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Preparation method of monodisperse polymer/SiO2 nano composite particles

A nano-composite particle and polymer technology, applied in the field of monodisperse polymer/SiO2 nano-composite particles, can solve the problems of reducing the composite efficiency of inorganic particles and polymers and increasing the solubility, etc.

Active Publication Date: 2016-07-20
浙江金嘉科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is a method of adding ethanol to the miniemulsion polymerization reaction system to synthesize monodisperse polymer nanoparticles, but this method has the following defects: (1) additional use of organic solvent is required; (2) after the introduction of ethanol, the addition of monodisperse polymer nanoparticles The solubility of the body in the continuous phase is easy to cause secondary nucleation to form blank polymer particles, reducing the composite efficiency of inorganic particles and polymers

Method used

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  • Preparation method of monodisperse polymer/SiO2 nano composite particles
  • Preparation method of monodisperse polymer/SiO2 nano composite particles
  • Preparation method of monodisperse polymer/SiO2 nano composite particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Tween-20 was selected as the non-ionic emulsifier, and 1.25 g was weighed and dissolved in 125 g of water to obtain an aqueous solution of Tween-20.

[0038] 8gSiO 2 Nanoparticles (15nm, coupling density 3.5μmol·(m 2 SiO 2 ) -1 ) pre-dispersed in 32g of methyl methacrylate, plus 13.6g of styrene and 2.2g of n-hexadecane to obtain SiO 2 Monomer dispersion of nanoparticles.

[0039] SiO 2 The monomer dispersion of nanoparticles is added to the aqueous solution of Tween-20, and the coarse emulsion is obtained after pre-emulsification. The container containing the coarse emulsion is placed in an ice-water bath, and a stable single body lotion. Take by weighing 0.013g dodecyl dimethyl hydroxypropyl sulfobetaine again, add in the monomer miniemulsion, stir 15min, then add 0.7g water-soluble initiator potassium persulfate, nitrogen deoxygenation, temperature rising Reaction at 75°C for 3h under nitrogen protection to obtain monodisperse polymer / SiO 2 nanocomposite part...

Embodiment 2

[0042] Use OP-10 as the non-ionic emulsifier, weigh 10 g, and dissolve it in 125 g of water to obtain an aqueous solution of OP-10.

[0043] 1.5gSiO 2 Nanoparticles (30nm, coupling density 2.5μmol·(m 2 SiO 2 ) -1 ) pre-dispersed in 13.5g methyl methacrylate, then add 5g 3-trimethoxysilyl methacrylate and 1.48g n-hexadecane to get SiO 2 Monomer dispersion of nanoparticles.

[0044] SiO 2 The monomer dispersion of nanoparticles is added to the aqueous solution of OP-10, and the coarse emulsion is obtained after pre-emulsification. The container containing the coarse emulsion is placed in an ice-water bath, and the ultrasonic power of 500W is ultrasonicated for 5 minutes to obtain a stable monomer. fine emulsion. Then weigh 1.13g of cetyltrimethylammonium bromide, add it to the monomer miniemulsion, stir for 30min, then add 0.19g of water-soluble initiator 2,2'-azobisbutylamidine dihydrochloride , Nitrogen to remove oxygen, the temperature rises to 65 ° C, and reacts for 5...

Embodiment 3

[0047] The non-ionic emulsifier is MOA-9, weigh 0.5g, dissolve it in 125g water, and obtain the aqueous solution of MOA-9.

[0048]0.2gSiO 2 Nanoparticles (50nm, coupling density 2.0μmol·(m 2 SiO 2 ) -1 ) pre-dispersed in 7.3g of methyl methacrylate, plus 2.5g of butyl acrylate and 0.3g of n-hexadecane to obtain SiO 2 Monomer dispersion of nanoparticles.

[0049] SiO 2 The monomer dispersion of nanoparticles is added to the aqueous solution of MOA-9, and the coarse emulsion is obtained after pre-emulsification. The container containing the coarse emulsion is placed in an ice-water bath, and the ultrasonic power of 60W is ultrasonicated for 45 minutes to obtain a stable monomer. fine emulsion. Then weigh 0.18g of sodium lauryl sulfate, add it to the monomer miniemulsion, stir for 30 minutes, add 0.03g of sodium bisulfite to the above monomer miniemulsion, pass nitrogen to remove oxygen, and the temperature rises to 40°C , then add 0.05g ammonium persulfate, and react for...

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Abstract

The invention provides a preparation method of monodisperse polymer / SiO2 nano composite particles. The method comprises the following steps of (1) dissolving a water-soluble non-ionic emulsifier into water so as to obtain an emulsifier aqueous solution; (2) dispersing hydrophobic SiO2 nano particles into part of monomers, and adding a co-stabilizer and residual monomers, thereby obtaining a monodisperse solution of the SiO2 nano particles, wherein the monomers are selected from at least one of styrene and acrylic ester compounds as shown in a formula (I); (3) adding the monodisperse solution of SiO2 into the non-ionic emulsifier aqueous solution, stirring for pre-emulsification so as to obtain a crude emulsion, performing ultrasonic treatment in an ice-water bath so as to obtain a monomer miniemulsion, adding a water-soluble ionic emulsifier into the monomer miniemulsion, introducing nitrogen to remove oxygen, and reacting in the protection of nitrogen so as to obtain the monodisperse polymer / SiO2 nano composite particles, wherein an initiator can be added through the following two modes: adding an oil-soluble initiator into the monodisperse solution of the SiO2 nano particles or adding a water-soluble initiator into the monomer miniemulsion. The formula I is as shown in the specification.

Description

(1) Technical field [0001] The invention relates to a method for preparing nanocomposite particles, in particular to a method for preparing monodisperse polymer / SiO with good sphericity, controllable size, and high composite rate of polymer and inorganic particles by using miniemulsion polymerization technology. 2 Methods for Nanocomposite Particles. (2) Background technology [0002] The polymer / inorganic particle nanocomposite material compounded at the nanoscale can maximize the synergistic properties of polymers and inorganic materials, not only can greatly improve the processing performance, mechanical properties and thermal properties of the material, but also endow the material with light, The functions of electricity, magnetism and catalysis make it have broad application prospects in high-end fields such as aerospace, biomedicine and catalysis. As an important representative of nanocomposites, SiO 2 Polymer / SiO with nanoparticles as dispersed phase and polymer as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/14C08F212/08C08F230/08C08F220/18C08F2/30C08F2/26C08F2/28C08F2/44C08K3/36
CPCC08F2/26C08F2/28C08F2/30C08F2/44C08F220/14C08K3/36C08K2201/011C08F220/1804C08F230/08
Inventor 曹志海陈群赵淑宁梁小琴刘金霖戚栋明
Owner 浙江金嘉科技有限公司
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