Reactivation method of biotin-intermediate hydrogenation palladium-carbon catalyst

A technology of palladium carbon catalyst and carbon catalyst, which is applied in the direction of catalyst regeneration/reactivation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., which can solve the problem of ineffective catalyst, unstable catalyst, Destroy catalyst structure and other problems, achieve continuous application, solve poisoning, and high activation efficiency

Active Publication Date: 2017-05-31
ZHEJIANG NHU CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN103623843A discloses a method for reactivating the palladium-carbon catalyst, washing the deactivated palladium-carbon catalyst with an alcohol solution, and then using water as a solvent to place the deactivated palladium-carbon catalyst on an ultrasonic cleaning machine for cleaning, then soaking the deactivated catalyst with alkaline water, Finally, wash with water to neutrality, and dry to obtain the reactivated palladium carbon catalyst. Although this method has a certain effect on catalysts with less poisoning, it has little effect on catalysts with deeper poisoning.
This method is also only effective for simple poisoning reactions, but it is not effective for palladium carbon catalysts deeply poisoned by mercaptans, and the oxidation treatment temperature is too high will cause the palladium carbon catalyst carrier activated carbon to be oxidized, destroying the catalyst structure and making the catalyst more unstable

Method used

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  • Reactivation method of biotin-intermediate hydrogenation palladium-carbon catalyst
  • Reactivation method of biotin-intermediate hydrogenation palladium-carbon catalyst
  • Reactivation method of biotin-intermediate hydrogenation palladium-carbon catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment 1 new palladium carbon biotin intermediate hydrogenation

[0034] Add 30 g of the substrate and 150 g of methanol to dissolve completely, add 1.5 g of 7.5% palladium carbon, put it into a high-pressure reactor, replace the air with nitrogen, then replace the nitrogen with hydrogen, then pass through hydrogen at 1.0 MPa, stir and heat up to 80°C, react for 10 hours, and filter out the material palladium on carbon, and the filtrate was sampled for analysis.

[0035] Replace the old palladium carbon that has been filtered with new palladium carbon and repeat the above hydrogenation process. After the reaction is completed, the material is discharged, the palladium carbon is filtered, and the filtrate is sampled and analyzed. The results are shown in Table 1 below

[0036] Table 1 Example 1 New and old palladium carbon hydrogenation activity comparison

[0037] catalyst raw material temperature pressure time Conversion rates new catalyst ...

Embodiment 2

[0039] Add 20ml of methanol to the catalyst filtered after hydrogenation of the new palladium carbon in Example 1, heat up to 50-60°C, stir and wash for 30min, filter and repeat washing 2-3 times; after filtration, put the catalyst in deionized water at 50-90°C and stir Wash for 0.5h to 3h, filter and repeat washing with deionized water for 1 to 2 times. This catalyst adopts embodiment 1 method to evaluate, and reaction finishes, and filter sampling analysis.

Embodiment 3

[0041] Add 15 ml of deionized catalyst washed with methanol and deionized water in Example 2, stir and heat up to 60° C., add 10 g of 30% hydrogen peroxide dropwise, continue stirring for 1 hour, and filter to obtain the oxidized catalyst. This catalyst adopts embodiment 1 method to evaluate, and reaction finishes, and filter sampling analysis.

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Abstract

The invention discloses a reactivation method of a biotin-intermediate hydrogenation palladium-carbon catalyst. The current biotin-intermediate hydrogenation palladium-carbon catalysts have the defects of deep poisoning and difficult treatment of poisoning impurities. The reactivation method comprises the following steps: firstly, washing an inactivated palladium-carbon catalyst with an alcohol, ketone or ester solvent, filtering, washing with pure water, performing oxidation treatment on the palladium-carbon catalyst with hydrogen peroxide, washing the palladium-carbon catalyst with alkaline water after oxidation treatment, then washing with pure water to neutral, filtering, adding a reducer for performing reduction after filtering, washing the palladium-carbon catalyst with pure water to neutral, filtering and drying to obtain the reactivated palladium-carbon catalyst. The reactivation method effectively activates deeply poisoned palladium-carbon catalysts, has high activation efficiency, restores the activity of the poisoned catalysts like a raw catalyst, can effectively solve the problem of catalyst poisoning when applied in production, realizes continuous application and reduces the production cost.

Description

technical field [0001] The invention relates to the field of biotin intermediate hydrogenation, in particular to a method for reactivating a biotin intermediate hydrogenation palladium carbon catalyst. Background technique [0002] Supported palladium-carbon catalyst has good catalytic performance, occupies an extremely important position in petrochemical industry and organic synthesis, and is widely used in various chemical reactions catalyzed by palladium, such as catalytic reforming, reduction of unsaturated hydrocarbons, benzoquinone Reduction, nitro hydrogenation reduction, oxidative dehydrogenation, benzylation hydrogenation deprotection and other reactions. However, during the reaction process of the palladium-carbon catalyst, due to various reasons, the activity of the catalyst gradually decreases. For example, the combination of palladium and sulfur-containing compounds in the material causes sulfur poisoning and deactivation. The active palladium is covered by high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/96B01J38/10B01J38/52B01J38/64B01J38/66B01J38/00
CPCB01J23/96B01J38/00B01J38/10B01J38/52B01J38/64B01J38/66
Inventor 王柳枫徐志超李建清王勇李浩然陈志荣
Owner ZHEJIANG NHU CO LTD
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