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Process for synthesizing mesoporous SiO2 melecular sieve with cubic structure

A technology of mesoporous silica and synthesis method, which is applied in molecular sieves and base exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., and can solve problems such as failure to synthesize cubic molecular sieves

Inactive Publication Date: 2002-04-03
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cubic molecular sieve with the space group Fd3m, which is the last easy-to-appear cubic liquid crystal structure, has not been synthesized so far.

Method used

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  • Process for synthesizing mesoporous SiO2 melecular sieve with cubic structure
  • Process for synthesizing mesoporous SiO2 melecular sieve with cubic structure
  • Process for synthesizing mesoporous SiO2 melecular sieve with cubic structure

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Example 1, 3g CH 3 (CH 2 ) 16 CH 2 N + (CH 3 ) 2 CH 2 CH 2 N + (CH 3 ) 2 CH 2 CH 2 CH 2 N + (CH 3 ) 3 ·3Br - Dissolve in 120g water, add 48g 0.5MolL -1 Add 8g TEOS (tetraethyl orthosilicate) after stirring evenly, and the molar ratio of the three-head quaternary ammonium salt cationic surfactant, water, sodium hydroxide and tetraethyl orthosilicate is: 0.11: 241.6: 0.625 : 1. The reaction temperature was 18°C. After continuous stirring for 3 hours, the mixture was filtered, washed with deionized water until neutral, dried at room temperature and calcined at 500°C for 4 hours. The position of the diffraction peak 2θ was measured by XRD (X-ray diffraction), and the position index of the diffraction peak 2θ was confirmed to be an Fd3m cubic phase structure. The samples were observed with a TEM (transmission electron microscope). XRD spectrum and TEM photos see Figure 1-Figure 4 . The unit cell parameter of the product calculated according to the d ...

Embodiment 2

[0014] Example 2, 12g CH 3 (CH 2 ) 16 CH 2 N + (CH 3 ) 2 CH 2 CH 2 N + (CH 3 ) 2 CH 2 CH 2 CH 2 N + (CH 3 ) 3 ·3Br - Dissolve in 370g water, add 29g 0.5Mol L -1 After stirring evenly, add 20g TEOS (tetraethyl orthosilicate), and the molar ratio of three quaternary ammonium salt cationic surfactants, water, NaOH and TEOS is: 0.176:230:0.152:1.0. After continuous stirring for 3 hours, the mixture was filtered, washed with deionized water until neutral, dried at room temperature and calcined at 50°C for 3.5 hours. The position of the diffraction peak 2θ was measured by XRD (X-ray diffraction), and the position index of the diffraction peak 2θ was confirmed to be an Fd3m cubic phase structure. According to the d value on XRD, the unit cell parameter of the product is a=7.36nm, and the BET surface area is 901m 2 g -1 , BJH pore diameter is 2.4nm, pore volume is 1.03cm 3 .g -1 .

Embodiment 3

[0015] Example 3, at a synthesis temperature of 20°C, 2.485g CH 3 (CH 2 ) 16 CH 2 N + (CH 3 ) 2 CH 2 CH 2 N + (CH 3 ) 2 CH 2 CH 2 CH 2 N + (CH 3 ) 3 ·3Br - Dissolve in 1500g water, add 660g aqueous solution of 2.24g potassium hydroxide, stir evenly, add 83.3g TEOS. The molar ratio of the three-head quaternary ammonium salt cationic surfactant, water, KOH and TEOS is: 0.088:300:1.0:1.0. After continuous stirring for 3 hours, the mixture was filtered, washed with deionized water until neutral, dried at room temperature and calcined at 500°C for 4 hours. The position of the diffraction peak 2θ was measured by XRD (X-ray diffraction), and the position index of the diffraction peak 2θ was confirmed to be an Fd3m cubic phase structure. According to the d value on the XRD, the unit cell parameter of the product is a=7.73nm, and the BET surface area of ​​the product is 951m 2 g -1 , BJH pore diameter is 2.7nm, pore volume is 0.90cm 3 .g -1 .

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Abstract

A mesoporous SiO2 as molecular sieve with novel cubic structure is synthesized in alkaline condition by using tri-quaterrary ammonium salt cationic surfactant as structure guide agent. It has 3-D cubic structure (its space group is Fd3m), great specific surface area (about 1000 sq.m / g) and uniform pore diameter.

Description

technical field [0001] The invention belongs to the technical field of inorganic molecular sieves, in particular to a synthesis method of a novel cubic phase structure mesoporous silica molecular sieve whose space group is Fd3m. technical background [0002] Mesoporous molecular sieve materials refer to a class of inorganic porous materials with a pore size of 2-30 nm and a regular structure, which are self-assembled by sol-gel molecules of inorganic species under certain conditions using surfactants as supramolecular templates. Compared with traditional microporous molecular sieves, mesoporous molecular sieve materials have the characteristics of large and uniform pore size distribution, finely adjustable pore size, long-range order of pores, high specific surface area, relatively good thermal stability and hydrothermal stability, etc. received widespread attention. Taking advantage of its special properties, people have carried out extensive application research on it in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00C01B39/04
Inventor 沈绍典李裕琦孙锦玉屠波赵东元
Owner FUDAN UNIV
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