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Preparation method for monodisperse hollow silicon dioxide nanosphere with controllable size and shell thickness

A silicon dioxide, monodisperse technology, applied in the direction of silicon dioxide, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problem of wide size distribution, wide size distribution of hollow silica nanospheres, The thickness of the shell layer is uncontrollable, etc., to achieve the effect of a simple preparation method

Inactive Publication Date: 2013-10-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation method disclosed in this patent can produce hollow silica nanospheres through one-step reaction, without removing the template through high-temperature calcination or acid-base corrosion. The process is simple, but the size distribution of the obtained hollow silica nanospheres is wide, And the size and shell thickness are uncontrollable
[0005] The hollow silica nanospheres obtained by the preparation method mentioned in the above-mentioned patent documents are all non-monodisperse structures, and there is a problem that the size distribution is wide, and the size and shell thickness are uncontrollable, which greatly limits the use of hollow silica nanospheres. Practical applications in the field of controlled drug release, catalysis and microencapsulation

Method used

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  • Preparation method for monodisperse hollow silicon dioxide nanosphere with controllable size and shell thickness
  • Preparation method for monodisperse hollow silicon dioxide nanosphere with controllable size and shell thickness
  • Preparation method for monodisperse hollow silicon dioxide nanosphere with controllable size and shell thickness

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Experimental program
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Effect test

Embodiment 1

[0042] 250 mg of N-isopropylacrylamide monomer was dissolved in 48 ml of deionized water to obtain monomer aqueous solution I. 10 mg of ammonium persulfate was dissolved in 2 ml of deionized water to obtain aqueous initiator solution II. Under the condition of stirring, the monomer aqueous solution I was heated to 70° C., and nitrogen gas was used to remove oxygen for 30 minutes. Then, the initiator aqueous solution II was added to the monomer aqueous solution I to initiate a radical polymerization reaction for 6 hours to obtain an emulsion of poly-N-isopropylacrylamide, and after the reaction was completed, the temperature was lowered to 50° C. to obtain emulsion A. At 50°C, 2ml tetraethyl orthosilicate was added to 18ml for prehydrolysis for 3 hours to obtain solution B. The emulsion A was added to the solution B, and reacted at 50° C. for 72 hours to obtain monodisperse nanoparticles of poly-N-isopropylacrylamide coated with silicon dioxide.

[0043] Drop the obtained aqu...

Embodiment 2

[0045] Dissolve 50 mg of N-isopropylacrylamide monomer in 48 ml of deionized water to obtain monomer aqueous solution I. 10 mg of azobisisobutylamidine hydrochloride was dissolved in 2 ml of deionized water to obtain aqueous initiator solution II. Under the condition of stirring, the monomer aqueous solution I was heated to 65° C., and nitrogen gas was used to remove oxygen for 30 minutes. Then, the initiator aqueous solution II was added to the monomer aqueous solution I to initiate a radical polymerization reaction for 3 hours to obtain an emulsion of poly-N-isopropylacrylamide. After the reaction, the temperature was lowered to 40° C. to obtain emulsion A. At 40°C, 0.5ml tetraethyl orthosilicate was added to 18ml for prehydrolysis for 2 hours to obtain solution B. The emulsion A was added to the solution B, and reacted at 45° C. for 96 hours to obtain monodisperse nanoparticles of poly-N-isopropylacrylamide coated with silica. Calcining the monodisperse nanoparticles of p...

Embodiment 3

[0047] 250 mg of N-isopropylacrylamide monomer was dissolved in 48 ml of deionized water to obtain monomer aqueous solution I. 150 mg of azobisisobutylamidine hydrochloride was dissolved in 2 ml of deionized water to obtain aqueous initiator solution II. Under the condition of stirring, the monomer aqueous solution I was heated to 75° C., and nitrogen gas was used to remove oxygen for 30 minutes. Then, the initiator aqueous solution II was added to the monomer aqueous solution I to initiate a free radical polymerization reaction for 6 hours to obtain an emulsion of poly-N-isopropylacrylamide. After the reaction, the temperature was lowered to 60° C. to obtain emulsion A. At 60°C, 0.5ml tetraethyl orthosilicate was added to 12ml for prehydrolysis for 5 hours to obtain solution B. The emulsion A was added to the solution B, and reacted at 55° C. for 84 hours to obtain monodisperse nanoparticles of poly-N-isopropylacrylamide coated with silica. Calcining the monodisperse nanopa...

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Abstract

The invention discloses a preparation method for a monodisperse hollow silicon dioxide nanosphere with the controllable size and shell thickness. The preparation method comprises the following steps of: preparing poly-N-isopropylacrylamide by polymerizing an N-isopropylacrylamide monomer with soap-free emulsion under an oxygen-free condition at 60-80 DEG C; after mixing the prepared poly-N-isopropylacrylamide emulsion with prehydrolysis solution of tetraethoxysilane at 40-60 DEG C, carrying out a thermostatic reaction for 48-96 hours, and obtaining the monodisperse hollow silicon dioxide nanosphere after separating and calcining. The preparation method is simple and controllable, and the water is taken as the solvent in each reaction, so that the preparation method is green and environment-friendly; the obtained hollow silicon dioxide nanosphere is of a monodisperse structure, the size is 100-500 nm, the shell thickness is 30-100 nm, and the size and the thickness are both controllable, so that the method can be widely applied to the fields of medical controllable slow release, catalysis, microcapsules and the like.

Description

technical field [0001] The invention relates to the field of inorganic nanometer materials, in particular to a method for preparing monodisperse hollow silica nanospheres with controllable size and shell thickness. Background technique [0002] Due to its high melting point, high stability, non-toxic and other special properties, hollow silica microspheres have potential application prospects in many fields, such as catalysis, drug controllable sustained release and microcapsules. s concern. [0003] The preparation of hollow silica nanospheres mainly adopts the template method, and the template material can be polymer latex, latex droplets, inorganic nanoparticles, aggregates or complexes of polymers, and micelles of surfactants. The size and distribution of the template material determine the size and distribution of the hollow silica nanospheres, so selecting a suitable template to prepare hollow silica nanospheres is the key to obtaining monodisperse and size-controllab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y30/00
Inventor 杜滨阳陈天有聂晶晶范志强
Owner ZHEJIANG UNIV
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