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Spherical ordered graded mesoporous silicon dioxide and preparation method thereof

A mesoporous silica and grade technology, applied in the field of mesoporous materials, can solve the problems of difficult control, irregular particles, and the second-level macroporous structure depends on preparation conditions, and achieves the effect of simple and direct method and simple preparation process.

Active Publication Date: 2016-04-13
NORTHEASTERN UNIV
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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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  • Spherical ordered graded mesoporous silicon dioxide and preparation method thereof
  • Spherical ordered graded mesoporous silicon dioxide and preparation method thereof
  • Spherical ordered graded mesoporous silicon dioxide and preparation method thereof

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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

The invention provides spherical ordered graded mesoporous silicon dioxide and a preparation method thereof and belongs to the technical field of mesoporous materials. The silicon dioxide is graded mesoporous SiO2 with a clew-shaped structure; a wire of the clew has a first-grade pore structure and second-grade pores are formed between the wires; first-grade mesopores are arrayed in an ordered structure. The preparation method comprises the following steps: (1) preparing a P123 clarified water solution and adding concentrated hydrochloric acid; putting the mixture into a water bath and uniformly stirring; (2) adding the first part of TEOS (Tetraethyl Orthosilicate) into a mixed solution and stirring; then adding the second part of TEOS and stirring; (3) transferring the mixed solution into a polytetrafluoroethylene reaction bottle and putting the polytetrafluoroethylene reaction bottle into a high-pressure kettle; carrying out hydro-thermal treatment; filtering sediment, washing, drying and roasting to prepare the spherical ordered graded mesoporous silicon dioxide. A preparation system provided by the invention is relatively simple, only relates to utilization of a soft template, but does not relate to utilization of other organic or inorganic additives; pore diameters and pore walls of the second-grade pores are controlled.

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.Vartulian and J.S.Beck, Nature, 1992, 359, 710], since then set off an upsurge of research on mesoporous materials by people 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 s...

Claims

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Application Information

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