/3706B01J2523/824B01J2523/31B01J2523/3712B01J2523/3737
Inventor 龚海燕刘俊涛宋海峰
Owner CHINA PETROLEUM & CHEM CORP
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