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Method for preparing TS-1 microsphere catalyst

A technology of TS-1 and catalyst is applied in the field of preparing TS-1 microsphere catalyst, which can solve the problems of affecting process efficiency and difficult separation of finished catalyst products, and achieve the effects of good catalytic activity, avoiding difficult separation and good mechanical strength.

Inactive Publication Date: 2019-11-15
淄博恒亿化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the finished powdered catalyst is not easy to separate from the reaction system, which affects the process efficiency to a certain extent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] SiO in silicon source 2 : Template agent: TiO in titanium source 2 :H 2 O (molar ratio) = 1:0.3:0.02:30, first stir and mix tetrapropylammonium hydroxide solution and tetraethyl silicate solution evenly, slowly add tetrabutyl titanate to the above solution under vigorous stirring, and stir Evenly, place for 12 hours; transfer the above reaction mixture to a high-pressure reactor, crystallize at 80°C for 24 hours, then crystallize at 110°C for 2 hours, and finally crystallize at 160°C for 24 hours. The crystallized reaction mixture is filtered and washed , dried and calcined to obtain TS-1 powder catalyst. Mix the prepared powdery TS-1 catalyst with a 30% silica solution evenly, and spray it onto a high-speed rotating turntable. The material is thrown out by centrifugation and falls in a nitrogen atmosphere at 400°C. When the material reaches the bottom of the tank, it is dried and forms TS-1 microspheres.

Embodiment 2

[0023] SiO in silicon source 2 : Template agent: TiO in titanium source 2 :H 2 O (molar ratio) = 1:0.5:0.02:30, first stir and mix tetrapropylammonium hydroxide solution and tetraethyl silicate solution evenly, slowly add tetrabutyl titanate to the above solution under vigorous stirring, and stir Evenly, place it for 12 hours; transfer the above reaction mixture to a high-pressure reactor, crystallize at 80°C for 24 hours, then crystallize at 110°C for 2 hours, and finally crystallize at 180°C for 24 hours. The crystallized reaction mixture is filtered and washed , dried and calcined to obtain TS-1 powder catalyst. Mix the prepared powdery TS-1 catalyst with a 30% silica solution evenly, and spray it onto a high-speed rotating turntable. The material is thrown out by centrifugation and falls in a nitrogen atmosphere at 400°C. When the material reaches the bottom of the tank, it is dried and forms TS-1 microspheres.

Embodiment 3

[0025] SiO in silicon source 2 : Template agent: TiO in titanium source 2 :H 2 O (molar ratio) = 1:0.7:0.02:30, first stir and mix tetrapropylammonium hydroxide solution and tetraethyl silicate solution evenly, slowly add tetrabutyl titanate to the above solution under vigorous stirring, and stir Evenly, place for 8 hours; transfer the above reaction mixture to a high-pressure reactor, crystallize at 80°C for 24 hours, then crystallize at 110°C for 2 hours, and finally crystallize at 175°C for 24 hours. The crystallized reaction mixture is filtered and washed , dried and calcined to obtain TS-1 powder catalyst. Mix the prepared powdery TS-1 catalyst with a 30% silica solution evenly, and spray it onto a high-speed rotating turntable. The material is thrown out by centrifugation and falls in a nitrogen atmosphere at 400°C. When the material reaches the bottom of the tank, it is dried and forms TS-1 microspheres.

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PUM

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Abstract

The invention provides a method for preparing a TS-1 microsphere catalyst. According to the technical scheme, a hydrothermal synthesis method is adopted, tetrabutyl titanate is adopted as a titanium source, tetraethyl orthosilicate is adopted as a silicon source, tetrapropylammonium hydroxide is adopted as a template agent, mixing, filtering, washing, drying and calcination synthesis are performedto obtain a TS-1 powder catalyst, and a spraying forming method is adopted for preparing the TS-1 microsphere catalyst. The synthesized catalyst is good in mechanical intensity and good in catalyticactivity, the catalyst can be easily separated from reaction system liquid phase substances, and the catalyst is applicable to large-scale industrial production. The hydrothermal synthesis method is used for preparing the powdered TS-1 catalyst, and on the basis, the spraying forming method is used for preparing TS-1 microspheres. The catalytic activity of the powdered catalyst synthesized by thehydrothermal synthesis method is reserved, and the microsphere catalyst avoids defect that the powdered catalyst is not likely to be separated in the reaction process.

Description

technical field [0001] The invention relates to the technical field of inorganic chemical synthesis, in particular to a method for preparing a TS-1 microsphere catalyst. Background technique [0002] TS-1 molecular sieve is a heteroatom molecular sieve with a skeleton structure composed of silicon and titanium. It has MFI topology and three-dimensional ten-membered ring channels. The four-coordinated titanium isolated on the skeleton is the catalytic active center of TS-1 molecular sieve. The oxidation system composed of it and hydrogen peroxide shows good selectivity for olefin epoxidation, ketone ammoximation and alkane oxidation. TS-1 exhibits excellent catalytic oxidation performance in the selective oxidation system composed of hydrogen peroxide, and the by-product is only water, which is an environmentally friendly catalyst. It has a wide range of application markets and broad development prospects. [0003] At present, there are three main synthesis methods of TS-1 ...

Claims

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Application Information

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IPC IPC(8): C01B39/08B01J29/89
CPCB01J29/89C01B39/085C01P2004/61
Inventor 郝子健倪志虎
Owner 淄博恒亿化工科技有限公司
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