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Regeneration method of deactivated catalyst

A technology for deactivated catalysts and catalysts, which is applied in the direction of catalyst regeneration/reactivation, chemical instruments and methods, physical/chemical process catalysts, etc. It can solve the problems that the regeneration methods of deactivated catalysts need to be improved, so as to improve production civilization and regeneration High efficiency and improved production safety

Active Publication Date: 2013-09-11
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, current regeneration methods for deactivated catalysts still need to be improved

Method used

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  • Regeneration method of deactivated catalyst
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  • Regeneration method of deactivated catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] refer to figure 1 , utilize the regeneration method of deactivated catalyst of the present invention to prepare regenerated catalyst, concrete steps are as follows:

[0030]Take 1.1g of deactivated organophosphorus-zerovalent nickel catalyst in a muffle furnace, raise the temperature of the muffle furnace to 100°C, maintain it for 2h, then raise the temperature to 350°C, and perform high-temperature calcination for 5h to obtain nickel oxide; at room temperature , the resulting nickel oxide was reacted with 30% hydrochloric acid to obtain a nickel salt solution; the nickel salt solution was placed in an oven at 200°C for 1h to obtain 1.6g of solid nickel salt; 1.0g of solid nickel salt was added to 8.8 g triphenyl phosphite, under the reduction action of 0.01g Zn powder, prepare catalyst, the quality that obtains catalyst is 6.10g.

[0031] The calculated yield of the regenerated catalyst was 98%.

Embodiment 2

[0033] refer to figure 1 , utilize the regeneration method of deactivated catalyst of the present invention to prepare regenerated catalyst, concrete steps are as follows:

[0034] Take 3.0g of deactivated organophosphorus-zerovalent nickel catalyst in a muffle furnace, raise the temperature of the muffle furnace to 120°C, maintain it for 1h, then raise the temperature to 400°C, and perform high-temperature calcination for 4h to obtain nickel oxide; at 30°C In order to obtain a nickel salt solution, the nickel oxide obtained was reacted with 5% nitric acid; the nickel salt solution was placed in an oven at 180° C. for 2 hours to obtain 4.5 g of solid nickel salt; 1.0 g of solid nickel salt was added to 9.5 g of tri-m-cresyl phosphite were reduced by 0.01 g of Zn powder to prepare a catalyst, and the quality of the obtained catalyst was 4.62 g.

[0035] The calculated yield of the regenerated catalyst was 95%.

Embodiment 3

[0037] refer to figure 1 , utilize the regeneration method of deactivated catalyst of the present invention to prepare regenerated catalyst, concrete steps are as follows:

[0038] Take 4.5g of deactivated organic phosphorus-zero-valent nickel catalyst in a muffle furnace, and raise the temperature of the muffle furnace to 80°C for 3h, then raise the temperature to 500°C, and perform high-temperature calcination for 3h to obtain nickel oxide; at 80°C In order to obtain a nickel salt solution, the obtained nickel oxide was reacted with 20% sulfuric acid; the nickel salt solution was placed in an oven at 150° C. for 3 hours to obtain 7.3 g of solid nickel salt; 1.0 g of solid nickel salt was added to 8.8 g of tri-p-cresyl phosphite were reduced by 0.01 g of Zn powder to prepare a catalyst, and the mass of the obtained catalyst was 5.38 g.

[0039] The calculated yield of the regenerated catalyst was 96%.

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Abstract

The invention relates to a regeneration method of a deactivated catalyst, and an organophosphorus-zero-valent nickel catalyst used for olefin hydrocyanation and isomerization reaction. The regeneration method of the deactivated catalyst is characterized in that the catalyst is the organophosphorus-zero-valent nickel catalyst. The regeneration method comprises the following steps of: roasting the deactivated catalyst at high temperature to obtain nickel oxide; reacting the nickel oxide with acid to obtain a nickel salt solution; drying the nickel salt solution to obtain solid nickel salt; processing the solid nickel salt by reducing so as to obtain the regenerated organophosphorus-zero-valent nickel catalyst. By adopting the regeneration method of the deactivated catalyst, the deactivated catalyst can be effectively regenerated, so that the regenerated catalyst with recovered activity can be obtained successfully.

Description

technical field [0001] The invention relates to the technical field of deactivated catalyst regeneration, in particular, the invention relates to a deactivated catalyst regeneration method and an organophosphorus-zero-valent nickel catalyst. Background technique [0002] Organophosphorus-zerovalent nickel complexes are more and more widely used as coordination catalysts in the hydrocyanation and isomerization of alkenes due to certain steric hindrance effects. However, such catalysts are mostly used for homogeneous catalysis, and the organophosphorus ligands in the catalyst are easily replaced by small molecule reactants during the reaction, which makes nickel change from zero valence to high valence, which leads to catalyst deactivation, which directly and seriously affects Reaction efficiency and production cost. Regenerating the deactivated catalyst can reduce the production cost on the one hand, reduce the discharge of solid waste residue and reduce the pollution to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/40B01J31/24B01J38/00B01J38/02B01J38/62B01J38/60
Inventor 韩明汉陈伟朱善斌左宜赞
Owner TSINGHUA UNIV