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Preparation method of surface amino-modified mesoporous molecular sieve

A mesoporous molecular sieve and amino modification technology, applied in the field of mesoporous materials, can solve the problems of preventing Si-OH amino modification, low functionalization amount, low mesopore order, etc., and achieve the effect of uniform pore size distribution.

Inactive Publication Date: 2013-11-27
LIAONING UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The co-hydrolysis polycondensation method is to directly add amino-containing organosiloxanes to the system for preparing mesoporous molecular sieves, and obtain surface amino-modified mesoporous molecular sieves through co-hydrolysis polycondensation of silicon sources. However, the mesoporous molecular sieves obtained by this method The mesopore order of molecular sieves is not high, and the amount of functionalization is low
The post-grafting method is to modify the surface of mesoporous molecular sieves by reacting Si-OH on the surface of molecular sieves with amino-containing organosiloxanes, but this method first introduces -NH 2 Easily form hydrogen bonds with Si-OH, thereby preventing further amino modification of Si-OH

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take 3 g m-benzylidene diisocyanate (XDI) and evenly disperse in 14 g toluene to obtain solution A. Disperse 6 g of ethylenediamine (EDA) in 5 g of ether to obtain solution B. Add 1.5 g of silicon-based SBA-15 mesoporous molecular sieves to solution A, stir at 40°C for 3 h, filter to obtain a white solid, and perform Soxhlet extraction on the obtained solid with dichloromethane for 12 h, then vacuum-dry at 50°C to obtain a white powder. Take 1 g of the dry white powder and add it to solution B, stir at room temperature for 5 hours, filter, and dry at 40°C to obtain a surface amino-modified SBA-15 mesoporous molecular sieve material.

Embodiment 2

[0018] Take 10 g m-benzylidene diisocyanate (XDI) and evenly disperse in 30 g toluene to obtain solution A. Disperse 10 g of ethylenediamine (EDA) in 20 g of ether to obtain solution B. Add 2 g of silicon-based SBA-15 mesoporous molecular sieves to solution A, stir at 60°C for 12 h, then filter to obtain a white solid, perform Soxhlet extraction on the obtained solid with dichloromethane for 24 h, and vacuum-dry at 40°C to obtain a white solid powder. Take 4 g of the dry white powder and add it to solution B, stir at room temperature for 48 hours, filter, and dry at 50°C to obtain a surface amino-modified SBA-15 mesoporous molecular sieve material.

Embodiment 3

[0020] Take 15 g of 1,6-hexamethylene diisocyanate (HMDI) and uniformly disperse in 35 g of toluene to obtain solution A. Disperse 25 g of ethylenediamine (EDA) in 15 g of ether to obtain solution B. Add 3 g of silicon-based MCM-41 mesoporous molecular sieves to solution A, stir at 60°C for 10 h, filter to obtain a white solid, and perform Soxhlet extraction on the obtained solid with dichloromethane for 60 h, then vacuum-dry at 60°C to obtain a white powder. Take 2 g of the dry white powder and add it to solution B, stir at room temperature for 10 h, filter, and dry at 60° C. to obtain the surface amino-modified MCM-41 mesoporous molecular sieve material.

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PUM

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Abstract

The invention relates to a preparation method of a surface amino-modified mesoporous molecular sieve, which comprises the following steps: by using diisocyanate molecules as a bridge, grafting the diisocyanate molecules through the reaction of Si-OH on the silicon dioxide molecular sieve surface and one uramido group in the diisocyanate diisocyanate, and grafting the amino group through the reaction of the other uramido group of the diisocyanate and one amino group in the ethylene diamine molecule, thereby finally obtaining the surface amino-modified mesoporous molecular sieve material. The preparation process can not damage the mesoporous orderliness of the molecular sieve, the pore sizes are uniformly distributed, and thus, the mesoporous molecular sieve can be used in the fields of catalysis, adsorption, separation and the like.

Description

technical field [0001] The invention relates to a method for preparing a surface amino-modified mesoporous molecular sieve, which belongs to the field of mesoporous materials. Background technique [0002] In 1992, the researchers of Mobile Company reported the M41S series mesoporous materials with high specific surface area and high order for the first time [Natrue, 1992, 359, 710]. Mesoporous molecular sieve materials with different pore structures and pore sizes, such as MCM-41, MCM-48, HMS, MSU-X, SBA-15, SBA-16, MAS-7 and other mesoporous molecular sieves with different surface texture properties . In recent years, the surface organic functional modification of mesoporous molecular sieves has become an important research direction, such as sulfhydryl, carboxyl, sulfonic acid, amino and organic hydrophobic modification. As an important organic functional group, the amino group is favored because the amino group is easy to be positively charged and is a basic group. It ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 张丹李君华
Owner LIAONING UNIVERSITY OF TECHNOLOGY
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