Closed mesoporous silicon oxide and preparation method of same

A mesoporous silica, closed-cell technology, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve the problem of narrow selection of raw materials, incomplete closed-pore mesoporous silica is difficult to apply, and cannot hinder the entry of resin matrix. problems such as mesoporous silica channels, to achieve excellent comprehensive performance, high specific surface area, and good universality.

Inactive Publication Date: 2012-08-15
SUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above-mentioned incompletely closed-pore mesoporous silica is not easy to apply, and there are mainly the following two problems: (1) Since this incompletely closed-pore mesoporous silica is oxidized by the active groups of some materials and the original mesoporous It is formed by the chemical action of the silanol at the opening of the silicon hole, so the size of the material used for "closed cells" determines the degree of closed cells of mesoporous silica; if the size of the material used for "closed cells" is small, it does not Completely closed mesoporous silica cannot prevent the resin matrix from entering the pores of mesoporous silica; this means that the size of the material used for "closed pores" must increase as the pore size of mesoporous silica increases, and the range of raw material selection is narrow

Method used

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  • Closed mesoporous silicon oxide and preparation method of same
  • Closed mesoporous silicon oxide and preparation method of same
  • Closed mesoporous silicon oxide and preparation method of same

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 5 g of mesoporous silica SBA-15 was kept at 110° C. for 2 hours to obtain dry SBA-15. 150 ml of anhydrous toluene was added to dry SBA-15, stirred, and 10.75 g of dimethyldichlorosilane was slowly added dropwise at 40°C. After the dropwise addition, the reaction was carried out at 40°C for 6 hours. Anhydrous toluene and unreacted polychlorosilane were removed by vacuuming to obtain a white powder, which was washed twice with anhydrous toluene to obtain a crude product. The crude product was dried at 55°C for 7 hours to obtain mesoporous silica with chlorine groups on the surface. Its infrared spectrum and scanning electron microscope (SEM) are shown in the attached figure 1 , 2 shown.

[0026] Add 0.3 g of mesoporous silica containing chlorine groups on the surface to 30 ml of anhydrous acetone to form solution A; add 0.3 g of octapoly(tetramethylammonium) silicate to 10 ml of anhydrous methanol to form solution B . Solutions A and B were mixed and the mixture was...

Embodiment 2

[0041] 5 g of mesoporous silica SBA-15 was kept at 110° C. for 2 hours to obtain dry SBA-15. 150 ml of anhydrous toluene was added to dry SBA-15, stirred, and 10.75 g of dimethyldichlorosilane was slowly added dropwise at 40°C. After the dropwise addition, the reaction was carried out at 40°C for 6 hours. Anhydrous toluene and unreacted polychlorosilane were removed by vacuuming to obtain a white powder, which was washed twice with anhydrous toluene to obtain a crude product. The crude product was dried at 55°C for 7 hours to obtain mesoporous silica with chlorine groups on the surface.

[0042] Add 0.6g of mesoporous silica containing chlorine groups on the surface to 60ml of anhydrous acetone to form solution A; add 0.6g of octapoly(tetramethylammonium)silicate to 20ml of anhydrous methanol to form solution B . Solutions A and B were mixed and the mixture was sonicated at 40°C for 20 min to form solution C. Solution D was formed by adding 5.4 g of octapoly(tetramethylamm...

Embodiment 3

[0044] 5 g of mesoporous silica SBA-15 was kept at 120° C. for 3 hours to obtain dry SBA-15. 150ml of anhydrous toluene was added to dry SBA-15, stirred, and 13.63g of (chloromethyl)methyldichlorosilane was slowly added dropwise at 30°C. After the dropwise addition, the reaction was continued for 8 hours. After the reaction, anhydrous toluene and unreacted polychlorosilane were removed by vacuuming to obtain a white powder and water, which was washed twice with anhydrous toluene to obtain a crude product. The crude product was dried at 55°C for 7 hours to obtain mesoporous silica with chlorine groups on the surface.

[0045] Add 0.3 g of mesoporous silica containing chlorine groups on the surface to 40 ml of anhydrous acetone to form solution A; add 0.3 g of octapoly(tetramethylammonium) silicate to 20 ml of methanol-free solution to form solution B. Solutions A, B were mixed and sonicated at 30°C for 30 min to form solution C. Solution D was formed by adding 2.7 g of octap...

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Abstract

The invention discloses closed mesoporous silicon oxide and a preparation method of same. The preparation method comprises the steps of treating dry mesoporous silicon oxide with polychlorinated silane to prepare mesoporous silicon oxide containing chlorine groups on the surface; reacting the mesoporous silicon oxide containing the chlorine groups on the surface with polyhedral silsesquioxanes and polychlorinated silane to obtain a crude product; and after washing and drying, conducting calcination at the temperature of 230-300 DEG C, thereby obtaining the closed mesoporous silicon oxide. A coating layer is formed at the outer surface and the mesopores of the mesoporous silicon oxide by polyhedron silsesquioxane and mutual connection is realized through a Si-O bond or Si-N bond. The inner pores of the mesoporous silicon oxide are kept; besides, the mesopores of the mesoporous silicon oxide are closed by polyhedron silsesquioxane, and a larger specific surface area and more pores are obtained, so that the dielectric constant of the materials is lowered and the adsorptive property of the mesoporous silicon oxide is improved and the method provided by the invention ensures that the advantages of the mesoporous silicon oxide in preparing materials with low dielectric constant are brought into full play.

Description

technical field [0001] The invention relates to a mesoporous silica and a preparation method thereof, in particular to a mesoporous silica as a basic material, polyhedral silsesquioxane as a closed-cell material, polychlorosilane as a surface modifier and cross-linking agent It has a large specific surface area, contains a hydrophobic group, and completely closes the mesoporous silica through the interconnection of polyhedral silsesquioxane to form a coating layer. Background technique [0002] Low dielectric constant materials have broad application prospects in the field of microelectronics. One current method for preparing such materials is to introduce inorganic materials with a porous structure into the polymer, since the dielectric constant of air in the pores is 1, thereby reducing the dielectric constant of the polymer. Mesoporous silica is one of the materials with this structural feature, but the preparation of mesoporous silica for low-dielectric materials faces ...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/30
Inventor 梁国正单伟顾嫒娟袁莉
Owner SUZHOU UNIV
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