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Preparation method of filled composite catalyst for CO gas-phase coupling synthesizing of oxalate and application of catalyst

A composite structure, catalyst technology, applied in catalyst activation/preparation, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc., can solve the problems of high content, high cost, low utilization rate, etc., achieve low roasting temperature, The effect of catalyst cost reduction and precious metal content reduction

Active Publication Date: 2018-06-22
XINJIANG CORPS MODERN GREEN CHLOR ALKALI CHEM ENG RES CENT LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a noble metal catalyst with high activity and high utilization rate in view of the shortcomings of the existing CO gas-phase oxidative coupling synthesis oxalate ester technology that the catalyst noble metal is evenly distributed in the carrier, the content is high, the cost is high, and the utilization rate is low. , low catalyst cost, simple preparation, low energy consumption filled composite structure catalyst and preparation method thereof

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Filling of alumina framework support

[0032] Dissolve aluminum nitrate nonahydrate in water, add urea as a precipitant, stir and mix evenly to obtain an impregnation filling solution, in which the concentration of aluminum ions is 2.5mol / L, and the molar concentration ratio of aluminum ions and urea is 1:5. Immerse the 4 mm spherical alumina used as the skeleton carrier in the filling liquid, control the temperature at 90°C with a glycerin bath, filter the impregnation residue after immersion for 4 hours, and dry the filled skeleton carrier in an oven at 120°C for 4 hours to remove moisture . The skeleton carrier was impregnated and dried in the above-mentioned impregnated filling solution for 6 cycles to prepare the precursor of the filled composite structure carrier.

[0033] Etching and Immobilization of Carrier Precursors for Filled Composite Structures

[0034] The precursor is etched by immersing it in a hydrochloric acid solution. The concentration of hydrochl...

Embodiment 2

[0040] In addition to the etching and fixing of the carrier precursor of the filled composite structure, the concentration of hydrochloric acid is 0.25mol / L, the immersion and washing time is 1 hour, and when the active components and additives are loaded, PdCl 2 and FeCl 3 Except that the molar concentrations are 0.34mol / L and 0.17mol / L, the other processes are the same as in Example 1, and the Pd content is 0.30wt.% (relative to the alumina skeleton support), and the Pd / Fe atomic ratio is 2:1 Catalyst 0.30%Pd-Fe / Al 2 o 3 @SkeletonCarrier (fill radius to skeleton carrier radius ratio 0.8:1). The reaction performance evaluation is the same as in Example 1, and the reaction results are shown in Table 1.

Embodiment 3

[0042] In addition to the etching and fixing of the carrier precursor of the filled composite structure, the concentration of hydrochloric acid is 0.15mol / L, the dipping and washing time is 1.5 hours, and when the active components and additives are loaded, PdCl 2 and FeCl 3 Except that the molar concentrations are 0.77mol / L and 0.39mol / L, the other processes are the same as in Example 1, and the Pd content is 0.30wt.% (relative to the alumina skeleton support), and the Pd / Fe atomic ratio is 2:1 Catalyst 0.30%Pd-Fe / Al 2 o 3 @skeleton_carrier (0.9:1 ratio of fill radius to skeletal carrier radius). The reaction performance evaluation is the same as in Example 1, and the reaction results are shown in Table 1.

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PUM

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Abstract

The invention relates to a preparation method of a filled composite catalyst for CO gas-phase coupling synthesizing of oxalate and application of the catalyst. The catalyst comprises an aluminum oxideframework, a filled composite carrier which is composed of a filler that fills the framework, an active component Pd which is loaded on the surface of the carrier, and additives Fe and Cu. Compared with the prior art, the catalyst shows outstanding catalyzing performance in the CO gas phase coupling synthesizing of dimethyl oxalate, and the catalyst has the advantages of being low in noble metalPd content, high in utilization rate, and low in cost.

Description

technical field [0001] The invention belongs to the field of catalyst preparation technology and catalytic application, and relates to a preparation method and application of a filled composite structure catalyst for CO gas-phase coupling synthesis of oxalate. Background technique [0002] Oxalate is an important chemical raw material, which can be used to manufacture oxalic acid, oxamide, ethylene glycol and intermediates of some drugs and dyes. Among them, the method of using coal or natural gas as raw material to synthesize oxalate ester and hydrogenation to prepare the basic chemical raw material ethylene glycol is a C1 chemical technology that conforms to the current situation of more coal and less oil in my country and has important strategic significance. [0003] The main production method of traditional oxalate ester is obtained by esterification and dehydration of oxalic acid and alkyl alcohol with toluene or benzene as dehydrating agent. The production method has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J37/02B01J37/08B01J37/18C07C67/36C07C69/36
Inventor 夏伦超夏锐周佳王伟田志坚潘振栋曲炜马怀军
Owner XINJIANG CORPS MODERN GREEN CHLOR ALKALI CHEM ENG RES CENT LTD
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