Nanometer hierarchical pore MFI molecular sieve one-step synthesis method

A microporous molecular sieve and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of high cost

Inactive Publication Date: 2009-12-30
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is simple and easy to implement, the surfactant used is laboratory-synthesized, which is special and expensive

Method used

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  • Nanometer hierarchical pore MFI molecular sieve one-step synthesis method
  • Nanometer hierarchical pore MFI molecular sieve one-step synthesis method

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preparation example Construction

[0005] The preparation method of the multi-level porous molecular sieve material of the present invention is characterized by the following steps: preparing a certain concentration of fluorocarbon surfactant and hydrocarbon surfactant solution. Under water bath conditions, tetrapropylammonium hydroxide was added. Maintain the temperature of the water bath, add silicon source, aluminum source or titanium source while vigorously stirring, and maintain for a certain period of time. The obtained sol is moved into a stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallized at a certain temperature for a period of time; the obtained solid is centrifuged, washed with deionized water, dried, and finally roasted to remove the template agent.

[0006] The characteristic of the mixed solution of the fluorocarbon surfactant and the hydrocarbon surfactant is that the molar ratio of the fluorocarbon surfactant to the hydrocarbon surfactant is 0.16-1.0, preferably ...

Embodiment 1

[0014] Dissolve 0.3 g of cetyltrimethylammonium bromide and 0.4 g of FSO-100 in deionized water. After a uniform solution was formed, 1.0ml of tetrapropylammonium hydroxide (mass percentage: 25%) was added, the temperature was raised to 35°C, 1.57g of sodium silicate was added, and vigorously stirred for 0.5h. The obtained sol was transferred into a stainless steel crystallization kettle and treated with hydrothermal treatment at 140°C for 5d. After centrifugation, the precipitate was dried overnight at 100°C, and then baked in a muffle furnace at 650°C for 6 hours to obtain the desired material. The specific surface area is 786m 2 / g, the total pore volume is: 0.68cm 3 / g, micropore area 173m 2 / g.

Embodiment 2

[0016] Dissolve 0.2 g of sodium dodecylbenzenesulfonate and 0.3 g of FC-4 in deionized water. After a uniform solution was formed, 4.0ml of tetrapropylammonium hydroxide (25% by mass) was added, the temperature was raised to 80°C, 1.108g of ethyl orthosilicate and 0.05g of tetrabutyl titanate were added, and vigorously stirred for 24h. The obtained sol was transferred into a stainless steel crystallization tank and treated with hydrothermal treatment at 180°C for 1d. After centrifugation, the precipitate was dried overnight at 100°C, and then baked in a muffle furnace at 650°C for 6 hours to obtain the desired material. The specific surface area is 897m 2 / g, the total pore volume is: 0.87cm 3 / g, micropore area 86m 2 / g.

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Abstract

The invention relates to a nanometer hierarchical pore MFI molecular sieve one-step synthesis method, belonging to the fields of catalytic chemistry, inorganic chemistry and physical chemistry; wherein, MFI molecular sieve can be Silicalite-1, ZSM-5 or TS-1, the specific surface is 400-1100m<2> / g and the total pore volume is 0.15-0.83 cm<3> / g. The preparation method is characterized in that commercial fluorocarbon / hydrocarbon surfactant is used as template agent of the mesoporous structure and the hierarchical pore MFI molecular sieve can be synthesized through one step reaction on the cooperative action between the commercial fluorocarbon / hydrocarbon surfactant and microporous molecular sieve template. The method is easy, the cost is low and the combination of mesoporous and microporous structures can be realized. The material not only has the characteristics of high activity and high hydrothermal stability of microporous molecular sieve, but also eliminates diffusion control, thus facilitating molecule reaction. The new material has wide application prospect in the fields of petrochemical engineering, chemical preparation, environmental catalysis and the like.

Description

technical field [0001] This patent relates to a method for directly preparing nanometer hierarchical porous MFI molecular sieves in one step. Background technique [0002] Microporous molecular sieves have high catalytic activity and hydrothermal stability, and are widely used in industrial fields such as petroleum cracking, hydrocracking, isomerization, reforming, and toluene disproportionation. Due to its uniform pore size, it plays a shape-selective catalytic role in the catalysis process for reactants and products, but its narrow pore size is not conducive to mass transfer of macromolecules, resulting in a decrease in conversion rate and activity. Mesoporous materials have the characteristics of large pore diameter, high specific surface area and ordered pore structure. Although it is beneficial to the adsorption and diffusion of macromolecules during the reaction process, the amorphous nature of the pore wall makes its catalytic activity and hydrothermal stability great...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/38
Inventor 王艳芹辜辛卢冠忠刘晓晖任家文郭耘郭杨龙张志刚龚学庆王筠松
Owner EAST CHINA UNIV OF SCI & TECH
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