Regeneration method of deactivated titanium-silicon molecular sieve

A technology of titanium-silicon molecular sieves and species, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, catalyst regeneration/reactivation, etc., can solve problems such as environmental protection and economic constraints, high material consumption and energy consumption, and cumbersome and complicated operation processes, and achieve Effects of relative crystallinity recovery, pollution reduction, and activity improvement

Active Publication Date: 2014-12-31
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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 10g of the above-mentioned inactivated molecular sieve SH-1, mix it with 65g of filtered waste liquid (from Comparative Example 1, the same below), and then put the mixture into a sealed autoclave with a polytetrafluoroethylene liner and react at 180°C for 12h. After the obtained molecular sieve was filtered and washed, it 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

[0035] Take 12g of BS-1 obtained by roasting and regenerating inactivated TS-1 molecular sieve, mix it with 45g of filtered waste liquid, and then put the mixture into a sealed autoclave with a polytetrafluoroethylene liner and react at 145°C for 54h. After the obtained molecular sieve was filtered and washed, it was dried at 100° C. for 270 minutes, and then calcined at 570° C. for 8 hours to obtain the regenerated TS-1 molecular sieve B.

Embodiment 3

[0037] Take 12g of BS-2 obtained by roasting and regenerating inactivated TS-1 molecular sieve, mix it with 155g of filtered waste liquid, and then put the mixture into a sealed autoclave with Teflon lining and react at 150°C for 24h. After the obtained molecular sieve was filtered and washed, it 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. Including a deactivated titanium-silicon molecular sieve roasting step, the method is characterized by also including the following step before roasting: contacting and mixing the deactivated titanium-silicon molecular sieve and a filtration waste liquid, placing them in an airtight reaction kettle, treating them at 80-200DEG C for at least 2h, then subjecting the treatment product to filtration, washing and drying under normal temperature and pressure. The activity of the regenerated titanium-silicon molecular sieve can be restored to a level close to that of a fresh agent. The method realizes reuse of filtration waste liquid, has low material consumption, and significantly reduces pollution emission.

Description

technical field [0001] The invention relates to a regeneration method of deactivated titanium-silicon molecular sieve. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. TS-1 with MFI structure, TS-2 with MEL structure, and Ti-MWW with larger pore structure have been synthesized so far. 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, oximation of cyclohexanone, oxidation of alcohols, etc. Titanium silicate molecular sieves have good application prospects as redox molecular sieve catalysts. [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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/90B01J29/89B01J38/66B01J38/02
Inventor 史春风朱斌林民汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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