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
23 Cites 3 Cited by

AI-Extracted 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 epox...
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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.

Application Domain

Technology Topic

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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(6)
  • Comparison scheme(2)

Example Embodiment

[0037] Example 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 sequence: 1) Nitrogen purge for 30min, volumetric space velocity of 80h -1 , Press to 2.5MPa; 2) 3wt% dilute hydrogen peroxide flushing for 12h, dilute hydrogen peroxide space velocity is 5h -1 , Temperature 60℃; 3) Switch to methanol and aqueous solution containing ammonia to modify for 6h, ammonia concentration is 1.0mmol/L, water content is 1wt%, mixed solution mass space velocity is 5h -1 4) Rinse with acetonitrile and hydrogen peroxide aqueous solution for 2h, the hydrogen peroxide content in the mixed solution is 10wt%, and the mass space velocity is 3.0h -1;.
[0039] After the modification is completed, the reaction temperature is adjusted to 35°C, the reaction materials are switched, and the evaluation results of the propylene epoxidation reaction are shown in the following table:
[0040]

Example Embodiment

[0041] Example 2
[0042] The catalyst containing TS-1 molecular sieve is loaded in the reactor and modified in situ in the reactor. Carry out the following modification treatments in sequence: 1) Nitrogen purge for 30min, volumetric space velocity of 100h -1 , Press to 3.0MPa; 2) Containing 5wt% dilute hydrogen peroxide for 24h, the dilute hydrogen peroxide space velocity is 5h -1; 3) Switch to methanol and aqueous solution containing ammonium fluoride to modify for 10h, ammonium fluoride concentration is 3.0mmol/L, water content is 3wt%, mixed solution mass space velocity is 8.0h -1; 4) Washing with a mixed aqueous solution of methanol and hydrogen peroxide for 5h, the hydrogen peroxide content is 15wt%, and the mass space velocity is 3.0h -1; Modification is carried out at 80°C.
[0043] After the modification is completed, the reaction temperature is adjusted to 35°C, the reaction materials are switched, and the evaluation results of the propylene epoxidation reaction are shown in the following table:
[0044]

Example Embodiment

[0045] Example 3
[0046] The catalyst containing TS-1 molecular sieve is loaded in the reactor and modified in situ in the reactor. Carry out the following modification treatments in sequence: 1) Nitrogen purge for 30min, volumetric space velocity of 100h -1 , Press to 3.0MPa; 2) Wash with 5wt% peroxyformic acid aqueous solution for 24h, and the space velocity of the peroxyformic acid aqueous solution is 5h -1; 3) Switch to methanol containing ammonium hydrogen phosphate and aqueous solution modification for 10 hours, the concentration of ammonium hydrogen phosphate is 2.3 mmol/L, the water content is 3 wt%, and the mass space velocity of the mixed solution is 10 hours -1 4) Rinse with a mixed aqueous solution of methanol and hydrogen peroxide for 5h, the hydrogen peroxide content is 15wt%, and the mass space velocity is 3.0h -1; Modification is carried out at 60°C.
[0047] After the modification is completed, the reaction temperature is adjusted to 35°C, and the reaction raw materials are switched. The evaluation results of the propylene epoxidation reaction are shown in the following table:
[0048]
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Description & Claims & Application Information

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