Preparation method of nano-silica with surface grafted with polystearylmethacrylate

A technology of polystearyl methacrylate and nano-silica, which is applied in the directions of dyeing organosilicon compound treatment, dyeing macromolecular organic compound treatment, fibrous filler, etc. The molecular structure and molecular weight are very different, and the polymer chains cannot penetrate each other, so as to increase the glass transition temperature, improve the shielding effect, and suppress the space charge.

Active Publication Date: 2015-04-08
TSINGHUA UNIV +1
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Problems solved by technology

[0005] Chemical modification includes surfactant method and surface graft polymerization method: (1) Commonly used surfactants include: silane coupling agent, stearic acid and silicone, etc. This method is simple to operate and is the most commonly used chemical modification method. However, because the surfactants are not macromolecular materials, they are very different from the molecular structure and molecular weight of the polymer matrix, and cannot interpenetrate with the polymer chains, so the effect of improving the dispersion of nanoparticles is not ideal; (2 ) Surface graft polymerization has become an important means of nanoparticle modification, with many types of graft polymers and good controllability

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  • Preparation method of nano-silica with surface grafted with polystearylmethacrylate
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  • Preparation method of nano-silica with surface grafted with polystearylmethacrylate

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preparation example Construction

[0020] The preparation method of the surface grafted polyoctadecyl methacrylate nano silicon dioxide that the present invention proposes comprises the following steps:

[0021] (1) First disperse silicon dioxide in a strong polar solvent to obtain a silicon dioxide solution with a mass percentage concentration of 10% to 40%. The strong polar solvent is: methanol, ethanol, methyl ethyl ketone, chloroform , tetrahydrofuran or toluene; add aminosilane to the silica solution so that the molar concentration of aminosilane in the silica solution is 1-10mol / L, and reflux at 50-120°C for 5-24 hours in a nitrogen atmosphere , to obtain the first mixed solution, the aminosilane is 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyldimethylmethoxysilane or 4-aminobutyl Base triethoxysilane; at normal temperature, n-hexane is added to the first mixed solution, and the volume ratio is: n-hexane: first mixed solution=(5~15): 1, after waiting for the solid to completel...

Embodiment 1

[0026] (1) At first, silicon dioxide is dispersed in methanol to obtain a silicon dioxide solution with a mass percent concentration of 30%; 3-aminopropyltriethoxysilane is added to the silicon dioxide solution to make 3-aminopropyl The molar concentration of triethoxysilane in the silicon dioxide solution is 3 mol / L, and in a nitrogen atmosphere, reflux at 60°C for 12 hours to obtain the first mixed solution; add n-hexane to the first mixed solution at normal temperature, The adding volume ratio is: n-hexane: the first mixed solution=10:1, after waiting for the solid to precipitate completely, the mixture is centrifuged, and the separated solid is dissolved in the above-mentioned methanol to obtain a mass volume concentration of 0.3g / mL of solution; repeat the steps of precipitation-centrifugation-dissolution, and finally obtain the nano-silica solution of surface-grafted aminosilane, which is denoted as the first solution;

[0027] (2) Cumyl dithiobenzoate is added to the m...

Embodiment 2

[0035] (1) At first, silicon dioxide is dispersed in ethanol to obtain a silicon dioxide solution with a mass percent concentration of 30%; 3-aminopropyltriethoxysilane is added to the silicon dioxide solution to make 3-aminopropyl The molar concentration of triethoxysilane in the silicon dioxide solution is 3 mol / L, and in a nitrogen atmosphere, reflux at 60°C for 12 hours to obtain the first mixed solution; add n-hexane to the first mixed solution at normal temperature, The adding volume ratio is: n-hexane: the first mixed solution=10:1, after waiting for the solid to precipitate completely, the mixture is centrifuged, and the separated solid is dissolved in the above-mentioned ethanol to obtain a mass volume concentration of 0.3g / mL of solution; repeat the steps of precipitation-centrifugation-dissolution, and finally obtain the nano-silica solution of surface-grafted aminosilane, which is denoted as the first solution;

[0036] (2) Cumyl dithiobenzoate is added to the eth...

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Abstract

The invention relates to a preparation method of nano-silica with the surface grafted with polystearylmethacrylate, belonging to the field of surface grafting and modification of nano-particles. The preparation method comprises the following steps of firstly grafting amino silane to the surface of nano-silica in a high polar solvent by virtue of a reversible addition-fragmentation chain transfer polymerization method; then grafting a chain transfer agent to the surfaces of nano-particles through amino silane by virtue of the combination between thiol ester functional groups and amino functional groups on the chain transfer agent; finally providing free radicals by an initiator, and polymerizing monomers of polystearylmethacrylate to the tail end of the chain transfer agent. According to the polystearylmethacrylate-grafted nano-silica nano-particles prepared by virtue of the preparation method, the dispersity of nano-silica in low density polyethylene and a crosslinked polyethylene matrix is improved. According to the preparation method, a firm foundation is laid for the further improvement of mechanical and electrical properties of polyvinyl nano-composite materials.

Description

technical field [0001] The invention relates to a preparation method of surface-grafted polyoctadecyl methacrylate nano-silica, which belongs to the field of nano-particle surface graft modification. Background technique [0002] Since entering the 21st century, nanotechnology has been used more and more, and its role in promoting the material industry cannot be underestimated. All industrialized countries are investing a lot of money in the research of nano-polymer materials to meet the growing industrial needs and gradually form an international competition. [0003] The improvement of the performance of polymer materials by the addition of nanoparticles is an important manifestation of the role of nanotechnology in promoting the material industry. Appropriate addition of nanoparticles can improve the mechanical, optical, electrical, and biological properties of polymer materials. However, nanoparticles have the characteristics of small volume and large surface energy, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/12C09C3/10C08F292/00C08F220/18C08L23/06C08K9/06C08K9/04C08K3/36
Inventor 周远翔张灵尹琪张云霄郭大卫程子霞
Owner TSINGHUA UNIV
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