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A kind of preparation method of mesoporous silica spherical nanoparticles

A mesoporous silica and nanoparticle technology, applied in silica, silica, nanotechnology and other directions, can solve the problems of large pollution, harsh conditions, and large amount of triethanolamine, so as to save tedious steps and simplify operations. Steps, the effect of reducing the cost of synthesis

Inactive Publication Date: 2011-12-14
EAST CHINA NORMAL UNIV
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Problems solved by technology

The current main synthetic strategies for the synthesis of mesoporous silica nanoparticles (MSNs) include: using a single CTAB cationic surfactant (Angew. Chem. Int. Ed., 2002, 2151, 2317.), in the early stage of the reaction, through a large number of Diluted with water, the particle growth has been quenched, thus preparing mesoporous silica nanoparticles with a size of less than 100 nm, but the shape of the particles is irregular, and the size distribution is very inhomogeneous; through the improved St?ber method (J. Phys . Chem. B 2004, 108, 20122.), using ethanol as a co-surfactant of CTAB cationic surfactant can prepare highly monodisperse mesoporous SiO 2 nanoparticles, but often larger than 100 nm in size; Bein by using triethanolamine (TEAH 3 ) to replace inorganic bases to synthesize mesoporous nanoparticles with a size of less than 200 nm (Adv. Funct. Mater. 2007, 17, 605.), but triethanolamine (TEAH 3 ) is used in a large amount, and high-speed centrifugation is required to obtain the final particles; Kuroda recently reported a new synthesis strategy to prepare mesoporous SiO with a size smaller than 50nm 2 Nanoparticles, but the molar ratio of CTAB / TMOS is greater than 0.5, the cost of synthesis is extremely high and the surfactant can only be removed through a complicated dialysis process (Chem. Commu., 2009, 5094.); Chinese patent CN1923684A utilizes dodecyl Using sodium sarcosinate as a template and (3-aminopropyl)trimethoxysilane as a co-structure directing agent, SiO with uniform size and controllable size was synthesized. 2 Nanoparticles, but the cost of synthesis is relatively high; the synthesis strategy of mixed templates can also be used to synthesize highly monodisperse mesoporous nanoparticles, but the expensive price of surfactants limits its wide application (Chemical Journal of Chinese Universities, 2011, 32, 560.)
It can be seen from the above reports that the existing synthetic methods have disadvantages such as harsh conditions, high cost, heavy pollution, and unfavorable for large-scale production.

Method used

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  • A kind of preparation method of mesoporous silica spherical nanoparticles
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Examples

Experimental program
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Effect test

Embodiment 1

[0019] First, 2.74 g of cetyltrimethyl-p-toluenesulfonate (CTATos) was added to a solution containing 144 ml of deionized water, 0.04 g of sodium hydroxide (NaOH) and 14.92 g of triethanolamine (TEAH 3 ) in a beaker, stirred at 80°C for 1 hour until the solution became clear, then quickly added 20.83g of tetraethoxysilicate (TEOS) into the beaker, and continued to stir at 80°C for 2 hours to obtain a white precipitate. The molar composition of this mixture is SiO 2 :CTATos:TEAH 3 :NaOH:H 2 O = 1:0.06:1:0.01:80; the obtained mixture is directly suction filtered, washed, and dried to obtain mesoporous SiO 2 Nanoparticles, yield 95%, average particle size 60 nm. The method of high-temperature roasting or acid treatment can remove the surfactant in the channel in one step. The specific method is as follows: (1) 1.0g raw powder is directly roasted in a muffle furnace at 550°C for 6 hours; (2) 1.0g raw powder is mixed with 40ml 1M hydrochloric acid ethanol solution, stirred at r...

Embodiment 2

[0021] First, 2.74g of cetyltrimethyl-p-toluenesulfonate (CTATos) was added to a solution containing 144ml of deionized water, 14.92g of triethanolamine (TEAH 3 ) and 0.20g NaOH mixed solution, stirred at 80°C for 1 hour until the solution became clear, then quickly added 20.83g tetraethoxysilicate (TEOS) into the beaker, and continued to stir at 80°C for 2 hours , a white precipitate was obtained, and the molar composition of the mixture was SiO 2 :CTATos:TEAH 3 :NaOH:H 2 O = 1:0.06:1:0.05:80; the obtained mixture is directly suction filtered, washed and dried to obtain mesoporous SiO 2 Nanoparticles, yield 95%, average particle size 180 nm. Change NaOH to TEAH 3 The molar ratio of the mesoporous silica nanoparticles with different particle sizes can be obtained, and the higher the alkalinity, the larger the particle size.

Embodiment 3

[0023] First, 2.74 g of cetyltrimethyl-p-toluenesulfonate (CTATos) was added to a solution containing 144 ml of deionized water, 1.4 g of NaOH and 14.92 g of triethanolamine (TEAH 3 ) mixed solution in a beaker, 80 o Stir at C constant temperature for 1 hour until the solution becomes clear, then quickly add 20.83g tetraethoxysilicate (TEOS) into the beaker, 80 o C constant temperature continued to stir for 2 hours, a white precipitate was obtained, and the molar composition of the mixture was SiO 2 :CTATos:TEAH 3 :NaOH:H 2 O = 1:0.06: 1:0.35:80; the obtained mixture is directly suction filtered, washed and dried to obtain mesoporous SiO 2 Nanoparticles, yield 95%, average particle size 800 nm.

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Abstract

The invention discloses a preparation method of mesoporous spherical Sio2 nanoparticles. The template agent used in the method is cetyl trimethyl p-methyl benzene sulfonate, the alkali source used in the method is a binary mixture comprising organic micro-molecular amine and inorganic base, the silica source used in the method is tetra alkyl silicate ester, and the molar ratio of cetyl trimethyl p-methyl benzene sulfonate to organic base to inorganic base to water is 1 to 0.03-0.06 to 0.5-2 to 0.01-0.35 to 80-500. By regulating the molar ratio of organic base to inorganic base, the particle size can be effectively controlled within 50-1000 nm. Compared with the prior art, the method disclosed in the invention has the most significant advantages that using cetyl trimethyl p-methyl benzene sulfonate as the template molecule can greatly reduce the dosage of surfactant, and regulating the molar ratio of the diacidic base can effectively regulate the final particle size. The method has theadvantages of simple processing, short cycle, low cost, and good repeatability, and is an environmental friendly synthetic method.

Description

technical field [0001] The invention relates to a method for preparing nano-spherical mesoporous molecular sieves, in particular to a method for preparing silicon-based mesoporous molecular sieve nanoparticles whose particle size can be adjusted. Background technique [0002] Mesoporous silica nanomaterial is a new type of inorganic nanomaterial with high specific surface area, large pore volume, and controllable shape and size. In recent years, its application research in the fields of material science, biomedicine, environmental protection, and biosensor has attracted attention received widespread attention. The current main synthetic strategies for the synthesis of mesoporous silica nanoparticles (MSNs) include: using a single CTAB cationic surfactant (Angew. Chem. Int. Ed., 2002, 2151, 2317.), in the early stage of the reaction, through a large number of Diluted with water, the particle growth has been quenched, thus preparing mesoporous silica nanoparticles with a size...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y40/00
Inventor 张坤侯琼玮罗琛赵安琪
Owner EAST CHINA NORMAL UNIV
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