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Method for preparing amino group or quaternary ammonium salt functional silicon dioxide mesoporous spherical material

A technology of silica and quaternary ammonium salts, which is applied in the field of preparation of metal adsorption technology, and can solve problems such as harsh reaction conditions and limited number of organic functional groups

Inactive Publication Date: 2010-06-16
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The obtained mesoporous materials contain a limited number of organic functional groups, and the reaction conditions are relatively harsh

Method used

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  • Method for preparing amino group or quaternary ammonium salt functional silicon dioxide mesoporous spherical material
  • Method for preparing amino group or quaternary ammonium salt functional silicon dioxide mesoporous spherical material
  • Method for preparing amino group or quaternary ammonium salt functional silicon dioxide mesoporous spherical material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 0.207g C 18 h 37 HOOCCH 2 CH 2 CH(NH 2 )COOH was dissolved in 21g of deionized water, then 0.3g of Brij56 was added, and 0.179g of 3-aminopropyltriethoxysilane and 1.5g of tetraethoxysilane were added to the aqueous solution of the surfactant under stirring at 80°C The system was stirred for 10min, left to react at 80°C for 48 hours, centrifuged to obtain solid matter, then washed with deionized water, freeze-dried for one day, weighed 0.5g mesoporous silica material, and dissolved in 200ml ethanolamine (17vol %) in an ethanol solution for 12 hours, centrifuged, and vacuum-dried at room temperature. , to obtain hollow spheres of silicon dioxide with organic template removed and amino functionalized.

[0032]The amino or quaternary ammonium salt functionalized silica mesoporous spherical material was characterized by transmission electron microscope, solid nuclear magnetic field, X-ray diffraction, scanning electron microscope and nitrogen adsorption instrument. fi...

Embodiment 2

[0034] 0.207g C 18 h 37 HOOCCH 2 CH 2 CH(NH 2 )COOH was dissolved in 21g of deionized water, then 0.1g of Brij56 was added, and 0.179g of 3-aminopropyltriethoxysilane and 1.1g of tetramethoxysilane were added to the aqueous solution of the surfactant under stirring at 80°C The system was stirred for 10min, left to react at 80°C for 48 hours, centrifuged to obtain solid matter, then washed with deionized water, freeze-dried for one day, weighed 0.5g mesoporous silica material, and dissolved in 200ml ethanolamine (17vol %) in an ethanol solution for 12 hours, centrifuged, and vacuum-dried at room temperature. , to obtain hollow spheres of silicon dioxide with organic template removed and amino functionalized.

[0035] The amino-functionalized silica mesoporous spherical material was characterized by X-ray diffraction, solid-state NMR, nitrogen adsorption and transmission electron microscopy. It is obtained that the average particle diameter of the silica hollow mesoporous ...

Embodiment 3

[0037] 0.207g C 18 h 37 HOOCCH 2 CH 2 CH(NH 2 )COOH was dissolved in 21g of deionized water, then 0.5g of Brij56 was added, and 0.179g of 3-aminopropyltriethoxysilane and 2.3g of tetrabutoxysilane were added to the aqueous solution of the surfactant under stirring at 80°C The system was stirred for 10min, left to react at 80°C for 48 hours, centrifuged to obtain solid matter, then washed with deionized water, freeze-dried for one day, weighed 0.5g mesoporous silica material, and dissolved in 200ml ethanolamine (17vol %) in an ethanol solution for 12 hours, centrifuged, and vacuum-dried at room temperature. , to obtain hollow spheres of silicon dioxide with organic template removed and amino functionalized.

[0038] The amino-functionalized silica mesoporous spherical material was characterized by X-ray diffraction, solid-state NMR, nitrogen adsorption and transmission electron microscopy. It is obtained that the average particle diameter of the silica hollow mesoporous s...

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Abstract

The invention relates to a method for preparing an amino group or quaternary ammonium salt functional silicon dioxide mesoporous spherical material in the technical field of metal adsorption. The silicon dioxide mesoporous spherical material is obtained by the following steps of: dissolving an anion surface active agent and a non-ionic surface active agent into deionized water; then adding ethanol into the deionized water, heating and stirring; sequentially adding siloxane and organic siloxane into the deionized water to prepare a silicon dioxide mixed solution; heating, standing and reacting the silicon dioxide mixed solution to obtain a silicon dioxide sediment; carrying out centrifugal drying on the obtained silicon dioxide sediment and removing the surface active agents by extraction processing. The steps are simple; by leading a co-structure-directing agent into a reaction system, the amido part of the co-structure-directing agent and the anion surface active agent are combined respectively by acid-base neutralization function and double-decomposition reaction, and the siloxane part and an inorganic source carry out copolycondensation to form a silicon wall, thereby the functional mesoporous silicon material containing an amino group or quaternary ammonium salt is synthesized.

Description

technical field [0001] The invention relates to a preparation method in the technical field of metal adsorption, in particular to a preparation method of an amino or quaternary ammonium salt functionalized silica mesoporous spherical material. Background technique [0002] Inorganic mesoporous materials have large specific surface area and pore volume, adjustable pore structure, adjustable pore size, surface properties that can be modified, and appearance that can be controlled; silica mesoporous modified with amino or quaternary ammonium salt functional groups Spherical materials have great application potential in catalytic reactions, wastewater treatment, immobilized enzymes, and heavy metal adsorbents. [0003] Found through literature retrieval to prior art, Lim M.H. etc. published the title " Comparative Studies of Grafting and Direct Syntheses of Inorganic-Organic Hybrid Mesoporous Materials " in " chemistry of materials " (Material Chemistry) 1999 the 11th phase 3285...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82B3/00
Inventor 车顺爱陈茜茹
Owner SHANGHAI JIAO TONG UNIV
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