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Method for modifying titanium silicon zeolite by aqueous solution containing ammonia

A titanium silicalite and aqueous solution technology, applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problems of complex synthesis process, unfavorable practical application of titanium silicalite, expensive synthetic raw materials, etc., and achieves low cost , the effect of improving space-time yield and simple method

Inactive Publication Date: 2003-04-30
DALIAN QIYUAN TECH CO LTD
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

However, hydrothermal synthesis of ultra-fine titanium silicalite and mesoporous titanium silicalite require not only complex synthesis processes, but also expensive synthetic raw materials, which are not conducive to the practical application of titanium silicalite.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: comparative experiment

[0038] According to Chinese patent application 01140509.0, titanium silicalite TS-1 was hydrothermally synthesized. The grain size of the obtained TS-1 zeolite is 1×2×6 μm, the Si / Ti molar ratio is about 53, and the Si / Al molar ratio is 1343. Get and remove the powder TS-1 zeolite catalyst of organic modulus through roasting and evaluate the catalytic performance of its propylene epoxidation by batch kettle evaluation method, the result is as follows:

[0039] Hydrogen peroxide conversion rate (%) 96.14

[0040] Propylene oxide selectivity (%) 92.46

[0041] Effective utilization rate of hydrogen peroxide (%) 89.21

Embodiment 2

[0043] Repeat embodiment 1, but the TS-1 zeolite catalyst is modified with the method of the present invention before the reaction: 8 grams of powder TS-1 zeolite catalyst through roasting are put into 200ml stainless steel still, add 100ml16M aqueous ammonia solution (liquid-solid volume Ratio of 12.5), sealed treatment at 170 ° C (liquid phase, self-generated pressure). Three samples were processed in parallel, and the sampling time of the three kettles was 6 hours, 79 hours, and 360 hours. After the sample was taken out, it was dried at 100°C, and then fired at 540°C for 3 hours. Evaluate its propylene epoxidation reaction performance with batch kettle as follows:

[0044] Modified treatment for 6 hours:

[0045] Hydrogen peroxide conversion rate (%) 98.31

[0046] Propylene oxide selectivity (%) 85.71

[0047] Effective utilization rate of hydrogen peroxide (%) 99.11

[0048] Modified treatment for 79 hours:

[0049] Hydrogen p...

Embodiment 3

[0057] Example 2 was repeated, but the modification of the powdered TS-1 zeolite catalyst was carried out at 80° C. (liquid phase, normal pressure), and the treatment times were 100 hours, 500 hours and 1200 hours, respectively. The reaction result of modified catalyst is as follows:

[0058] After 100 hours of hydrothermal treatment:

[0059] Hydrogen peroxide conversion rate (%) 97.83

[0060] Propylene oxide selectivity (%) 91.06

[0061] Effective utilization rate of hydrogen peroxide (%) 96.74

[0062] After 500 hours of hydrothermal treatment:

[0063] Hydrogen peroxide conversion rate (%) 98.92

[0064] Propylene oxide selectivity (%) 90.31

[0065] Effective utilization rate of hydrogen peroxide (%) 97.55

[0066] After 1200 hours of hydrothermal treatment:

[0067] Hydrogen peroxide conversion rate (%) 99.17

[0068] Propylene oxide selectivity (%) 87.00

[0069] ...

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Abstract

A process for modifying the TiSi zeolite used as catalyst features that the said TiSi zeolite is modified by making the ammonia contained aqueous solution in liquid or gas phase contact with it or the oxide copmosition containing TiSi zeolite at 80-600 deg.C for 0.5-1200 hr. When the modified catalyst is used to prepare epoxy propane by epoxidizing propene, the output rate can be greatly increased.

Description

technical field [0001] The invention belongs to the technical field of petrochemical catalysts. It involves the modification of titanium silicalite or titanium-containing silicalite oxide compound under the condition of heating by aqueous solution containing ammonia. The modified catalyst is used for the selective oxidation reaction of various hydrocarbons with dilute hydrogen peroxide as oxygen source, especially the epoxidation reaction of dilute hydrogen peroxide and propylene. Background technique [0002] Titanium silicalite, represented by TS-1 (Titanium silicalite-1), can combine hydrogen peroxide in dilute hydrogen peroxide to epoxidize olefins to form epoxides, and make benzene rings to undergo hydroxylation to produce phenol or quinone , make cyclohexanone undergo ammoxidation reaction to generate cyclohexanone oxime, make alcohols undergo selective oxidation reaction to generate aldehyde or ketone. The above-mentioned catalytic reaction is usually carried out at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89
Inventor 郭洪臣王祥生刘娜陈黎行
Owner DALIAN QIYUAN TECH CO LTD
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