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Method for preparing mesoporous titanium silicate molecular sieve

A titanium-silicon molecular sieve and mesoporous technology, which is applied in the field of preparation of mesoporous molecular sieve catalytic materials, can solve the problems of titanium-silicon molecular sieves with great differences in catalytic performance, reduced catalytic reaction efficiency, poor product repeatability, etc., to achieve mild reaction conditions and synthetic raw materials The effect of easy availability, good selectivity and conversion

Inactive Publication Date: 2009-06-17
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is a relatively traditional synthesis method. Due to the harsh synthesis conditions, the repeatability of the product is very poor. Even if the same reagents and preparation methods are used, the catalytic performance of the titanium-silicon molecular sieve obtained is often very different.
And the synthesized mesoporous titanium-silicon molecular sieve is easy to lead to the formation of non-skeleton titanium, the existence of non-skeleton titanium can lead to the hydrolysis of hydrogen peroxide, reducing the catalytic reaction efficiency

Method used

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  • Method for preparing mesoporous titanium silicate molecular sieve
  • Method for preparing mesoporous titanium silicate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dodecyltrimethylammonium bromide is dissolved in deionized water to form a uniform solution with a mass percentage concentration of 0.7%, adding ammonia water to adjust the pH value of the solution to 10, and ethyl tetrasilicate is added to the solution (silicon source The molar ratio to dodecyltrimethylammonium bromide is 7), and magnetically stirred for 4h. The product was filtered, washed with deionized water, and dried at 30 °C. Calcined at 550°C for 6h to obtain white silica mesoporous molecular sieves (see figure 1 ).

[0021] Take silica mesoporous molecular sieve and add it to ethanol for dispersion (mass percentage concentration is 3%), dissolve tetraethyl titanate in ethanol (molar ratio of titanium / silicon is 0.15) and add to silica mesoporous molecular sieve ethanol In the solution, stirred and reacted at 30°C for 4h, the product was filtered, washed with ethanol to obtain a white powder, dried at 90°C, and calcined at 300°C for 6h to obtain a mesoporous t...

Embodiment 2

[0024] Dissolve cetyltrimethylammonium bromide in deionized water to form a uniform solution with a mass percent concentration of 0.7%, add ammonia water to adjust the pH value of the solution to 10, and mix ethyl orthosilicate and diphenyldimethoxy Add silane into the solution (the molar ratio of silicon source to hexadecyltrimethylammonium bromide is 7), and magnetically stir for 6h. The product was filtered, washed with deionized water, and dried at 30 °C. Calcined at 550°C for 6 hours to obtain white silica mesoporous molecular sieves.

[0025] Take silica mesoporous molecular sieve and add it to ethanol for dispersion (mass percentage concentration is 3%), dissolve tetraethyl titanate in ethanol (molar ratio of titanium / silicon is 0.15) and add to silica mesoporous molecular sieve ethanol In the solution, stirred and reacted at 30°C for 4h, the product was filtered, washed with ethanol to obtain a white powder, dried at 90°C, and calcined at 300°C for 6h to obtain a meso...

Embodiment 3

[0028] Hexadecyltrimethylammonium bromide is dissolved in deionized water to form a uniform solution with a mass percent concentration of 1.7%, adding ammonia water to adjust the pH value of the solution to 10, adding sodium orthosilicate to the solution (silicon source and ten The molar ratio of hexyltrimethylammonium bromide is 7), and magnetic stirring is carried out for 6h. The product was filtered, washed with deionized water, and dried at 30 °C. Calcined at 550°C for 6 hours to obtain white silica mesoporous molecular sieves.

[0029] Get silica mesoporous molecular sieve and join in ethanol and disperse (mass percent concentration is 3%), dissolve titanium trichloride in isopropanol (the molar ratio of titanium / silicon is 0.15) add to silica mesoporous molecular sieve In the ethanol solution, stirred and reacted at 30°C for 4h, the product was filtered, washed with ethanol to obtain a white powder, dried at 90°C, and calcined at 300°C for 6h to obtain a mesoporous tita...

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Abstract

The invention relates to a method for preparing mesoporous titanium silicon molecular sieves, which belongs to the technical field of preparation of mesoporous molecular sieve catalytic materials. The method comprises: adopting a cationic surfactant as a template agent, dispersing the cationic surfactant into deionized water, adding ammonia water to adjust the pH value of the solution, and adding silicon sources after the template agent is completely dissolved; making the materials undergo filtration, washing, drying and roasting, removing the organic template agent, and obtaining silicon dioxide mesoporous materials; and dispersing the obtained silicon dioxide mesoporous materials into ethanol, slowly adding titanium sources, loading titanium ions after hydrolysis of the titanium sources on the silicon dioxide mesoporous molecular sieves to form an active center, and obtaining titanium-loaded mesoporous molecular sieves. The reaction is easy to control, and the product has good repeatability and is suitable for mass production. By adoption of the prepared titanium silicon molecular sieves as a catalyst and hydrogen peroxide as an oxygen source to catalyze olefin epoxidation and alcohol oxidation, the reaction conditions are mild and the reaction has good selectivity and conversion rate.

Description

technical field [0001] The invention belongs to the technical field of preparation of mesoporous molecular sieve catalytic materials, and in particular relates to a preparation method of mesoporous titanium-silicon molecular sieve and its catalytic epoxidation application. Background technique [0002] Selective catalytic oxidation is an important synthetic method in the production fields of fine chemicals, agrochemicals and pharmaceutical intermediates. Using high-efficiency solid catalysts and using dilute aqueous hydrogen peroxide as an oxidant to realize new catalytic processes in these fields is more in line with the requirements of "green chemistry and chemical engineering". Therefore, the development of high-efficiency solid catalysts has become one of the primary issues and core technologies for realizing these green processes. [0003] Since Ti-MCM-41 was first synthesized by Corma et al. in 1994, the unique structure, large specific surface area and catalytic perf...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 王戈杨穆王莹莹
Owner UNIV OF SCI & TECH BEIJING
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