Method for synthesizing titanium silicalite molecular sieve TS-1 for catalytic hydrogen peroxide oxidation

A titanium-silicon molecular sieve and oxidation reaction technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of long cycle time, complex precursor solution process, and different material properties, so as to reduce usage and shorten Effects of crystallization time and optimized synthesis conditions

Active Publication Date: 2018-03-13
SHANGHAI LVQIANG NEW MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis method needs to form a complex with hydrogen peroxide and an organic titanium source to maintain the stability of the titanium source. The process of configuring the precursor solution of the titanium source is complicated and the cycle is lengthy.
The above shows that in the process of gelation, the mechanism of action of the introduced fluoride or the steps before and after the introduction are different, as well as the difference of the precursor of the fluoride, which will lead to very different properties of the final synthesized material.

Method used

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  • Method for synthesizing titanium silicalite molecular sieve TS-1 for catalytic hydrogen peroxide oxidation
  • Method for synthesizing titanium silicalite molecular sieve TS-1 for catalytic hydrogen peroxide oxidation

Examples

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Embodiment 1

[0070] Weigh and weigh 50.0g ethyl orthosilicate and 2.5g tetrabutyl titanate at room temperature, after mixing uniformly, add 73.2g tetrapropyl ammonium hydroxide solution (12.5wt%), dropwise Keep stirring vigorously to obtain a clear and transparent solution, continue to hydrolyze for 1.5 h, and wash alcohol at 75 ° C for 2 h to obtain a light yellow sol. Take a certain amount of ammonium fluoride solid, dissolve it in concentrated ammonia water (30wt%) to form an ammonia solution of ammonium fluoride, and add this solution dropwise to the light yellow sol, continue stirring evenly, and then add water again to make the mother liquor SiO by molar ratio 2 :TiO 2 :TPAOH:H 2 O:F - =1:0.03:0.17:20:0.12. Then crystallize at 170°C for 24h, and cool down to room temperature. After the obtained crystallization solution was centrifuged, the filter cake was washed until neutral, spray-dried, and calcined at 550° C. for 3 hours to obtain titanium-silicon molecular sieve TS-1F. Its...

Embodiment 2

[0074] Weigh 50.0 g of tetrabutyl titanate and 50.0 g of tetrabutyl titanate at room temperature, and mix them uniformly. Dissolve a certain amount of ammonium fluoride in concentrated ammonia water (30wt%) to form an ammonia solution of ammonium fluoride, and add this solution dropwise to the mixed solution of titanium source and silicon source, after stirring evenly, add 10g, 25wt% Hydrogen peroxide, continue to stir, then add 73.2g tetrapropyl ammonium hydroxide solution (12.5wt%), keep stirring vigorously during the dropwise addition. Hydrolyzed for 1.5h, followed by alcohol at 75°C for 2h to obtain light yellow sol. Add water again, so that the mother liquor is calculated as SiO according to the molar ratio 2 :TiO2 :TPAOH:H 2 O:F - =1:0.03:0.17:20:0.1. Then it was crystallized under hydrothermal conditions at 170°C for 24h, and cooled down to room temperature. After the obtained crystallization solution was centrifuged, the filter cake was washed until neutral, spray...

Embodiment 3

[0076] Weigh 50.0g ethyl orthosilicate and 2.5g tetrabutyl titanate under ice-water bath conditions, after mixing evenly, add 73.2g tetrapropyl ammonium hydroxide solution (12.5wt%), keep vigorous After stirring to obtain a clear and transparent solution, continue to hydrolyze for 3 hours, and chase alcohol at 75°C for 2 hours to obtain a light yellow sol. Dissolve a certain amount of ammonium fluoride in aqueous ammonia (15wt%) to form an aqueous ammonia solution of ammonium fluoride, add this solution dropwise into the light yellow sol, and after stirring evenly, add water again so that the mother liquor is calculated according to the molar ratio. SiO 2 :TiO 2 :TPAOH:H 2 O:F - =1:0.03:0.17:20:0.27. Then crystallize at 180°C for 24h, and cool down to room temperature. After the obtained crystallization solution was centrifuged, the filter cake was washed until neutral, spray-dried, and finally calcined at 550° C. for 3 hours to obtain titanium-silicon molecular sieve TS-...

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Abstract

The invention relates to a method for synthesizing a titanium silicalite molecular sieve TS-1 for catalytic hydrogen peroxide oxidation. The method comprises the following steps of (1) uniformly mixing a titanium source with a silicon source through stirring, so as to obtain clear liquid; (2) mixing an organic template agent with the first clear liquid, hydrolyzing through drastic stirring till clear liquid is formed again, warming to remove glycol so as to obtain second clear liquid, wherein the pH is 11-14; (3) slowly dripping an ammonia solution of ammonium fluoride into the second clear liquid, and stirring while dripping, and finally obtaining clear mother liquid with the same pH as the second clear liquid; (4) crystallizing the clear mother liquid for 12-36 hours at 130-190 DEG C under autogenous pressure, then separating, drying and burning so as to obtain solid powder TS-1 molecular sieve. Compared with the prior art, the method has specific process steps, reduces the particlesize of the crystal due to introduction of fluoride, and improves the catalysis performance.

Description

technical field [0001] The invention relates to a method for synthesizing a titanium-silicon molecular sieve, in particular to a method for synthesizing a titanium-silicon molecular sieve TS-1 for catalyzing the oxidation reaction of hydrogen peroxide. Background technique [0002] Titanium-silicon molecular sieves are new heteroatom molecular sieves that were researched and developed in the early 1980s. The types of titanium-silicon molecular sieves that have been synthesized so far include TS-1, TS-ZSM-11, Ti-Beta, and Ti -MOR, Ti-ITQ-7 and Ti-MWW, Ti-MCM-41, Ti-HMS, Ti-MSU and Ti-SBA-15 with mesoporous structure and TS-48 with larger pore structure, etc. These molecular sieves have excellent catalytic activity and orientation for organic oxidation reactions involving hydrogen peroxide, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, catalytic oxidation of ketone hydrogen peroxide, oxidation of alcohols, hydroxylation of phenols, etc. Oxidation pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/40C07C249/08C07C251/42
Inventor 李春成王鹏飞徐华胜
Owner SHANGHAI LVQIANG NEW MATERIALS CO LTD
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