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Dual mesoporous silica microsphere and preparation method thereof

A silica and double mesoporous technology, applied in the field of mesoporous silica microspheres and preparation, can solve the problems of slow hydrolysis rate, high price, hinder the industrial application of mesoporous silica beads, etc., and achieve pore distribution. Good concentration and dispersion

Active Publication Date: 2016-03-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Because the organosilicon source used in the synthesis of mesoporous materials has the advantages of slow hydrolysis rate and easy control, it is widely used, but its high price hinders the industrial application of mesoporous silica spheres prepared from it to a certain extent.

Method used

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  • Dual mesoporous silica microsphere and preparation method thereof
  • Dual mesoporous silica microsphere and preparation method thereof
  • Dual mesoporous silica microsphere and preparation method thereof

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preparation example Construction

[0023] The preparation method of the dual mesoporous silica microspheres provided by the invention comprises the following steps:

[0024] (1) Prepare an acid solution with a concentration of 0.5 to 5.0 mol / L, add polyethylene glycol therein so that the concentration of polyethylene glycol is 0.001 to 1.0 mol / L,

[0025] (2) Add silicate to the mixed solution prepared in step (1), so that the concentration of silicate in the mixed solution is 0.01 to 5.0 mol / L, so that the silicate, polyethylene glycol, acid and water as SiO 2 : polyethylene glycol: acid: the molar ratio of water is 1: (0.012 ~ 0.04): (2 ~ 5): (100 ~ 150),

[0026] (3) After stirring the mixture obtained in step (2), place it in a crystallization reaction kettle, and crystallize it at 140-180° C. for 28-60 hours under autogenous pressure, and dry the solid product obtained after crystallization at 500- Baking at 800°C.

[0027] In the method of the present invention, an acid solution with a suitable concent...

example 1

[0037] Prepare 50 mL of sulfuric acid solution with a concentration of 2.0 mol / L, add 0.009 mol of polyethylene glycol (PEG) with a molecular weight of 6000, and then add 16 mL of water glass (modulus 3.15) with a concentration of 4.2 mol / L to make SiO in the solution 2 : polyethylene glycol : acid : H 2 The molar ratio of O is 1:0.014:3:100. After mixing evenly, the silica sol is placed in a crystallization kettle with a polytetrafluoroethylene liner and sealed, and is hydrothermally crystallized at 150°C for 30h. After solid-liquid separation, the solid was washed with water until the washing liquid was neutral. The filter cake was dried at 80°C for 24h and calcined at 550°C for 4h. The scanning electron microscope image of the obtained silica microsphere sample was as follows: figure 1 shown. Depend on figure 1 It can be seen that the obtained silica microspheres are uniformly dispersed and regular in shape.

[0038] The low-temperature nitrogen adsorption-desorption cu...

example 2

[0042] Prepare 100 mL of nitric acid solution with a concentration of 4.0 mol / L, add 0.009 mol of polyethylene glycol (PEG) with a molecular weight of 4000, and then add 16 mL of water glass (modulus 3.0) with a concentration of 4.2 mol / L to make SiO in the solution 2 : polyethylene glycol : acid : H 2 The molar ratio of O is 1:0.014:3:100. After mixing evenly, the silica sol is placed in a crystallization kettle with a polytetrafluoroethylene liner and sealed, and is hydrothermally crystallized at 160°C for 48h. After solid-liquid separation, the solid was washed with water until the washing liquid was neutral. The filter cake was dried at 80°C for 24h and calcined at 600°C for 4h, the obtained silica sample had figure 1 Spherical features are shown, and the microspheres are evenly dispersed. The low-temperature nitrogen-adsorption-desorption curve has figure 2 The characteristic H2-type adsorption isotherms shown indicate that it is a mesoporous material.

[0043] The s...

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Abstract

A dual mesoporous silica microsphere has the specific surface area of 300 m<2> / g to 600 m<2> / g, the pore volume ranges from 0.4 mL / g to 0.9 mL / g, the small pore diameter of the silica microsphere ranges from 2 nm to 4 nm, and the large pore diameter of the silica microsphere ranges from 6 nm to 10 nm. A preparation method of the dual mesoporous silica microsphere is simple, and the double-pore distribution silica microsphere can be obtained through a cheap silicon source and a single template by controlling reaction conditions.

Description

technical field [0001] The invention relates to a mesoporous silica microsphere and a preparation method thereof, in particular to a double mesoporous silica microsphere and a preparation method thereof. Background technique [0002] Dual mesoporous materials are a new type of porous materials developed on the basis of mesoporous molecular sieves in recent years. The material has two kinds of pore structures with different pore diameters. The large mesopores can allow molecules with larger diameters to enter, and at the same time serve as the transport channel of substances, which has small diffusion resistance and is conducive to mass transfer; the small mesopores provide large specific surface area and can As the adsorption point and reaction site of substances, it has good shape-selective catalytic ability. The characteristic of double mesoporous materials is conducive to improving the diffusion rate and the dispersion of carrier metals, so that it has great development ...

Claims

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Application Information

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IPC IPC(8): C01B33/12
Inventor 徐广通徐华
Owner CHINA PETROLEUM & CHEM CORP
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