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Method for preparing mesoporous material with hydrophobic inner surface and hydrophilic outer surface

A mesoporous material and outer surface technology, applied in chemical instruments and methods, inorganic chemistry, other chemical processes, etc., to achieve the effect of simple method, improved analysis efficiency, improved screening ability and extraction efficiency

Inactive Publication Date: 2010-06-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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The method is simple and easy

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  • Method for preparing mesoporous material with hydrophobic inner surface and hydrophilic outer surface
  • Method for preparing mesoporous material with hydrophobic inner surface and hydrophilic outer surface
  • Method for preparing mesoporous material with hydrophobic inner surface and hydrophilic outer surface

Examples

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Embodiment 1

[0022] 1) Co-precipitation synthesis of materials:

[0023] Tetraethoxysilane: vinyltriethoxysilane: hexadecyltrimethylammonium bromide: sodium hydroxide: water is mixed in a molar ratio of 1:0.25:0.15:0.38:125, Hydrothermal reaction at 87°C for 2 days. After filtering, washing and drying the material. (References: Lim, M.H.; Blanford, C.F.; Stein, A.J. Am. Chem. Soc. 1997, 119, 4090.)

[0024] 2) External surface modification:

[0025] External surface modification: 1.0 g of the above-mentioned synthesized powder was vacuum-dried at 90°C for 12 hours, and the dried material containing the pore-forming agent was added to a round-bottomed flask, and 60 mL of dry toluene was added to the flask under nitrogen protection. After the material was completely dispersed in a dry organic solvent, 3mL of 3-(2,3-glycidoxy)propyltrimethoxysilane was added, and reacted at 100°C for 24 hours under the protection of nitrogen. After the reaction, the product was obtained by suction filtrat...

Embodiment 2

[0029] 1) Co-precipitation synthesis of materials:

[0030] Tetraethoxysilane: vinyltriethoxysilane: hexadecyltrimethylammonium bromide: sodium hydroxide: water is mixed in a molar ratio of 1:0.25:0.15:0.38:125, Hydrothermal reaction at 87°C for 2 days. After filtering, washing and drying the material. (References: Lim, M.H.; Blanford, C.F.; Stein, A.J. Am. Chem. Soc. 1997, 119, 4090.)

[0031] 2) External surface modification:

[0032] External surface modification: 2.0g of the above-mentioned synthesized powder was vacuum-dried at 80°C for 15 hours, the dried material containing the pore-forming agent was added to a round-bottomed flask, and 100mL of dry cyclohexane was added to the flask under nitrogen protection. After the material was completely dispersed in dry cyclohexane, 6 mL of 3-(2,3-epoxypropoxy)propyltrimethoxysilane was added, and reacted at 60°C for 24 hours under nitrogen protection. After the reaction, the product was obtained by suction filtration, washed...

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Abstract

The invention relates to a method for preparing mesoporous material with the hydrophobic inner surface and the hydrophilic outer surface, comprising the steps of coprecipitating and synthesizing the mesoporous material, modifying the outer surface of the mesoporous material and removing the pore-forming agent. Tetra-alkoxy silicane and siloxane containing hydrophobic functional groups are used as mixed silicon source, the mixed silicon source is hydrolyzed and synthesized into hydrophobic mesoporous material which contains pore forming agent under the alkaline condition, the hydrophobic mesoporous material reacts with the siloxane which contains or can generate the hydrophilic functional groups in methylbenzene under the protection of nitrogen, the products of reaction are extracted by acidified alcohol, and the pore-forming agent is removed. The mesoporous material with the hydrophobic inner surface and the hydrophilic outer surface can greatly reduce the interference of high molecular weight biological matrix in the process of pretreating the sample, improve the protein or peptide screening ability and highly elute and recover the small molecule protein or the small molecule peptide and is suitable for selectively extracting the medicament and the low molecular weight protein in the complex biological matrix.

Description

technical field [0001] The invention relates to a hybrid mesoporous material, in particular to a preparation method for modifying different organic functional groups on the inner and outer surfaces of the pores of the mesoporous silicon material. Background technique [0002] In recent years, there have been reports on the adsorption of drugs and biomolecules based on mesoporous materials, making mesoporous materials develop vigorously in the biological field. In particular, the strictly limited pore size of mesoporous materials is used to selectively extract target molecules that are smaller than the pore size. However, there are certain problems in the selective extraction of mesoporous materials: 1. Although the pore size can strictly limit the entry of large proteins into the pores, the outer surface of the pores can still adsorb molecules with a molecular size larger than the pore size, which are often mistaken for the molecules inside the pores. The adsorption of larg...

Claims

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Application Information

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IPC IPC(8): B01J20/10B01J20/283B01J20/30
Inventor 祁艳霞关亚风王华朱道乾卢烈娟
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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