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Preparation method of catalyst for CO gas-phase catalyzed synthesis of dimethyl oxalate

A technology of dimethyl oxalate and catalyst, which is applied in the field of carbon monoxide gas-phase catalytic synthesis of dimethyl oxalate, can solve the problems of increased cost, complex synthesis conditions, lack of technical means, etc., and achieve reduced usage, high catalytic activity, and high practicality Effects on value and application prospects

Inactive Publication Date: 2016-05-25
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the synthesis conditions are relatively complicated, and various functional reagents are used, such as stabilizers, templates, etc., and the cost is greatly increased, and there is no technical means for large-scale method application at this stage, and there is no relevant test data.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve 0.15g of palladium acetate in 100ml of acetic acid solution with a concentration of 10%, weigh 100g of a spherical alumina carrier with a particle size of 3mm and soak it in the above impregnation mother liquor containing palladium acetate, let it stand for 6h, and then pour out the excess liquid ,

[0020] The alumina balls were put into 100 ml of 50% aqueous methanol solution, and then the reaction vessel was placed in a drying oven at a constant temperature of 60° C. for 12 hours. Pour out the excess liquid, fully wash the reduced sample with deionized water 10 times, then put the alumina ball into the evaporating dish, and place it in a constant temperature drying oven from room temperature to 150°C at a rate of 5°C / min. , keep the temperature for 3h, then raise the temperature to 250°C at a rate of 1-2°C / min, keep the temperature for 5h and then lower it to room temperature, that is, Pd / Al 2 o 3 catalyst.

[0021] Get 10ml about 6.5g above-mentioned cat...

Embodiment 2

[0023] Dissolve 0.2g of palladium nitrate and 0.2g of magnesium nitrate in 100ml of deionized water, weigh 100g of a spherical alumina carrier with a particle size of 3mm and soak it in the above impregnation mother liquor containing palladium acetate, let it stand for 6h, and then pour out the excess liquid , put the alumina ball into 100 ml of 30% methanol aqueous solution, and then place the reaction vessel in a constant temperature drying oven at 60° C. for 12 hours. Pour out the excess liquid and keep it for later use. Wash the reduced sample with deionized water for 10 times, then put the alumina ball into the evaporating dish, and place it in a constant temperature drying oven from room temperature to 150 at a rate of 5°C / min. ℃, keep the temperature for 3h, then raise the temperature to 300°C at a rate of 1-2°C / min, keep the temperature for 3h and then lower it to room temperature to get Pd-Mg / Al 2 o 3 catalyst.

[0024] Adopt the condition with embodiment 1 to evalu...

Embodiment 3

[0026] The preparation steps are the same as in Example 1, except that the reducing agent is 100% formaldehyde solution.

[0027] Adopt the condition with embodiment 1 to evaluate, gained oxalate yield is 640g / h l, and DMO content is 97.5% in the liquid phase product, wherein contains 1.2% dimethyl carbonate, 0.8% methyl formate and Trace amounts of other by-products.

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Abstract

The invention provides a preparation method of a catalyst for CO gas-phase catalyzed synthesis of dimethyl oxalate. Palladium chloride, palladium nitrate, palladium acetate and other conventional palladium salt are used as precursors, spherical aluminum oxide with the diameter of 1-5 mm is used as a carrier, and a dipping and direct-reduction mode, namely direct reduction and dipping conducted on carrier spheres precious metal components by adopting a mild reducing agent, is adopted to enable an active component palladium to be supported on an alumina carrier in more optimized state so as to prepare the supported Pd-M / Al2O3 catalyst. The catalyst prepared by means of the method has higher active component dispersity and has good catalytic activity on CO based dimethyl oxalate synthesis reaction under the condition of lower precious metal content.

Description

technical field [0001] The invention relates to a technology for preparing a supported catalyst by adopting an improved impregnation method, which is mainly used for the gas-phase catalytic synthesis of dimethyl oxalate from carbon monoxide. Background technique [0002] "CO gas-phase catalytic coupling synthesis of oxalic acid diester" is an important topic in the research and development of C1 chemical industry at home and abroad. It has attracted extensive attention because of its advantages such as mild reaction conditions, high efficiency, energy saving, and no pollution. [0003] For the oxalate synthesis catalyst, the catalyst used in the world's first 10,000-ton coal-to-ethylene glycol industrial device that passed the acceptance test in 2009 is Pd-Fe / Al 2 o 3 The catalyst has a noble metal Pd content of 1.2% to 1.5%, a performance index of DMO yield of 750g / L·h, and is prepared by a traditional impregnation method. The type and performance of industrially applied c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/58C07C69/36C07C67/36
CPCB01J23/44B01J23/58C07C67/36C07C69/36
Inventor 姚元根潘鹏斌张鑫黄园园覃业燕周张锋林凌
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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