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Method for reactivating palledium/carbon catalyst

A carbon catalyst and reactivation technology, applied in physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc. Activation and other issues to achieve effective reactivation effect

Inactive Publication Date: 2008-10-08
SINOPEC YANGZI PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And to the heavier palladium / carbon catalyst of deactivation degree, its palladium content only has 0.2~0.3%, adopts the method for washing with alkaline solution to not restore its activity, generally adopt incineration and extract wherein palladium by chemical method, and this method There are disadvantages such as polluting the environment and low resource utilization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 20g of deactivated palladium / carbon catalyst in supercritical CO 2 Add supercritical CO with a temperature of 50℃ and a pressure of 12MPa to the extraction kettle 2 , Extract for 4h.

[0026] Supercritical CO 2 The deactivated catalyst after extraction was placed in a 30% HNO3 solution and heated to boiling for 2 hours. Then wash with deionized water to neutrality and dry.

[0027] Place the dried deactivated catalyst in 200ml of deionized water, then slowly add ammonia water dropwise until the ammonia water concentration in the solution reaches 0.1mol / L, and slowly stir for 2h.

[0028] For the preparation of Pd solution, weigh out 0.062g PdCl according to 0.34% of the weight of the deactivated palladium / carbon catalyst. 2 , Add 20ml ammonia water dropwise to make PdCl 2 Completely dissolved, forming Pd(NH 3 ) 4 Cl 2 Solution: slowly add this solution to the deactivated palladium / carbon catalyst soaked in ammonia water, stir for 3 hours, suction filtration, and wash wi...

Embodiment 2～5

[0031] Change supercritical CO 2 The extraction temperature is 40℃, 60℃, 80℃, 100℃ supercritical CO 2 Extraction deactivation of palladium-carbon catalyst. The rest is the same as in Example 1.

Embodiment 6～8

[0033] Change supercritical CO 2 The extraction pressure uses 9.7MPa, 14MPa, 20MPa supercritical CO 2 Extraction deactivation of palladium-carbon catalyst. The rest is the same as Example 1

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Abstract

The invention relates to a Pd carbon catalyst anew active method. The method did justice of inactivation catalyst to obtain anew active Pd / carbon catalyst supplied for the TA hydrorefining reaction. The method includes: use out threshold CO2 extract washing inactivation Pd / carbon catalyst; put the inactivation Pd / carbon catalyst into nitric acid solution to boil up; after drying park in the hartshorn; in addition add to PdCl2; after filtration get the catalyst prosome; catalyst prosome through NaOH and formaldehyde revert,drying get the anew active Pd / carbon catalyst.

Description

Technical field [0001] The present invention relates to a method for reactivating a palladium / carbon catalyst, and more specifically, to a method for reactivating a palladium / carbon catalyst that has been deactivated in the hydrorefining reaction in the production process of purified terephthalic acid (PTA). Background technique [0002] It is well known that the palladium / carbon catalyst is a special catalyst used in the PTA hydrofining reaction process. During the use of the palladium / carbon catalyst, with the loss of palladium metal in the catalyst, the growth of palladium crystal grains, the poisoning of poisons, the masking of deposits and other factors, the activity of the catalyst gradually decreases until it is completely deactivated. [0003] Palladium is a rare metal, and palladium / carbon catalysts are more expensive. Properly treat the deactivated palladium / carbon catalyst to restore its activity and continue to be used in the TA hydrofining reaction; or treat the deac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/96B01J23/44
Inventor 汪洋王保正袁浩堵文彬周启慧尹淑华
Owner SINOPEC YANGZI PETROCHEM