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Carbon monoxide gas phase coupling oxalate synthesis catalyst and preparation method and application thereof

A carbon monoxide and catalyst technology, applied in the field of carbon monoxide gas-phase coupling synthesis of oxalate ester catalyst, preparation and application, can solve the problems of low space-time yield of synthetic oxalate ester, low dispersion of active component Pd, etc.

Active Publication Date: 2016-03-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] One of the technical problems to be solved by the present invention is the low dispersion of active component Pd in ​​prior art catalysts and the low space-time yield of synthetic oxalic acid esters. A new catalyst for gas phase synthesis of oxalic acid esters is provided

Method used

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  • Carbon monoxide gas phase coupling oxalate synthesis catalyst and preparation method and application thereof
  • Carbon monoxide gas phase coupling oxalate synthesis catalyst and preparation method and application thereof
  • Carbon monoxide gas phase coupling oxalate synthesis catalyst and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0033] Take 60g of α-alumina carrier. Dissolve 0.3g of palladium chloride and add sodium carbonate 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. Pre-freeze the catalyst precursor at -20°C for 3 hours, then vacuum freeze-dry at -10°C and 10Pa for 8 hours, and then put it in a muffle furnace for 4 hours and roast at 450°C to obtain carbon monoxide gas-phase synthesis of oxalate Catalyst cat-1A.

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

Embodiment 2

[0036] Take 60g of α-alumina carrier. Dissolve 0.8g of palladium chloride and 1.2g of lanthanum nitrate and add sodium carbonate to adjust the pH to 1 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. Pre-freeze the catalyst precursor at -20°C for 3 hours, then vacuum freeze-dry at -15°C and 15Pa for 8 hours, and then put it in a muffle furnace for 4 hours and roast at 450°C to obtain carbon monoxide gas phase synthesis of oxalate Catalyst cat-2A.

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

Embodiment 3

[0039]Take 60g of silica carrier. Dissolve 0.02g of palladium chloride and add sodium carbonate to adjust the pH to 5 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. Pre-freeze the catalyst precursor at -10°C for 10 hours, then vacuum freeze-dry at -10°C and 10Pa for 8 hours, put it in a muffle furnace and bake it at 550°C for 4 hours, and obtain carbon monoxide gas phase synthesis of oxalate after roasting Catalyst cat-3A.

[0040] The test results of the components, palladium dispersion and palladium grain average particle size of the analysis test catalyst are shown in Table 1

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Abstract

The invention relates to a carbon monoxide gas phase coupling oxalate synthesis catalyst and a preparation method and application thereof. The problem that the oxalate synthesis caviation yield is low due to the fact that an existing catalyst is low in active component Pd dispersity and microcrystal content is mainly solved. The catalyst prepared from, by weight, 0.02-3 parts of an active component Pd and 97-100 parts of at least one carrier of alpha-aluminum oxide or a molecular sieve or silicon oxide is prepared through the method comprising the steps of impregnation, vacuum freeze drying and calcination, wherein the dispersity of the active component Pd is larger than 26%. The problems are well solved, and the carbon monoxide gas phase coupling oxalate synthesis catalyst can be used for industrial production of carbon monoxide gas phase coupling oxalate synthesis.

Description

technical field [0001] The invention relates to a preparation method of a carbon monoxide gas-phase coupling synthesis oxalate ester catalyst, in particular to a preparation method of a synthesis dimethyl oxalate or diethyl oxalate catalyst. 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 proc...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/63B01J29/44B01J23/62B01J23/644B01J37/32C07C69/36C07C67/36
Inventor 龚海燕宋海峰
Owner CHINA PETROLEUM & CHEM CORP
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