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A kind of spherical ordered mesoporous silica and its preparation method

A mesoporous silica and grade technology, applied in the field of mesoporous materials, can solve the problems of difficult control, irregular particles, and low hydrothermal stability of the structure, and achieve the effect of simple preparation process and simple and direct method

Active Publication Date: 2017-06-20
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is currently used to prepare grades of mesoporous SiO 2 However, there are still the following problems: (1) the mesopores are disordered, resulting in low hydrothermal stability of the structure and a wide pore size distribution; (2) the particle morphology is irregular, which limits its performance in chromatographic separation and pharmaceutical Application in support; (3) The control of the secondary macroporous structure of the hierarchical structure depends heavily on various preparation conditions, and the control is difficult, and the pore size does not exceed 33nm

Method used

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  • A kind of spherical ordered mesoporous silica and its preparation method
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  • A kind of spherical ordered mesoporous silica and its preparation method

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Embodiment 1

[0036] Spherical ordered graded mesoporous silica, which is a kind of graded mesoporous SiO with coil structure 2 , the wires of the coils have the first-order pore structure, and the second-order pores exist between the wires, the average width of the wires is 25nm, the first-order mesopores are arranged in an orderly structure, and the The average pore diameter is 9.4nm, the average pore diameter of the secondary pores is 33.7nm, and the average particle diameter of silica is 2.3μm.

[0037] The preparation method of spherical ordered grade mesoporous silica specifically comprises the following steps:

[0038] step 1:

[0039] (1) preparation 80g mass fraction is the clear aqueous solution of P123 surfactant of 2.5%, wherein, the molecular weight of P123 is 5800;

[0040] (2) adding 11.5g concentration is the concentrated hydrochloric acid of 37%;

[0041] (3) Place in a water bath, the temperature of the water bath is 36°C, stir and mix evenly to obtain a mixed solution; ...

Embodiment 2

[0050] Spherical ordered graded mesoporous silica, which is a kind of graded mesoporous SiO with coil structure 2 , the lines of the coils have the first-order pore structure, and the second-order pores exist between the lines. The average width of the lines is 56nm. The first-order mesopores are arranged in an orderly structure, and the first-order mesopores The average pore diameter is 8.8nm, the average pore diameter of the secondary pores is 128nm, and the average particle diameter of silicon dioxide is 3.0μm.

[0051] The preparation method of spherical ordered grade mesoporous silica specifically comprises the following steps:

[0052] step 1:

[0053] (1) preparation 80g mass fraction is the clear aqueous solution of P123 surfactant of 2.5%, wherein, the molecular weight of P123 is 5800;

[0054] (2) adding 11.5g concentration is the concentrated hydrochloric acid of 37%;

[0055] (3) Place in a water bath, the temperature of the water bath is 31°C, stir and mix even...

Embodiment 3

[0064] Spherical ordered graded mesoporous silica, which is a kind of graded mesoporous SiO with coil structure 2 , the lines of the coils have the first-order pore structure, and the second-order pores exist between the lines. The average width of the lines is 40nm. The first-order mesopores are arranged in an orderly structure, and the first-order mesopores The average pore diameter is 8.9nm, the average pore diameter of the secondary pores is 78.4nm, and the average particle diameter of silica is 3.1μm.

[0065] The preparation method of spherical ordered grade mesoporous silica specifically comprises the following steps:

[0066] step 1:

[0067] (1) preparation 80g mass fraction is the clear aqueous solution of P123 surfactant of 2.5%, wherein, the molecular weight of P123 is 5800;

[0068] (2) adding 11.5g concentration is the concentrated hydrochloric acid of 37%;

[0069] (3) Place in a water bath, the temperature of the water bath is 36°C, stir and mix evenly to ob...

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Abstract

A kind of spherical ordered graded mesoporous silica and its preparation method, belonging to the technical field of mesoporous materials. The silica is a hierarchical mesoporous SiO2 with a coil-like structure. The lines of the coil have a first-level pore structure, and the second-level pores exist between the lines. The first-level mesopores have an ordered structure. Arrange; the preparation method is: (1) Prepare a clear aqueous solution of P123, add concentrated hydrochloric acid, place it in a water bath, and stir evenly; (2) Add the first part of TEOS to the mixed solution, stir, and then add the second part of TEOS and stir; (3) Transfer the mixed liquid into a polytetrafluoroethylene reaction bottle, place it in an autoclave, undergo hydrothermal treatment, filter, wash, dry and roast the precipitate to obtain spherical ordered graded mesoporous silica. The preparation system of the present invention itself is relatively simple and only involves the use of a soft film plate and does not involve the use of other organic or inorganic additives; it realizes the control of the pore diameter and pore wall of the second-level hole.

Description

technical field [0001] The invention belongs to the technical field of mesoporous materials, and in particular relates to a spherical ordered grade mesoporous silica and a preparation method thereof. Background technique [0002] Since 1992, Mobil scientists have successfully synthesized a novel M41S mesoporous molecular sieve using alkyl quaternary ammonium cationic surfactants as templates [C.T.Kresge, M.E.Leonowicz, W.J.Roth, J.C.Vartuli and J.S.Beck, Nature , 1992, 359, 710], which set off an upsurge of research on mesoporous materials in the scientific community. Due to its ordered mesoscopic structure, high specific surface area and large pore volume, mesoporous materials have great application prospects in adsorption, catalysis, and separation. In order to better adapt to the ever-growing demand for the application of ordered mesoporous materials, it has become an important task for researchers to control a series of physical and chemical properties such as the struc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12
CPCC01B33/12C01P2004/03C01P2004/32C01P2004/61
Inventor 王伟
Owner NORTHEASTERN UNIV LIAONING
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