Method for synthesizing ordered mesoporous titanium oxide molecular sieve

A technology of mesoporous titanium oxide and synthesis method, applied in the direction of molecular sieve characteristic aluminum phosphate, crystalline aluminosilicate zeolite, etc., can solve the problems of difficult matching, inability to form an ordered mesoscopic structure, and fast hydrolysis speed of titanium source.

Inactive Publication Date: 2008-10-01
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the problem is that the hydrolysis rate of the titanium source is too fast, it is difficult to match the hydrolysis rate of the silicon source, resulting in the production of titanium oxide
This phenomenon is more likely to occur when the titanium content is higher, so that the ordered mesostructure cannot be formed

Method used

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  • Method for synthesizing ordered mesoporous titanium oxide molecular sieve
  • Method for synthesizing ordered mesoporous titanium oxide molecular sieve
  • Method for synthesizing ordered mesoporous titanium oxide molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Preparation of mesoporous titanium oxide silicon molecular sieve with Si / Ti molar ratio of 20.

[0029] Step 1: At 40°C, mix 2.0g P123, 30g 1M hydrochloric acid, 15g H 2 O mixed, stirred at 40°C until all surfactants were dissolved, then added 4.23mL TEOS and continued to stir for 4 hours.

[0030] Step 2: Stir 8.0 mL of isopropanol, 0.043 mL of titanium tetrachloride, and 0.204 mL of n-butyl titanate at 40° C. for 2 hours. The solution described in mixing step 1 was continued to stir at the same temperature for 20 hours. The obtained mixed solution was transferred to an oven at 80° C. to volatilize for 2 hours, then transferred to a polytetrafluoroethylene hydrothermal kettle, and reacted hydrothermally in an oven at 100° C. for 1 day. After cooling, white powder was obtained after suction filtration, washing and natural drying at room temperature.

[0031] Step 3: Calcining 1.5 g of the sample without removing the surfactant at 450° C. for 8 hours in the...

Embodiment 2

[0033]Example 2: Preparation of mesoporous titania silica molecular sieve with Si / Ti molar ratio of 12.5.

[0034] Step 1: At 20°C, mix 2.0g P123, 30g 1M hydrochloric acid, 15g H 2 O mixed, stirred at 20°C until all surfactants were dissolved, then added 4.04mL TEOS and continued to stir for 4 hours.

[0035] Step 2: Stir 8.0 mL of isopropanol, 0.070 mL of titanium tetrachloride, and 0.310 mL of n-butyl titanate at 20° C. for 2 hours. The solution described in mixing step 1 was continued to stir at the same temperature for 28 hours. Transfer the obtained mixed solution to a 70°C oven to volatilize for 4 hours, then transfer it to a polytetrafluoroethylene hydrothermal kettle, and conduct a hydrothermal reaction in a 100°C oven for 1 day. A white powder was obtained after drying.

[0036] Step 3: Calcining 1.5 g of the sample without removing the surfactant at 350° C. for 15 hours in the air, and the obtained white powder is the product.

[0037] The product is a two-dimens...

Embodiment 3

[0038] Example 3: Preparation of a titania-silicon molecular sieve with a Si / Ti molar ratio of 10.

[0039] Step 1: At 30°C, mix 2.0g P123, 30g 1M hydrochloric acid, 15g H 2 O mixed, stirred at 40°C until all surfactants were dissolved, then added 4.00 mL TEOS and continued to stir for 3 hours.

[0040] Step 2: Stir 8.0 mL of isopropanol, 0.090 mL of titanium tetrachloride, and 0.410 mL of n-butyl titanate at 30° C. for 2 hours. The solution described in mixing step 1 was continued to stir at the same temperature for 40 hours. Transfer the obtained mixed solution to an oven at 80°C to volatilize for 2 hours, then transfer it to a polytetrafluoroethylene hydrothermal kettle, and react hydrothermally in an oven at 100°C for 1 day. A white powder was obtained after drying.

[0041] Step 3: Calcining 1.5 g of the sample without removing the surfactant at 550° C. for 10 hours in the air, and the obtained white powder is the product.

[0042] The product is a two-dimensional hex...

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Abstract

The invention pertains to the technical filed of the preparation of mesoporous materials and more particularly relates to a method for synthesizing an ordered mesoporous titanium oxide-silicon molecular sieve. The synthesis method of the invention comprises the procedures that a mixed titanium source is pre-hydrolysed in an organic solvent to form the precursor of the titanium source; the precursor is then mixed with a silicon source and a nonionic surfactant for carrying out organic-inorganic self-assembly in an aqueous solution. The inorganic titanium source and the silicon source are treated with cross-bridging and polymerization around the surfactant so as to obtain the composite material of silicon oxide molecular sieves containing titanium and the nonionic surfactant; the surfactant is removed by counter-current extraction with solvent or roasting in air so as to obtain the ordered mesoporous titanium oxide-silicon molecular sieves. The prepared material has high specific area (700-1600m<2>/g), large pore volume (0.5-1.5cm<3>/g) and uniform pore diameter (4.0-8.0nm) and has a two-dimensional hexagonal mesoscopic structure or a three-dimensional cubic mesoscopic structure. Compared with the traditional method for preparing the titanium oxide-silicon molecular sieves, the synthesis method of the invention has the advantages of simple operation, low material cost and low requirement for facilities, etc.

Description

technical field [0001] The invention belongs to the technical field of preparation of mesoporous materials, and in particular relates to a method for synthesizing ordered mesoporous titanium oxide silicon molecular sieves. Background technique [0002] Epoxy compounds (such as propylene oxide, octene oxide, epichlorohydrin, styrene oxide) are important intermediates in organic synthesis, widely used in petrochemical, fine chemical, organic synthesis, pharmaceuticals, spices and electronics Industry plays an important role in the national economy. The discovery of the Shell Petroleum Company catalyst in 1970 and the TS-1 molecular sieve catalyst in 1980 is considered to be an important catalyst for catalyzing the epoxidation reaction. TS-1 zeolite molecular sieve can use low-concentration hydrogen peroxide as oxygen source to selectively catalyze the epoxidation reaction of olefins, and the by-product is water. This reaction is considered to be a representative of atom-econ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B37/06
Inventor 万颖楚华琴赵东元
Owner FUDAN UNIV
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