Method for preparing mesoporous silica spherical nanoparticles

A mesoporous silica and nanoparticle technology, applied in the direction of silica, silicon oxide, nanotechnology, etc., can solve the problems of unfavorable large-scale production, irregular particle shape, harsh conditions, etc., and achieve the convenience of macro-synthesis, The effect of uniform pore size and regular shape

Inactive Publication Date: 2017-11-24
EAST CHINA NORMAL UNIVERSITY
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  • Abstract
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Problems solved by technology

The current main synthetic strategies for the synthesis of small-sized 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, By diluting with a large amount of water, the particle growth has been quenched, thereby 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; by the improved Stöber 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 amount of water used is extremely high, the cost of synthesis is extremely high and the surfactant can only be removed through a complicat

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  • Method for preparing mesoporous silica spherical nanoparticles
  • Method for preparing mesoporous silica spherical nanoparticles

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0017] First, add 1.05g cetyltrimethylammonium bromide (CTAB) to 69.12ml deionized water, 6.2g sodium methoxide (CH 3 ONa), 0.238g triethanolamine (TEAH 3 In the beaker of ), stir at 80°C for 1 hour until the solution becomes clear, then add 10g of tetraethoxysilicate (TEOS) dropwise into the beaker, and continue to stir at 80°C for 2 hours to obtain a white precipitate. The molar composition of the mixture is SiO 2 :CTAB:TEAH 3 :H 2 O: CH 3 ONa = 1:0.06:0.026:80:0. 1; the obtained mixture is directly filtered, washed, and dried to obtain mesoporous SiO 2 Nano particles, the yield is 94%, and the average particle size is 31nm. The method of high temperature roasting or acid treatment can be used to remove the surfactant in the pores in one step. The specific methods are 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 in 40ml 1M In the hydrochloric acid ethanol solution, stirred at room temperature for 1 hour, f...

Embodiment 2

[0019] First, 1.05g cetyltrimethylpara-methylammonium bromide (CTAB) was added to 69.12ml deionized water, 0.123g sodium methoxide, 2.38g triethanolamine (TEAH 3 In the beaker of ), stir at 80°C for 1 hour until the solution becomes clear, then add 10g of tetraethoxysilicate (TEOS) dropwise into the beaker, and continue to stir at 80°C for 2 hours to obtain a white precipitate. The molar composition of the mixture is SiO 2 :CTAB:TEAH 3 :H 2 O: CH 3 ONa = 1:0.06:0. 26:80:0.002; the obtained mixture is directly filtered, washed, and dried to obtain mesoporous SiO 2 Nano particles, the yield is 95%, and the average particle size is 42nm. Change CH 3 With the molar ratio of ONa, mesoporous silica nanoparticles of different particle sizes can be obtained.

Embodiment 3

[0021] First, add 1.05g cetyltrimethyl-p-methylammonium bromide (CTAB) to 248.83ml deionized water, 0.123g sodium methoxide, 0.238g triethanolamine (TEAH 3 In the beaker of ), stir at 80°C for 1 hour until the solution becomes clear, then add 10g of tetraethoxysilicate (TEOS) dropwise into the beaker, and continue to stir at 80°C for 2 hours to obtain a white precipitate. The molar composition of the mixture is SiO 2 :CTAB:TEAH 3 :H 2 O: CH 3 ONa = 1:0.06:0.026:288:0.002; the obtained mixture is directly filtered, washed, and dried to obtain mesoporous SiO 2 Nano particles, the yield is 95%, and the average particle size is 25 nm. Increasing the water ratio and the amount of sodium methoxide can also reduce the particle size.

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Abstract

The invention discloses a method for preparing mesoporous silica spherical nanoparticles. According to the method, the used template agent refers to cetyl trimethyl ammonium bromide, the alkali source refers to an organic small molecule amine, the silicon source refers to tetraethyl orthosilicate (TEOS), and the organic alcohol salt serves as a promoter. According to the molar composition of the raw materials, a ratio of the silicon source to the cetyl trimethyl ammonium bromide to organic alkali to sodium methylate to water is (1):(0.03-00.06):(0.5-2):(0.001-0.5):(80-500). Accurate synthesis in the particle size range of 25-50nm is realized by regulating the amount of the organic alcohol salt and regulating the nucleation rate of particles. Compared with the prior art, the method disclosed by the invention has the most significant advantage that the hydrolysis and condensation rate of the silicon source is promoted by taking the organic alcohol salt with high nucleophilicity as the promoter. Therefore, the silicon source is subjected to burst nucleation in a very short time, so that the small-size mesoporous silica spherical nanoparticles are prepared. The synthetic method disclosed by the invention is simple, short in cycle, low in cost and high in repeatability and is an environment-friendly green synthetic method.

Description

Technical field [0001] The invention relates to a preparation method of nano spherical mesoporous molecular sieve, in particular to a preparation method of silicon-based mesoporous molecular sieve nano particles with a particle size of 50 nm. Background technique [0002] Mesoporous silica nanomaterial is a new type of inorganic nanomaterial with high specific surface area, large pore volume, morphology and size controllable. In recent years, its application research in the fields of materials science, biomedicine, environmental protection, and biosensors has caused Received widespread attention. On the one hand, due to its low toxicity and easy elimination, it has become more and more widely used in drug slow-release and biological applications; on the other hand, in the use of solar energy, it has a smaller refractive index and more pores. , Is a good anti-reflective (AR) material; but both of these applications require its size to be below 50nm, so the macro-quantitative and ...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y40/00
CPCC01B33/12C01P2004/03C01P2004/04C01P2004/32C01P2004/64C01P2006/12C01P2006/14C01P2006/16
Inventor 张坤刘鹏程宁田雨单冰倩聂梦真彭博宗玉欣
Owner EAST CHINA NORMAL UNIVERSITY
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