Hollow silica nanosphere and preparing method thereof

A technology of silica and nanospheres, which is applied in the field of inorganic nanomaterials, can solve the problems of complex configuration of template double emulsions and obstacles to the practical application of hollow silica nanospheres, and achieve a simple and controllable process

Inactive Publication Date: 2009-10-21
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent application (publication number is CN101214965A) discloses a kind of preparation method of macroporous-mesoporous silica hollow microsphere, uses block copolymer P123 as template agent, generates stable oil / water / oil in water phase After the double emulsion, silicon source tetraethyl orthosilicate TEOS is added, hydrolyzed under the action of precipitant, filtered and dried, and calcined at 550°C to obtain silica hollow microspheres with macropore and mesoporous structure. And the application of this material as a slow-release carrier for abamectin drugs was studied, but the configuration of the template double emulsion required by this patent is relatively complicated, and the post-processing process requires high-temperature calcination to remove surfactants and organic solvents
The preparation methods of hollow silica microspheres involved in the above-mentioned patent applications or documents all require acid or alkaline conditions to catalyze the hydrolysis and condensation reactions of silicon sources such as tetraethyl orthosilicate, or simultaneously use high-temperature calcination or chemical corrosion To remove the template agent, it still cannot solve the above two problems, which greatly hinders the practical application of hollow silica nanospheres in the fields of catalytic systems, controlled drug release and microcapsules.

Method used

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Examples

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Effect test

Embodiment 1

[0045] 1.040g temperature-sensitive monomer N-isopropylacrylamide (NIPAm) was dissolved in anhydrous 1,4-dioxane, stirred under nitrogen atmosphere to fully dissolve, then added 5mg azobisisobutyl Nitrile, fully stirred, reacted at 80°C in an oil bath for 24 hours at a constant temperature under a nitrogen atmosphere, then took it out and cooled it to room temperature naturally; precipitated the resulting reactant with ether, centrifuged and vacuum dried to obtain poly-N-isopropyl Acrylamide white powder, tested by GPC, its weight average molecular weight is 3.7×10 4 , with a polydispersity index of 1.43.

[0046] Weigh 250mg of homopolymer poly-N-isopropylacrylamide and completely dissolve it in 50ml of deionized water at 20°C for 1 day to prepare a solution with a mass percentage concentration of 5‰. After heating to 50°C, the solution became turbid, indicating that polymer chains were aggregated, and stirred at constant temperature for 6 hours to obtain solution A. At the...

Embodiment 2

[0048] Weigh 150 mg of the homopolymer poly-N-isopropylacrylamide prepared in Example 1 and completely dissolve it in 50 ml of deionized water at 15°C for 1 day to prepare a solution with a mass percent concentration of 3‰. After heating to 50°C, the solution became turbid, indicating that polymer chains were aggregated, and stirred at constant temperature for 6 hours to obtain solution A. At the same time, measure 2.5ml of tetraethyl orthosilicate in 20ml of deionized water, and pre-hydrolyze at a constant temperature of 50°C for 3 hours to prepare solution B. Quickly transfer solution A to solution B, and react with magnetic sub-stirring at a constant temperature of 50°C for 160 hours. After the reaction is completed, the solution is translucent and slightly milky white. Add ethanol to the reaction solution for cleaning, first ultrasonically shake for 10 minutes, then centrifuge at a speed of 2000 rpm for 10 minutes, repeat this three times, and finally redisperse the obtai...

Embodiment 3

[0050] Weigh 150 mg of the homopolymer poly-N-isopropylacrylamide prepared in Example 1 and completely dissolve it in 50 ml of deionized water at 15° C. for 1 day to prepare a solution with a mass percent concentration of 3‰. After heating to 60°C, the solution became turbid, indicating that polymer chains were aggregated, and stirred at constant temperature for 6 hours to obtain solution A. At the same time, measure 2.5ml of tetraethyl orthosilicate in 20ml of deionized water, and pre-hydrolyze at a constant temperature of 60°C for 3 hours to prepare solution B. Quickly transfer solution A to solution B, and react with magnetic sub-stirring at a constant temperature of 60°C for 160 hours. After the reaction is completed, the solution is translucent and slightly milky white. Add ethanol to the reaction solution for cleaning, first ultrasonically shake for 10 minutes, then centrifuge at a speed of 2000 rpm for 10 minutes, repeat this three times, and finally redisperse the obt...

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Abstract

The invention discloses a method for preparing a hollow silica nanosphere by one step. The method comprises the following steps: mixing a poly-N-isopropyl acrylamide aqueous solution and an ethyl orthosilicate prehydrolysis solution at a temperature of 40 to 60 DEG C to react at a constant temperature for 160 to 180 hours; and carrying out ethanol washing, ultrasonic concussion, centrifugal separation and drying on a reaction liquid, and then obtaining the hollow silica nanosphere. The hollow silica nanosphere has a hollow core and mesoporous shell structure, the particle diameter is between 200 and 600 nm, and the shell thickness is between 30 and 100 nm. The invention also discloses the hollow silica nanosphere and the application. The method does not need to use an organic solvent to catalyze or further remove a template agent by high-temperature calcination or chemical corrosion, and can control the hollow nanosphere size and the shell thickness by simply changing the reaction temperature, the reaction time and the feed ratio.

Description

technical field [0001] The invention belongs to the field of inorganic nanomaterials and relates to hollow silica nanospheres, in particular to a hollow silica nanosphere based on a temperature-sensitive poly-N-isopropylacrylamide template, a preparation method and an application thereof. Background technique [0002] In recent years, hollow silica nanospheres have received extensive attention due to their potential applications in many fields such as catalysis, controlled drug release and microencapsulation. [0003] The method used to prepare hollow silica nanospheres is generally a template-based two-step method, in which the template material can be polymer latex, latex droplets, inorganic nanoparticles, aggregates or complexes of polymers, and surfactants. micelles. The first step: In the dispersion medium of the template material, the rapid hydrolysis and condensation of the silica precursor (such as tetraethyl orthosilicate) under alkaline conditions or the self-asse...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12C01B33/18B01J13/02
Inventor 杜滨阳曹峥李镇冰梅爱雄张兴宏聂晶晶徐君庭范志强
Owner ZHEJIANG UNIV
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