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A kind of in-situ combined regeneration method of deactivated titanium-silicon molecular sieve catalyst

A titanium-silicon molecular sieve and catalyst technology, which is applied in the field of in-situ combined regeneration of titanium-silicon molecular sieve catalysts, can solve the problems of incomplete regeneration of titanium-silicon molecular sieve, cumbersome operation, and short service life of catalysts.

Active Publication Date: 2021-11-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, the above-mentioned treatment methods have technical problems such as cumbersome operation, incomplete regeneration of titanium-silicon molecular sieves, and short service life of catalysts.

Method used

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  • A kind of in-situ combined regeneration method of deactivated titanium-silicon molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 5G inactivated catalyst was filled in a fixed bed reaction tube constant temperature section, 0.5 MPa, 60 ° C for 6 hours, and the amount of feed was 10 g / h. Then, the aqueous oxide solution was introduced, the amount of feed was 5 g / h, and the peroxide mass fraction was 5%, and the treatment time was 12 hours. The aqueous tetramethyl ammonium chloride solution was re-formed, and the amount of feed was 10 g / h, and the mass fraction of tetramethyl chloride was 2%. Processing time 2H. The methanol solvent was subjected to 3 hours, and the amount of feed was 10 g / h. Example A of the titanium silicon molecular sieve catalyst after regeneration was obtained.

Embodiment 2

[0033] The 5G inactivated catalyst was filled in the constant temperature section of the fixed bed reaction tube, from 1.0 MPa, 80 ° C for 12 hours, and the amount of feed was 5 g / h. The peroxide methanol solution was then introduced, the amount of feed was 5 g / h, and the peroxide mass fraction was 10%, and the treatment time was 6 hours. The aqueous solution of 4-.fluated ammonium chloride was incorporated, the feed was 5 g / h, and the quadratic chloride mass fraction was 5%. Processing time is 8h. The acetone solvent was treated again for 2 hours, and the amount of feed was 10 g / h. Example B of the titanium silicon molecular sieve catalyst after regeneration was obtained.

Embodiment 3

[0035] 5G inactivated catalyst was filled in a fixed bed reaction tube constant temperature section, at 1.0 MPa, 100 ° C for 2 hours, and the feed volume was 8 g / h. Then, the peroxide acetone solution was then introduced, the amount of feed was 10 g / h, and the peroxide mass fraction was 12%, and the treatment time was 2 hours. The aqueous tetrabutylammonium chloride solution is then introduced, the amount of feed is 6 g / h, and the mass fraction of tetrabutylammonium chloride is 5%. Processing time is 3h. The acetonitrile solvent was treated again for 6 hours, and the amount of feed was 10 g / h. Example C of titanium silicon molecular sieve catalyst after regeneration was obtained.

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Abstract

The invention discloses an in-situ combined regeneration method for an inactivated titanium-silicon molecular sieve catalyst. The inactivated titanium-silicon molecular sieve catalyst is sequentially treated with a solvent, a urea peroxide solution, and an aqueous ionic liquid solution, and then treated with a solvent again to realize deactivation. The active catalyst is regenerated in situ. The hydrogen peroxide conversion rate, propylene oxide selectivity and hydrogen peroxide effective utilization rate of the titanium-silicon molecular sieve obtained by the combined regeneration method of the present invention are basically restored to the level of fresh catalysts.

Description

Technical field [0001] The present invention belongs to the field of petrochemical catalyst regeneration method, and more particularly to the inner combination regeneration method of a titanium silicon molecular sieve catalyst. Background technique [0002] In 1983, Taramasso et al. First publicly reported (US4410501) synthesis of titanium silicon molecular sieve (TS-1) having an MFI structure. TS-1 has excellent selective catalytic oxidation properties to h 2 O 2 For the oxidizing agent, high activity, selectivity is shown in the reaction of olefin epoxidation, aromatic hydrocarbon hydrocarbon hydroside, oxidation of ketone, oxidation of alcohol and alkane oxidation, and by-products only water, belonging to an environmentally friendly process, Available in people's widespread concern. However, since the TS-1 pore size (0.56 nm × 0.53 nm) on the diffusion limit of the reactants and the product, the reactant and the active center contact is limited, and the product cannot diffuse ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/90B01J29/89B01J38/48B01J38/52
Inventor 黄家辉龙化云吕强贾玉华
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI