Nanosilicon dioxide pellet and preparing method thereof

A technology of nano-silica and silicon dioxide, which is applied in the preparation of microspheres, silicon dioxide, silicon oxide, etc., can solve the problems of not being able to obtain an ideal core-shell structure, limiting silica deposition, and polymer agglomeration. Achieve the effects of controllable shell thickness and cavity ratio, good monodispersity and high hollow ratio

Active Publication Date: 2017-02-22
宁波特粒科技有限公司
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  • Abstract
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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

Method used

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  • Nanosilicon dioxide pellet and preparing method thereof
  • Nanosilicon dioxide pellet and preparing method thereof
  • Nanosilicon dioxide pellet and preparing method thereof

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preparation example Construction

[0045] A preparation method for nano silicon dioxide microspheres, comprising the following steps:

[0046] 1) uniformly dispersing the initiator and the polyalkoxysiloxane in the nuclei forming material to obtain an organic phase;

[0047] 2) adding the organic phase to the water phase to obtain a mixed system of two-phase separation; stirring and heating the mixed system under the condition of nitrogen protection, and obtaining an emulsion containing nanocomposite microspheres after the reaction;

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

[0049] 4) removing the polymer core body 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, mixed uni...

Embodiment 1

[0053] A preparation method for nano silicon dioxide microspheres, comprising the following steps:

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

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

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

Embodiment 2

[0060] The difference between embodiment 2 and embodiment 1 is that the amount of azobisisobutyronitrile (AIBN) in step (1) is reduced to 0.01 gram, and 1.2 gram of methyl methacrylate monomer is changed into 0.8 gram of methyl methacrylate A mixture of methyl acrylate monomer and 0.4 gram of hexadecane; the heating temperature in step (3) was raised 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 a polymethyl methacrylate layer, and the inner layer is hexadecane. After the hexadecane is released, it will enter the hollow nanocomposite microspheres. After removing the polymer core, the cavity of the hollow microspheres is further enlarged, but still maintains a complete spherical shape, 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 nanocomposite microspheres, in particular to a nano silicon dioxide 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 both the plasticity, ease of processing, and light weight of organic materials and the rigidity, heat resistance, wear resistance, and durability of inorganic materials. Chemically corrosive, easy to modify, and various functional properties, such as magnetism, 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 colloid interface research. Silica hollow microspheres show great application prospects in the fields of drug encapsulation and sustain...

Claims

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Application Information

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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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