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Propylene epoxidation catalyst in-situ modification method

An in-situ modification and catalyst technology, applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of slow activation of propylene epoxidation catalysts, poor PO selectivity, and many by-products. Achieve the effects of shortening the unstable period of driving, improving selectivity, activity and product selectivity

Active Publication Date: 2019-03-08
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problems of slow activation of propylene epoxidation catalyst, many by-products and poor PO selectivity, and provide a method for in-situ modification of propylene epoxidation titanium silicon catalyst, which has the advantages of eliminating catalyst surface impurities and Advantages of side reaction active center, dredging pores, and improving the diffusion performance of reacting substances

Method used

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  • Propylene epoxidation catalyst in-situ modification method
  • Propylene epoxidation catalyst in-situ modification method
  • Propylene epoxidation catalyst in-situ modification method

Examples

Experimental program
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Effect test

Embodiment 1

[0038] The catalyst containing Ti-MWW molecular sieve is loaded in the reactor, and modified in situ in the reactor. Carry out the following modification treatments in turn: 1) Nitrogen purging for 30min, volumetric space velocity is 80h -1 , stamped to 2.5MPa; 2) 3wt% dilute hydrogen peroxide rinse for 12h, dilute hydrogen peroxide space velocity is 5h -1 , temperature 60°C; 3) Switch to methanol and aqueous solution containing ammonia for 6 hours, the ammonia concentration is 1.0mmol / L, the water content is 1wt%, and the mass space velocity of the mixed solution is 5h -1 ; 4) Acetonitrile and hydrogen peroxide aqueous solution were washed for 2h, the hydrogen peroxide content in the mixed solution was 10wt%, and the mass space velocity was 3.0h -1 ;.

[0039] After the modification is completed, adjust the reaction temperature to 35°C, switch the reaction raw materials, and see the following table for the evaluation results of propylene epoxidation reaction:

[0040]

Embodiment 2

[0042] The catalyst containing TS-1 molecular sieve is packed in the reactor and modified in situ in the reactor. Carry out the following modification treatments in turn: 1) Nitrogen purging for 30min, volumetric space velocity is 100h -1 , punched to 3.0MPa; 2) Rinse with dilute hydrogen peroxide containing 5wt% for 24 hours, and the space velocity of dilute hydrogen peroxide is 5 hours -1 ; 3) Switch to methanol and aqueous solution containing ammonium fluoride for 10h modification, the ammonium fluoride concentration is 3.0mmol / L, the water content is 3wt%, and the mass space velocity of the mixed solution is 8.0h -1 ; 4) rinse with methanol and hydrogen peroxide mixed aqueous solution for 5h, the hydrogen peroxide content is 15wt%, and the mass space velocity is 3.0h -1 ; The modification was carried out at 80°C.

[0043] After the modification is completed, adjust the reaction temperature to 35°C, switch the reaction raw materials, and see the following table for the ev...

Embodiment 3

[0046] The catalyst containing TS-1 molecular sieve is packed in the reactor and modified in situ in the reactor. Carry out the following modification treatments in turn: 1) Nitrogen purging for 30min, volumetric space velocity is 100h -1 , punched to 3.0MPa; 2) containing 5wt% peroxyformic acid aqueous solution for 24h, the space velocity of peroxyformic acid aqueous solution is 5h -1 ; 3) switch to methanol containing ammonium hydrogen phosphate and modify the aqueous solution for 10h, the concentration of ammonium hydrogen phosphate is 2.3mmol / L, the water content is 3wt%, and the mass space velocity of the mixed solution is 10h -1 ; 4) Rinse with a mixed aqueous solution of methanol and hydrogen peroxide for 5 hours, the content of hydrogen peroxide is 15wt%, and the mass space velocity is 3.0 hours -1 ; The modification was carried out at 60°C.

[0047] After the modification is completed, adjust the reaction temperature to 35°C, and switch the reaction raw materials. ...

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Abstract

The invention discloses a propylene epoxidation catalyst in-situ modification method. The propylene epoxidation catalyst in-situ modification method achieves in-situ modification of propylene epoxidation catalysts filled inside a reactor and comprises purging a propylene epoxidation catalyst bed inside the reaction through air or nitrogen, then sequentially, inletting peroxide-containing aqueous solution for modification, then switching to a mixed solution composed of organic solvent, water and additives for modification, and lastly switching to an organic solvent-containing and hydrogen peroxide-mixed aqueous solution for modification, thereby achieving the aims of eliminating impurities and side reaction activity centers on the surface of the catalysts, dredging pores and improving the dispersing performance of reaction materials. The propylene epoxidation catalyst in-situ modification method can shorten reaction activating time and improve catalyst activity as well as product selectivity and stability and meanwhile is simple, wide in application range, capable of effectively shortening the starting time and applicable to epoxypropane industrialized production with direct propylene epoxidation.

Description

technical field [0001] The invention relates to the field of preparation of propylene oxide, in particular to a method for in-situ modification of a propylene epoxidation catalyst. Background technique [0002] Propylene oxide (PO) is an important organic chemical intermediate, and its derivatives are widely used in chemical industry, light industry, medicine, food, textile and other industries, and have a profound impact on the development of the chemical industry and the national economy. With the expansion of PO usage and the growth of downstream product usage, PO market demand is increasing. At present, the industrial production of PO mainly adopts chlorohydrin method, co-oxidation method and direct epoxidation method. When the chlorohydrin method is used to synthesize PO, the equipment is severely corroded and consumes a large amount of toxic gas Cl 2 , produces a large amount of "three wastes", which does not meet the requirements of green chemistry and clean product...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D301/12C07D301/14C07D303/04
CPCC07D301/12C07D301/14C07D303/04B01J29/89Y02P20/52
Inventor 宋万仓洪鲁伟潘月秋王银斌臧甲忠刘冠锋于海斌石芳王凌涛季超
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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