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Regeneration method of deactivated titanium-silicon molecular sieve catalyst

A titanium-silicon molecular sieve and catalyst technology, which is applied in the field of regeneration of deactivated titanium-silicon molecular sieve catalysts, can solve the problems of cumbersome and complicated operation process, high material consumption and energy consumption, environmental protection and economical restrictions, etc., and achieves cost reduction and three waste emissions. , the effect of relative crystallinity recovery

Active Publication Date: 2013-07-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operation process of this method is cumbersome and complicated, and repeated filtration and washing produce a large amount of industrial wastewater containing acid and ammonia nitrogen, which has high material consumption and energy consumption, and is limited in environmental protection and economy.

Method used

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  • Regeneration method of deactivated titanium-silicon molecular sieve catalyst

Examples

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Effect test

Embodiment 1

[0034] This example illustrates the process of regenerating the titanium-silicon molecular sieve catalyst deactivated in the hydroxylation reaction of phenol by the method of the present invention.

[0035] Take 10 g of the above-mentioned inactivated molecular sieve SH-1 and mix it with 6.5 g of filtered waste liquid (from Comparative Example 1, the same below). The mixture was charged into a 50 mL polytetrafluoroethylene liner and placed in a 100 mL polytetrafluoroethylene liner, and then reacted at 180° C. for 12 h in a sealed autoclave. The obtained molecular sieve was dried at 150° C. for 120 minutes, and then calcined at 650° C. for 4 hours to obtain regenerated TS-1 molecular sieve A.

Embodiment 2

[0037] This example illustrates the regeneration process of the deactivated titanium-silicon molecular sieve catalyst in the ammoximation reaction of cyclohexanone using the method of the present invention.

[0038] Take 12g of SH-2 obtained by regenerating and deactivating TS-1 molecular sieve, and mix it with 4.5g of filtered waste liquid. The mixture was filled into 50mL polytetrafluoroethylene liner and placed on the support of 100mL polytetrafluoroethylene liner, while 5mL of water was added under it, and then reacted at 145°C for 54h in a sealed autoclave. The obtained molecular sieve was dried at 100° C. for 270 minutes, and then calcined at 570° C. for 8 hours to obtain regenerated TS-1 molecular sieve B.

Embodiment 3

[0040] This example illustrates the regeneration process of the deactivated titanium-silicon molecular sieve calcined catalyst by the method of the present invention in the phenol hydroxylation reaction.

[0041] Take 12 g of BS-1 obtained by roasting and regenerating inactivated TS-1 molecular sieve, and mix it with 1.5 g of filtered waste liquid. Put the mixture into 50mL polytetrafluoroethylene liner and place it on the support of 100mL polytetrafluoroethylene liner, add water 5mL under it at the same time, and then react in a sealed autoclave at 150°C for 24h. The obtained molecular sieve was dried at 160° C. for 120 minutes, and then calcined at 700° C. for 2 hours to obtain the regenerated TS-1 molecular sieve C.

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Abstract

The invention relates to a regeneration method of a deactivated titanium-silicon molecular sieve catalyst. Including a deactivated titanium-silicon molecular sieve catalyst roasting step, the method is characterized by also including the following step before roasting: contacting and mixing the deactivated titanium-silicon molecular sieve catalyst and a filtration waste liquid obtained in titanium-silicon molecular sieve preparation, placing the mixture in an airtight reaction kettle to undergo a hydro-thermal treatment, then drying the treatment product under normal temperature and pressure without filtering and washing. Specifically, the airtight reaction kettle minimally contains a water amount for forming saturated steam under the reaction conditions, and the treating amount of the deactivated titanium-silicon molecular sieve catalyst is at least 5g / L reaction kettle volume. The method does not need filtering and washing processes, and can directly carry out drying and roasting treatment. The method has low material consumption, activity of the regenerated titanium-silicon molecular sieve can be restored to a fresh agent level, and the filtration waste liquid is utilized, so that the method is environment-friendly.

Description

technical field [0001] The invention relates to a regeneration method of a deactivated titanium-silicon molecular sieve catalyst. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, and Ti-MWW with larger pore structure have been synthesized. This type of molecular sieve has excellent selective oxidation performance and high catalytic activity for many organic oxidation reactions, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, oxidation of cyclohexanone, and oxidation of alcohols. They are used as redox molecular sieves The catalyst has a good application prospect. [0003] TS-1 is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing the transition metal element titanium into the molecular sieve framework with ZSM-5 structure. It no...

Claims

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Application Information

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IPC IPC(8): B01J29/90B01J29/89B01J38/66B01J38/48
Inventor 史春风林民朱斌汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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