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Method for preparing modification functional groups on external surfaces of pores of mesoporous silica material

A technology of functional groups and outer surfaces, which is applied in the field of mesoporous silica materials, can solve the problems of affecting selective adsorption capacity and adsorption capacity, affecting material screening capacity, and hindering adsorption, so as to improve screening capacity and adsorption Improvement of action and reduction of clogging effect

Inactive Publication Date: 2011-08-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, mesoporous materials also have certain problems in selective extraction: although the pore size can strictly limit the entry of large proteins into the pores, molecules with a molecular size larger than the pore size can still be adsorbed on the outer surface of the pores, which are often mistaken for adsorption in the pores. , and the larger protein adsorbed on the outer surface hinders the adsorption of the smaller target protein by the mesopore, which affects the sieving ability of the material, thereby affecting the selective adsorption capacity and adsorption capacity.

Method used

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  • Method for preparing modification functional groups on external surfaces of pores of mesoporous silica material
  • Method for preparing modification functional groups on external surfaces of pores of mesoporous silica material
  • Method for preparing modification functional groups on external surfaces of pores of mesoporous silica material

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Embodiment 1

[0025] 1) Preparation of mesoporous silica powder containing pore-forming agent:

[0026] After mixing the above raw materials with cetyltrimethylammonium bromide, tetraethoxysilane, ammonia water, sodium hydroxide, and water in a molar ratio of 0.1:1.0:3.2:0.3:80, stir at room temperature for 3 hours Finally, the mixture was transferred to a polytetrafluoro reactor for crystallization at 100° C. for 120 hours, then filtered, washed, and dried. (Chu, C.T-W., ect, J. Am. Chem. Soc., 114(1992) 10834.)

[0027] 2) The step of modifying the material includes: drying 1.0 g of mesoporous MCM-41 silica powder containing cetyltrimethylammonium bromide in vacuum at 100° C. for 10 hours. Add the dried material containing the pore-forming agent into a round bottom flask, and add 50mL of dry toluene to the flask under nitrogen protection. After the material is completely dispersed in toluene, add 3mL of 3-(2,3-glycidyloxypropoxy ) Propyltrimethoxysilane, reflux reaction at 110° C. for 2...

Embodiment 2

[0031] 1) Preparation of mesoporous silica powder containing pore-forming agent:

[0032] After mixing the above raw materials with cetyltrimethylammonium bromide, tetraethoxysilane, ammonia water, sodium hydroxide, and water in a molar ratio of 0.1:1.0:3.2:0.3:80, stir at room temperature for 3 hours Finally, the mixture was transferred to a polytetrafluoro reactor for crystallization at 100° C. for 120 hours, then filtered, washed, and dried. (Chu, C.T-W., ect, J. Am. Chem. Soc., 114(1992) 10834.)

[0033] 2) The step of modifying the material includes: drying 2.0 g of mesoporous MCM-41 silica powder containing cetyltrimethylammonium bromide in vacuum at 80° C. for 16 hours. Add the dried material containing the pore-forming agent into a round-bottomed flask, and add 100 mL of dry n-hexane into the flask under nitrogen protection. After the material is completely dispersed in n-hexane, add 6 mL of 3-(2,3-epoxy Propoxy)propyltrimethoxysilane was refluxed at 60° C. for 24 ho...

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Abstract

The invention relates to a method for preparing modification functional groups on the external surfaces of pores of a mesoporous silica material. The method comprises two steps of modifying the material and removing a hole-forming agent. The mesoporous silica material containing the hole-forming agent is reacted with organic siloxane with the functional groups in a dry inert organic solvent, and the reaction is carried out under the protection of nitrogen. Products after reaction are extracted by adopting acidified alcohol, the hole-forming agent is removed, and 3-(2,3-epoxypropoxy)propyl is simultaneously transformed into alkyl diol. The material can improve the screening capacity to proteins or peptides, greatly reduce the interferences of a high molecular weight biological matrix during the pre-treatment process of a sample and be applicable to selective enrichment to small molecule drugs and small peptides in the complex biological matrix.

Description

technical field [0001] The invention relates to a mesoporous silicon dioxide material, in particular to a preparation method for modifying functional groups on the outer surface of the pores of the mesoporous silicon dioxide material. Background technique [0002] Mesoporous materials have large specific surface area and pore volume, uniform pore size and can be continuously adjusted from one dimension to three dimensions on the nanometer scale, making them incomparable to traditional adsorbents in the adsorption and separation of macromolecules or macroions. Compared with superiority and broad application prospects. 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, mesoporous...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/10B01J20/30
Inventor 关亚风祁艳霞王华朱道乾
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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