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Preparation method for organic functional ordered mesoporous titanium oxide silicon molecular sieve

A technology of mesoporous titanium oxide and silicon molecular sieve, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of difficulty in hybridizing mesoporous silicon oxide molecular sieve, uneconomical synthesis, etc., and achieves high mesoscopic order and equipment requirements. Low, uniform distribution of organic functional groups

Inactive Publication Date: 2012-01-25
SHANGHAI NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the bridging of the organosilicon source makes the synthesis very uneconomical, and the hydrophobic organic groups lead to phase separation and disordered materials in the case of high organic content, especially when the silica framework contains heteroatoms such as titanium, iron, This phenomenon is more prominent when gallium etc.
Because the heteroatoms in the framework endow mesoporous silica with unique catalytic active centers, this type of material has broad application prospects in catalysis, adsorption, etc., but the synthesis of hybrid mesoporous silica with multifunctional and high organic group content Molecular sieves are very difficult

Method used

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  • Preparation method for organic functional ordered mesoporous titanium oxide silicon molecular sieve
  • Preparation method for organic functional ordered mesoporous titanium oxide silicon molecular sieve
  • Preparation method for organic functional ordered mesoporous titanium oxide silicon molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] a) Add 2.0g of surfactant-P123 into 30g of 1M hydrochloric acid aqueous solution, stir at 40°C until the surfactant is completely dissolved and the solution is clear;

[0031] b) Add 3.61mL of inorganic silicon source-tetraethyl orthosilicate (TEOS) dropwise at 40°C to the above solution, stir at 40°C for 30 minutes, then add 0.29mL of organic silicon source-1,2-bis( Triethoxysilane) ethane (BTESE), continue stirring for 1 to 2 hours;

[0032] c) Add 0.78mL of inorganic titanium source-TiCl drop by drop 3 , continue stirring at 40°C for 22 hours;

[0033] d) carrying out a hydrothermal reaction at 100° C. for 24 hours;

[0034] e) After cooling, a white powder is obtained after suction filtration, washing, and natural drying at room temperature;

[0035] f) Reflux extraction with ethanol solvent for 24 hours, cooling, suction filtration, washing, and drying to obtain: an organic functional ordered mesoporous titanium oxide silicon molecular sieve with a silicon-titan...

Embodiment 2

[0042] a) Add 2.0g of surfactant-P123 into 45g of 0.5M hydrochloric acid aqueous solution, and stir at 40°C until the surfactant is completely dissolved and the solution is clear;

[0043] b) First add 3.39mL of inorganic silicon source-orthoethyl silicate (TEOS) dropwise to the above solution at 40°C

[0044] solution, stirred at 40°C for 30 minutes, then added 0.28 mL of organosilicon source-1,2-bis(triethoxysilyl)ethane (BTESE), and continued to stir for 1 to 2 hours;

[0045] c) Add 1.0 mL of inorganic titanium source-TiCl drop by drop 3 , continue stirring at 40°C for 22 hours;

[0046] d) carrying out a hydrothermal reaction at 100° C. for 24 hours;

[0047] e) After cooling, a white powder is obtained after suction filtration, washing, and natural drying at room temperature;

[0048] f) Reflux extraction with ethanol solvent for 24 hours, cooling, suction filtration, washing, and drying to obtain: an organic functional ordered mesoporous titanium oxide silicon molecu...

Embodiment 3

[0053] a) Add 2.0g of surfactant-P123 into 45g of 0.5M hydrochloric acid aqueous solution, and stir at 40°C until the surfactant is completely dissolved and the solution is clear;

[0054] b) Add 3.35 mL of inorganic silicon source-tetraethyl orthosilicate (TEOS) dropwise at 40°C to the above solution, stir at 40°C for 30 minutes, then add 0.27mL of organic silicon source-1,2-bis( Triethoxysilane) ethane (BTESE), continue stirring for 1 to 2 hours;

[0055] c) Add 1.28mL of inorganic titanium source-TiCl drop by drop 3 , continue stirring at 40°C for 22 hours;

[0056] d) carrying out a hydrothermal reaction at 100° C. for 24 hours;

[0057] e) After cooling, a white powder is obtained after suction filtration, washing, and natural drying at room temperature;

[0058] f) Reflux extraction with ethanol solvent for 24 hours, cooling, suction filtration, washing, and drying to obtain: an organic functionalized ordered mesoporous titanium oxide silicon molecular sieve with a si...

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Abstract

The invention discloses a preparation method for an organic functional ordered mesoporous titanium oxide silicon molecular sieve. The method comprises the following steps: first, introducing a surfactant self-assembly system, adding an inorganic titanium source for self assembly on the basis of pre-hydrolysis of an inorganic silica source and an organic silica source, then by hydrothermal reaction, carrying out sucking filtration, washing and drying, and finally extracting and removing a surfactant by organic solvent backflow. The aperture of the molecular sieve prepared by the method is 3.0-9.0 nm, the pore volume is 0.3-1.5 cm3 / g, the specific area is 400-1015 m2 / g, and the space structure is a 2D hexagon structure (space group p6 mm). The molecular sieve has the advantages of high order, large specific area, uniform pore size, adjustable silicon and titanium molar ratio and uniform distribution of organic functional groups. In addition, the preparation method has the advantages of simple operation, wide source of raw materials, low equipment requirement, low preparation cost, and the like.

Description

technical field [0001] The invention relates to a method for preparing an organic functionalized ordered mesoporous titanium oxide silica molecular sieve, belonging to the technical field of mesoporous material preparation. Background technique [0002] Mesoporous molecular sieves are a research field that has developed rapidly in recent years. In 1992, Mobil Kresge and Beck first used alkyl quaternary ammonium salt cationic surfactants as structure-directing agents to synthesize new M41S series silica (aluminum)-based ordered media with adjustable pore diameters in the range of 1.5-10 nm. Molecular sieve. In 1998, Zhao Dongyuan and others used block copolymers as surfactants to successfully obtain SBA-15 with a pore size of 10-40nm, which has the characteristics of high degree of order and good stability. These achievements have attracted great attention from scientists in the field of molecular sieve research and even in the field of materials science. The micropores of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 万颖楚华琴赵东元
Owner SHANGHAI NORMAL UNIVERSITY
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