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Preparation method of palladium-based supported hydrogenation catalyst and catalyst thereof

A hydrogenation catalyst and supported technology, which is applied in the field of preparation of palladium-based supported hydrogenation catalysts, can solve problems such as poor catalytic performance, particle aggregation, and inability to accurately control the dispersion of active component palladium, and achieve low manufacturing costs and high efficiency. High hydrogen activity and good stability

Pending Publication Date: 2021-01-19
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problem that the dispersion of palladium, the active component of the palladium-carbon catalyst in the prior art, cannot be accurately controlled, and the particle aggregation is easily caused by high-temperature agglomeration, resulting in poor catalytic performance. The invention provides a preparation method of a palladium-based supported hydrogenation catalyst

Method used

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  • Preparation method of palladium-based supported hydrogenation catalyst and catalyst thereof
  • Preparation method of palladium-based supported hydrogenation catalyst and catalyst thereof

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Experimental program
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Effect test

Embodiment 1

[0029] Step (1), zinc nitrate hexahydrate (0.297g), polyvinylpyrrolidone (0.3g) and sodium chloropalladate solution (0.05mol / L, 3ml) were dissolved in 10ml methanol solution, 4.0g gac was dispersed in 10ml In the methanol solution, join in the above-mentioned salt solution, obtain system I; Step (2), dissolve 2-methylimidazole (0.082g) in the 10ml methanol solution, and join it in the system I; Step (3) , transfer the turbid liquid obtained in step (2) to a 250ml reaction kettle with a polytetrafluoroethylene liner, feed 1.0MPa hydrogen, react at 60°C for 2h, and the product is suction filtered, washed, and dried to obtain a catalyst Precursor; step (4), the precursor sample obtained in step (3) was treated at 900° C. for 3 hours under nitrogen atmosphere to obtain catalyst A. The XRD figure and thermogravimetric curve figure of the catalyst precursor prepared in step (3) are shown in respectively figure 1 and figure 2 .

Embodiment 2

[0031] Step (1), zinc nitrate hexahydrate (0.297g), polyvinylpyrrolidone (0.3g) and sodium chloropalladate solution (0.05mol / L, 3ml) were dissolved in 10ml methanol solution, 4.0g gac was dispersed in 10ml In the methanol solution, join in the above-mentioned salt solution, obtain system I; Step (2), dissolve 2-methylimidazole (0.164g) in the 20ml methanol solution, and join it in the system I; Step (3) , transfer the turbid liquid obtained in step (2) to a 250ml reaction kettle with a polytetrafluoroethylene liner, feed 1.0MPa hydrogen, react at 60°C for 2h, and the product is suction filtered, washed, and dried to obtain a catalyst precursor body; step (4), the sample obtained in step (3) was treated at 900° C. for 3 h under a nitrogen atmosphere to obtain catalyst B.

Embodiment 3

[0033] Step (1), zinc nitrate hexahydrate (0.297g), polyvinylpyrrolidone (0.3g) and sodium chloropalladate solution (0.05mol / L, 3ml) were dissolved in 10ml methanol solution, 4.0g gac was dispersed in 10ml In the methanol solution, join in the above-mentioned salt solution, obtain system I; Step (2), dissolve 2-methylimidazole (0.246g) in the 30ml methanol solution, and join it in the system I; Step (3) , transfer the turbid liquid obtained in step (2) to a 250ml reaction kettle with a polytetrafluoroethylene liner, feed 1.0MPa hydrogen, react at 60°C for 2h, and the product is suction filtered, washed, and dried to obtain a catalyst precursor body; step (4), the sample obtained in step (3) was treated at 900° C. for 3 h under a nitrogen atmosphere to obtain catalyst C.

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Abstract

The invention relates to a preparation method and application of a palladium-based supported hydrogenation catalyst. The problems that in a traditional preparation method, dispersion of an active component palladium cannot be accurately controlled, agglomeration is likely to happen at high temperature, and consequently the hydrogenation performance of a catalyst is poor are mainly solved. The preparation method comprises the steps: respectively dispersing palladium salt, zinc salt, an imidazole compound and a carrier in a solvent, proportionally mixing, and sequentially carrying out thermal reaction, reduction and roasting treatment on the mixture to obtain the palladium-based supported catalyst. The method is simple in technological process, easy to control and amplify in process, novel and unique in catalyst structure and high in p-carboxybenzaldehyde conversion efficiency, and has potential industrial application prospect in crude terephthalic acid hydrofining reaction.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to a preparation method of a palladium-based supported hydrogenation catalyst and a catalyst thereof. Background technique [0002] Palladium carbon catalyst is the core catalyst for the hydrogenation of crude terephthalic acid. Specifically, it refers to converting the impurity p-carboxybenzaldehyde (4-CBA) in crude terephthalic acid into other compounds by hydrogenation under the action of a palladium-carbon catalyst, and then purifying crude terephthalic acid through subsequent crystallization and separation steps the goal of. At present, industrial palladium-carbon catalysts are mainly prepared by impregnation. Due to the influence of the surface tension of the impregnation solution and the solvation effect, as well as the weak force between the carrier and the metal salt solution, it is difficult to precisely control the distribution of the active component palladiu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/60C07C51/487C07C63/26
CPCB01J23/60C07C51/487C07C63/26Y02P20/52
Inventor 何丽敏谢在库王仰东畅延青杨贺勤高焕新
Owner CHINA PETROLEUM & CHEM CORP
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