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Mesoporous silica nanosphere with ultrahigh specific surface area and preparation method thereof

A mesoporous silica, ultra-high specific surface area technology, applied in the direction of silica, silicon oxide, nanotechnology, etc., can solve the problems of large particle diameter, difficult pore size and shape, particle agglomeration, etc., to achieve particle size Easy to control, short preparation time, good spherical effect

Pending Publication Date: 2021-03-09
SHIHEZI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hydrothermal method to obtain porous SiO 2 The specific surface area of ​​nanospheres is mostly less than 500m 3 / g, the preparation method of hydrothermal method is cumbersome, and reacts under the environment of high temperature and high pressure, its energy consumption is higher, and can not produce in batches continuously, this method is time-consuming and cost is slightly higher
Precipitation method, the method is simple, but the shape of silicon dioxide nanospheres is difficult to control, and the specific surface area of ​​the prepared silicon dioxide nanospheres is small, usually 300m 3 / g, and the particle size of the obtained silica nanospheres is large, the particle size distribution is wide, the precipitation process cannot be controlled, and the particle agglomeration is serious, which seriously restricts the product properties.
The silica nanospheres prepared by the gas phase method have high purity and simple process, but the specific surface area of ​​the silica nanospheres prepared by it is 200-400m 3 / g, the particle diameter and specific surface area are uncontrollable, so that the silica nanospheres still have the problem of large particle diameter and low specific surface area
Although the airgel method can prepare 500-900m 3 / g of mesoporous silica nanomaterials, but its shape is difficult to control into a spherical shape, and it is difficult to control the pore size and shape, that is, the higher the specific surface area, the less likely it is to form a spherical shape
Therefore, the nano-silica spheres prepared by the prior art cannot meet the application requirements of various industries at the present stage.

Method used

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  • Mesoporous silica nanosphere with ultrahigh specific surface area and preparation method thereof
  • Mesoporous silica nanosphere with ultrahigh specific surface area and preparation method thereof
  • Mesoporous silica nanosphere with ultrahigh specific surface area and preparation method thereof

Examples

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preparation example Construction

[0050] A method for preparing mesoporous silica nanospheres with an ultrahigh specific surface area, comprising the following steps:

[0051] (1) Preparation of precursor solution:

[0052] Dissolve ethyl orthosilicate in ethanol solution, and mix evenly with magnetic stirring to obtain precursor solution A;

[0053] Mix ammonia water, water and pore-forming agent uniformly to obtain precursor solution B;

[0054] (2) Equally draw the precursor solutions A and B, place them on a micro-injection pump, and mix them quickly through a microchannel reactor at the same injection speed to obtain a microemulsion;

[0055] (3) After the microemulsion is left to stand, it is subjected to demulsification, suction filtration, washing, drying, and high-temperature calcination to obtain the mesoporous silica nanospheres with ultra-high specific surface area.

[0056] Preferably, in the precursor solution A, the volume ratio of ethyl tetrasilicate to ethanol solution is 1-10:450;

[0057]...

Embodiment 1

[0067] The specific operation steps are as follows:

[0068] (1) Dissolve 5ml of ethyl orthosilicate in 450ml of ethanol solution (the volume ratio of ethanol to water in the ethanol solution is 1:1), stir and mix evenly to obtain the precursor A;

[0069] (2) After dissolving 4.10g of cetyltrimethylammonium bromide (CTAB) in 450ml of deionized water, quickly drop 15ml of ammonia water to obtain the precursor solution B;

[0070] (3) Take equal amounts of precursor solutions A and B, place them on a micro-injection pump, set the injection speed to 60ml / min, and mix quickly through a microchannel reactor to prepare a transparent microemulsion by mixing precursor solution A and precursor solution B system;

[0071] (4) After the microemulsion was allowed to stand for 20 minutes, add 100 ml of acetone, heat and reflux at 60° C. for 20 minutes to make the colloid coagulate and achieve the effect of breaking the emulsion, and then suction filter at room temperature;

[0072] Afte...

Embodiment 2

[0078] The operating steps of Example 2 are the same as those of Example 1, except that the amount of cetyltrimethylammonium bromide (CTAB) is 1.00 g.

[0079] The silicon dioxide nanosphere prepared in this embodiment is measured, and the specific surface area is 1322m 2 / g, the pore volume is 0.99cm 3 / g and an average pore diameter of 3nm ultra-high specific surface area mesoporous silica nanospheres.

[0080] Compared with Example 1, it can be seen that the amount of pore forming agent will affect the specific surface area.

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Abstract

The invention relates to a mesoporous silica nanosphere with an ultrahigh specific surface area and a preparation method of the mesoporous silica nanosphere. The preparation method of the mesoporous silica nanospheres with the ultrahigh specific surface area comprises the following steps: (1) dissolving tetraethoxysilane in an ethanol solution, and magnetically stirring and uniformly mixing to obtain a precursor solution A; and uniformly mixing ammonia water, water and a pore-forming agent to obtain a precursor solution B; (2) equivalently sucking the precursor solution A and the precursor solution B, placing the precursor solution A and the precursor solution B on a micro-injection pump, and quickly mixing the precursor solution A and the precursor solution B through a micro-channel reactor at the same injection speed to obtain a micro-emulsion; and (3) standing the micro-emulsion, carrying out water bath heating demulsification, carrying out suction filtration, drying, and carrying out high temperature calcination to obtain the mesoporous silica nanospheres. According to the preparation method disclosed by the invention, the mesoporous silica nanospheres with the specific surfacearea of about 700-1860m < 2 > / g can be rapidly and continuously prepared, the pelletizing effect is good, and the process time is short.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a mesoporous silica nanosphere with an ultrahigh specific surface area and a preparation method thereof. Background technique [0002] Silica nanosphere is an inorganic nanomaterial widely used at present. Due to its special surface effect, small size effect and macroscopic quantum tunneling, it has many unique physical and chemical properties, making it widely used. space. Due to the ultra-high specific surface area of ​​SiO 2 Nanospheres, with ultra-high specific surface area, rich pore volume and ordered mesopores, have a wider range of applications in the fields of catalysis, adsorption and pharmaceutical preparations. [0003] The particle size and specific surface area of ​​silica nanospheres are the key factors affecting its performance. The larger the specific surface area, the higher the activity, the better the affinity and reinforcem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y40/00
CPCC01B33/12B82Y40/00C01P2004/32C01P2006/12C01P2006/16C01P2004/03C01P2004/04C01P2002/72C01P2006/17
Inventor 于锋陈强
Owner SHIHEZI UNIVERSITY
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