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
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[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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