A kind of nano silicon dioxide microsphere and preparation method thereof

A nano-silicon dioxide, silicon dioxide technology, applied in the fields of silicon dioxide, microsphere preparation, silicon oxide, etc., can solve the problems of inability to obtain an ideal core-shell structure, polymer agglomeration, and restricting the deposition of silicon dioxide, etc. To achieve the effect of controllable shell thickness and cavity ratio, high hollow ratio and good monodispersity

Active Publication Date: 2018-12-11
宁波特粒科技有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

However, due to the use of persulfates (such as potassium persulfate or ammonium persulfate) in traditional soap-free emulsion polymerization systems, the surface of polymer microspheres is usually negatively charged, and the electrostatic repulsion with the silica shell greatly limits Further deposition of silica on its surface
[0009] Literature (Macromolecules 2016,49,1552.) also mentions the one-step synthesis of polystyrene / silica core-shell nanocomposite particles by miniemulsion polymerization of styrene stabilized by hyperbranched polyethoxysiloxane, but this This method needs to use high-speed shear emulsification equipment to obtain fine emulsion, otherwise the polymer will agglomerate later, and the ideal core-shell structure cannot be obtained. More importantly, this method can only be used for hydrophobic and weakly polar monomers such as styrene. Not suitable for highly polar and water-soluble monomers such as methacrylates, acrylates, acrylonitrile and methacrylonitrile
[0010] In short, there is no simple and efficient method in the prior art that can prepare nano-silica composite microspheres with a core-shell structure on a large scale

Method used

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  • A kind of nano silicon dioxide microsphere and preparation method thereof
  • A kind of nano silicon dioxide microsphere and preparation method thereof
  • A kind of nano silicon dioxide microsphere and preparation method thereof

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preparation example Construction

[0045] A preparation method of nano-silica microspheres, comprising the following steps:

[0046] 1) uniformly dispersing the initiator and the polyalkoxysiloxane in the core formation to obtain an organic phase;

[0047] 2) adding the organic phase to the water phase to obtain a two-phase-separated mixed system; under the condition of nitrogen protection, the mixed system is stirred and heated to react, and an emulsion containing nanocomposite microspheres is obtained after the reaction is finished;

[0048] 3) removing the solvent in the emulsion, retaining the nanocomposite microspheres, and drying the nanocomposite microspheres, namely obtaining nano-silica microspheres comprising a silica shell and a polymer core ;

[0049] 4) remove the polymer core in the nano-silica microspheres to obtain nano-silica hollow microspheres

[0050] Wherein, in step 1), firstly, the initiator is uniformly dispersed in the polymer forming material, then polyalkoxysiloxane is added, and mi...

Embodiment 1

[0053] A preparation method of nano-silica microspheres, comprising the following steps:

[0054] (1) Disperse 0.012 g of oil-soluble initiator azobisisobutyronitrile (AIBN) uniformly in 1.2 g of methyl methacrylate, add 1.2 g of polyethoxysiloxane, and ultrasonically disperse to obtain a uniform organic Mutually;

[0055] (2) The above organic phase was added to 30 grams of water (pH=7), and the mass of the organic phase was 8% of the mass of the aqueous phase. The two-phase mixture was stirred and heated to 65°C under nitrogen protection, and reacted for 24 hours. After the reaction, a polymethyl methacrylate / silica nanocomposite microsphere emulsion with a core-shell structure was obtained;

[0056] (3) centrifuge the above-mentioned emulsion for 10 min at a rotating speed of 8000 rpm, pour off the supernatant, redisperse the lower layer white solid object in water, ultrasonically wash, centrifuge again, wash again, and finally dry to obtain a dry Polymethyl methacrylate / ...

Embodiment 2

[0060] The difference between Example 2 and Example 1 is that the amount of azobisisobutyronitrile (AIBN) in step (1) is reduced to 0.01 g, and 1.2 g of methyl methacrylate monomer is changed to 0.8 g of methyl methacrylate. A mixture of methyl methacrylate monomer and 0.4 g of hexadecane; increase the heating temperature in step (3) to 70°C.

[0061] Finally, nanocomposite microspheres with a three-layer structure (silica / polymethyl methacrylate / hexadecane) are obtained, the size of the microspheres is about 400nm, and the outermost layer of the microspheres is a continuous and uniform silica layer , the middle layer is polymethyl methacrylate layer, and the inner layer is hexadecane. When the hexadecane is released, it goes to the hollow nanocomposite microspheres. After the polymer core was removed, the cavity of the hollow microspheres was further enlarged, but the spherical shape remained intact, showing good thermal and mechanical stability.

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Abstract

The invention discloses a nanosilicon dioxide pellet. The nanosilicon dioxide pellet comprises a silicon dioxide shell body and a polymer nuclear body which is wrapped inside the silicon dioxide shell body. The grain size of the silicon dioxide shell body is 50-1000 nm and the shell thickness of the silicon dioxide shell body is 5-75 nm. The nanosilicon dioxide pellet has a uniform size distribution, a controllable pellet size, shell thickness and cavity rate and good biocompatibility; in addition, the nanosilicon dioxide pellet has good heat stability, a high mechanical property and very good water dispersibility. The invention also discloses a preparing method of the nanosilicon dioxide pellet. The preparing method is a soap-free emulsion polymerization method and is simple to operate; a nano composite pellet with a nuclear shell structure can be synthesized in a large scale, that is, the polymer nuclear body and the silicon dioxide shell body can be formed at the same time; meanwhile, the preparing process is simple and efficient, and the product yield and the product purity are high, and thus the cost is reduced sharply.

Description

technical field [0001] The invention relates to the technical field of preparation of organic / inorganic nano-composite microspheres, in particular to a nano-silica microsphere and a preparation method thereof. Background technique [0002] In recent years, organic / inorganic nanocomposite microspheres have received more and more attention, because they have the plasticity, ease of processing, light weight of organic materials and the rigidity, heat resistance, wear resistance, and resistance of inorganic materials. Chemical corrosiveness, easy modification, and various functional properties, such as magnetic properties, electrical conductivity, etc. As a kind of organic / inorganic composite materials, polymer / silica nanocomposite microspheres with core-shell structure have been widely used in the fields of biomedicine, catalysis, electronic devices and colloidal interface research. The silica hollow microspheres show great application prospects in the fields of drug encapsula...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18C08F120/14C08F220/14C08F220/18B01J13/14B01J13/04
CPCB01J13/04B01J13/14C01B33/18C01P2004/03C01P2004/04C01P2004/32C01P2004/62C08F120/14C08F220/14C08F220/1804
Inventor 赵永亮邱雄豪
Owner 宁波特粒科技有限公司
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