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Method for regenerating a palladium catalyst

A palladium catalyst and catalyst technology, applied in the direction of catalyst regeneration/reactivation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of increased loss of precious metals, shortened life of palladium catalysts, complex processes, etc., and achieve rapid diffusion Effect

Inactive Publication Date: 2004-11-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is complex and lengthy, which not only leads to increased loss of precious metals and increased fresh catalyst stock, but also becomes a bottleneck in production, seriously affecting production efficiency
Another example, in the process of preparing isopropyl cyclohexane formic acid and ethyl cyclohexane formic acid by hydrogenation of p-isopropyl benzoic acid and p-ethyl benzoic acid, the life-span of the palladium catalyst is also reduced due to the adsorption of organic impurities. shorten

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0027] These examples illustrate the regeneration effect of toluene-carbon dioxide on the catalyst.

[0028] The palladium charcoal catalyst that has reduced activity by 500g is placed in the container that volume is 1 liters, then adds toluene (Shijiazhuang oil refinery product, chemically pure) by the weight ratio of 1: 1, temperature remains on 40-80 ℃, stirs 4 After hours, the toluene was filtered off.

[0029]Put the palladium-carbon catalyst contacted with toluene in a closed extraction kettle with a volume of 1 liter. The liquid carbon dioxide from the liquid carbon dioxide cylinder is pressurized by a high-pressure metering pump, and then passes through the high-pressure buffer kettle, the extraction kettle, and the first-stage pressure reducing valve in sequence. , secondary pressure reducing valve, separation kettle, and finally vented through wet flow meter measurement. Liquid carbon dioxide was continuously extracted at a flow rate of 8NL / (h·kgCat) for 8 hours at ...

Embodiment 6-9

[0034] These examples demonstrate the effect of dichloromethane-carbon dioxide on catalyst regeneration.

[0035] The palladium charcoal catalyst that has reduced activity by 500g is placed in the container that volume is 1 liter, then adds dichloromethane (Honghe Chemical Co., Ltd. product, chemically pure) by the weight ratio of 1: 1, and temperature remains on 40-60 °C, after stirring for 4 hours, dichloromethane was filtered off.

[0036] Place the palladium carbon catalyst after contacting with dichloromethane in a closed extraction kettle with a volume of 1 liter. The liquid carbon dioxide from the liquid carbon dioxide steel cylinder is pressurized by a high-pressure metering pump, and passes through the high-pressure buffer kettle, the extraction kettle, and the first-stage reducer in sequence. Pressure valve, secondary pressure reducing valve, separation tank, and finally vented by wet flow meter. Liquid carbon dioxide was continuously extracted at a flow rate of 8NL...

Embodiment 10-15

[0038] These examples illustrate the regeneration effect of the solvent-carbon dioxide provided by the present invention on the catalyst.

[0039] 500g of palladium carbon catalyst with reduced activity is placed in a closed extraction kettle with a volume of 1 liter. The liquid carbon dioxide from the liquid carbon dioxide steel cylinder is pressurized by a high-pressure metering pump, and the solvent from another high-pressure metering pump is entrained to pass through the high-pressure buffer in sequence. Kettle, extraction kettle, primary pressure reducing valve, secondary pressure reducing valve, separation kettle, and finally vented by wet flow meter. The solvent-carbon dioxide was extracted continuously at 15 MPa and 80° C. at a flow rate of 8 NL / (h·kgCat) for 8 hours, and then the extraction tank was cooled. The palladium-carbon catalyst taken out from the extraction kettle was evaluated for activity according to the method of Examples 1-5, and the evaluation results a...

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PUM

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Abstract

The regeneration process of supported Pd catalyst includes intermittent or continuous contact between the Pd catalyst with activity lowered in the hydrogenation reaction of unsaturated organic compound and organic solvent, which is one or several selected from toluene, benzene, n-hexane, methane dichloride, ethane dichloride, ethanol and cyclohexane, and CO2 successively or simultaneously; and processing organic solvent and CO2 after contacted with Pd catalyst through separating for reuse. The said method can restore Pd catalyst with activity lowered in the interaction with organic matter, especially Pd catalyst with activity lowered by 70 % or more, effectively.

Description

technical field [0001] The present invention relates to a method for regenerating a palladium catalyst, more particularly to a method for regenerating a supported palladium catalyst used for hydrogenation of unsaturated organic compounds. technical background [0002] Supported palladium catalysts are widely used in the hydrogenation reaction of unsaturated organic compounds, such as olefins, unsaturated carboxylic acids, etc., especially for aryl carboxylic acids, such as benzoic acid, p- In the hydrogenation / purification process of phthalic acid and p-isopropyl benzoic acid. [0003] Usually, in the hydrogenation reaction of unsaturated organic compounds, the main reason for the reduction of catalyst activity is the change of reaction environment, such as reaction temperature and reaction heat (sintering), the physical change of the active center of the catalyst itself, or the accumulation of poisons on the catalyst. . In order to avoid the reduction of catalyst activity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J38/58
Inventor 张晓昕宗保宁闵恩泽卢立军
Owner CHINA PETROLEUM & CHEM CORP
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