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Preparation method of polyacrylic acid hollow microgel

A technology of polyacrylic acid and microgel, which is applied in the field of preparation of polyacrylic acid hollow microgel to achieve good emulsification stability, easy implementation, and good monodispersity

Active Publication Date: 2015-09-09
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no patent or literature to prepare polyacrylic acid hollow microgel by using Pickering miniemulsion method with acrylonitrile as monomer

Method used

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  • Preparation method of polyacrylic acid hollow microgel
  • Preparation method of polyacrylic acid hollow microgel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 12g of acrylonitrile, 1.2g of divinylbenzene, 0.8g of hexadecane, 2.4g of isooctane, 10g of ethyl orthosilicate, 1.0g of γ-(methacryloyloxy)propyltrimethoxysilane and 0.2 g azobisisoheptanonitrile was magnetically stirred for 30 minutes to fully dissolve it as an oil phase;

[0037]Weigh 0.02g of sodium nitrite and dissolve it in deionized water with magnetic stirring for 10min to fully dissolve it as the water phase; slowly add the oil phase into the water phase, then add 1g of triethylamine, stir magnetically at room temperature for 30min to form a mixed solution; Then use a high-speed shearing device to homogeneously emulsify for 5 minutes at a shear rate of 16000 rpm under an ice-water bath to form a fine emulsion;

[0038] Transfer the fine emulsion to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, pass nitrogen gas for 30 minutes under stirring to remove the air in the system, and react at a constant temperature in a water bath...

Embodiment 2

[0040] 12g of acrylonitrile, 1.2g of divinylbenzene, 0.8g of hexadecane, 1.2g of isooctane, 10g of ethyl orthosilicate, 1.0g of γ-(methacryloyloxy)propyltrimethoxysilane and 0.2 g azobisisoheptanonitrile was magnetically stirred for 30 minutes to fully dissolve it as an oil phase;

[0041] Weigh 0.02g of sodium nitrite and dissolve it in deionized water and stir it magnetically for 10 minutes to make it fully dissolved as the water phase;

[0042] Slowly add the oil phase to the water phase, then add 1g of triethylamine, stir magnetically at room temperature for 30 minutes to form a mixed solution; then use a high-speed shearing device in an ice-water bath to homogeneously emulsify at a shear rate of 16000rpm for 5 minutes to form a fine emulsion ;

[0043] Transfer the fine emulsion to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, pass nitrogen gas for 30 minutes under stirring to remove the air in the system, and react at a constant tem...

Embodiment 3

[0045] 12g of acrylonitrile, 1.2g of divinylbenzene, 0.8g of hexadecane, 2.4g of isooctane, 10g of ethyl orthosilicate, 2.0g of γ-(2,3-epoxypropoxy)propyltrimethoxy Silane and 0.2 g of azobisisoheptanonitrile were magnetically stirred for 30 minutes to fully dissolve it as an oil phase;

[0046] Weigh 0.02g of sodium nitrite and dissolve it in deionized water with magnetic stirring for 10min to fully dissolve it as the water phase; slowly add the oil phase into the water phase, then add 1g of triethylamine, stir magnetically at room temperature for 30min to form a mixed solution; Then use a high-speed shearing device to homogeneously emulsify for 5 minutes at a shear rate of 16000 rpm under an ice-water bath to form a fine emulsion;

[0047] Transfer the fine emulsion to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, pass nitrogen gas for 30 minutes under stirring to remove the air in the system, and react at a constant temperature in a wat...

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Abstract

The invention discloses a preparation method of polyacrylic acid hollow microgel. According to the preparation method, an oil phase is added into a water phase, triethylamine and tetraethoxysilane are dropwise added under an alkaline condition to carry out in-situ hydrolysis to generate nano-silica particles as a surfactant, and a stable 'oil-in-water' form Pickering emulsion is generated; polyacrylonitrile is incompatible with isooctane, so that raw monomer droplets are subjected to phase separation, and isooctane is extruded to the centers of the droplets of a mini-emulsion to form liquid cores; after monomers are polymerized, polyacrylonitrile hollow microspheres are obtained and are subjected to basic hydrolysis to generate the polyacrylic acid hollow microgel. The preparation method has the advantages that the process is simple, the operation is feasible, reaction conditions are mild and easy to control, the consumption of the surfactant is reduced, and the preparation method is applicable to industrial production and is environment-friendly. The prepared polyacrylic acid hollow microgel is stable in structure and controllable in hollow size and can be applied to the fields of medicine controlled release, chemical separation, biosensing and the like.

Description

technical field [0001] The invention belongs to the field of microgel preparation, in particular to a preparation method of polyacrylic acid hollow microgel. Background technique [0002] Polymer nano hollow microspheres are functional materials with a special structure. Due to their high specific surface area, low density, large loading space and encapsulation effect functionalization, they are widely used in biology, chemistry, catalysis, optics and other fields. has received widespread attention. Polymer nano hollow microspheres are usually spherical shells formed by polymers. If the polymers that make up the hollow microspheres contain magnetic particles, photosensitive groups, temperature sensitive groups or -COOH, -NH 2 ,-CONH 2 and other easily ionizable groups, the hollow microspheres will have strong environment-dependent properties such as magnetic field, optics, temperature, pH or ionic strength. This environmental response characteristic makes polymer nano ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/44C08F212/36C08F8/12C08F2/24
Inventor 张建安吴庆云吴明元杨建军陆正全
Owner ANHUI UNIVERSITY
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