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Carboxyl functional high-cross-linking monodisperse polymer microsphere and preparation method thereof

A technology of monodisperse microspheres and carboxyl functionalization, which is applied in the preparation of microspheres and microcapsule preparations, and can solve the problems of low input of epoxy-based monomers, poor hydrophilicity of microspheres, and inability to withstand pressure. To achieve the effect of safe and reliable reaction conditions, high carboxyl content and rapid reaction

Inactive Publication Date: 2017-06-13
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent document CN102399340A discloses a method for preparing carboxylated polystyrene microspheres by soap-free emulsion polymerization. The microspheres obtained by this method are linear microspheres, which are not resistant to pressure and are not suitable for liquid chromatography systems under high pressure conditions.
However, the amount of epoxy-based monomer input in the microspheres obtained by this method is low, and the epoxy group content in the microspheres is only 30%, and the hydrophilicity of the obtained microspheres is relatively poor.

Method used

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  • Carboxyl functional high-cross-linking monodisperse polymer microsphere and preparation method thereof
  • Carboxyl functional high-cross-linking monodisperse polymer microsphere and preparation method thereof
  • Carboxyl functional high-cross-linking monodisperse polymer microsphere and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0029] Add 3.11 ml of divinylbenzene monomer, 1.86 ml of methacrylic acid monomer, and 379.6 mg of azobisisobutyronitrile into 30 ml of acetonitrile. Infuse nitrogen for 15 min, remove oxygen, and seal. Then place it in an oil bath, and the temperature of the oil bath is set to 85°C. Reaction time 4 hours. Stop heating, wash with ethanol, centrifuge, and dry to obtain poly(methacrylic acid-divinylbenzene) microspheres with a particle size of 3.046 µm, a polydispersity coefficient of 1.016, and a yield of 97.2% ( figure 1 ).

Embodiment 2

[0031] Add 2.59 ml of divinylbenzene monomer, 2.33 ml of methacrylic acid monomer, and 380.2 mg of azobisisobutyronitrile into 30 ml of acetonitrile. Infuse nitrogen for 15 min, remove oxygen, and seal. Then place it in an oil bath, and the temperature of the oil bath is set to 85°C. Reaction time 4 hours. Stop heating, wash with ethanol, centrifuge, and dry to obtain poly(methacrylic acid-divinylbenzene) microspheres with a particle size of 2.898 µm, a polydispersity coefficient of 1.029, and a yield of 75.2% ( figure 2 ).

Embodiment 3

[0033] Add 4.42 ml of divinylbenzene monomer, 0.66 ml of methacrylic acid monomer, and 378.8 mg of azobisisobutyronitrile to 27.20 ml of acetonitrile and 2.72 ml of propanol. After mixing, add to the polytetrafluoroethylene in the stainless steel reactor In the inner lining, nitrogen gas was passed through for 15 minutes, and after oxygen was removed, it was sealed. Then place it in an oil bath, and the temperature of the oil bath is set to 85°C. Reaction time 4 hours. Stop heating, wash with ethanol, centrifuge, and dry to obtain poly(methacrylic acid-divinylbenzene) microspheres with a particle size of 4.146 µm, a polydispersity coefficient of 1.019, and a yield of 83.6% ( image 3 ).

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Abstract

The invention relates to a carboxyl functional high-cross-linking monodisperse polymer microsphere and a preparation method thereof. The method comprises the following steps: adopting solvent thermal precipitation polymerization for adding methacrylic acid, diethyl benzene and initiator into solvent and uniformly mixing; placing into a stainless steel reaction kettle; increasing temperature and polymerizing; controlling the reaction temperature within 82 DEG C-200 DEG C and the reaction time within 1-12 hours; washing the acquired product with the solvent; centrifugally precipitating and drying, thereby acquiring the carboxyl functional high-cross-linking monodisperse polymer microsphere. The preparation method provided by the invention is simple; the monomer dosage reaches 20%; the microsphere yield is above 90%; the acquired microsphere is high in carboxyl content and is excellent in hydrophilicity.

Description

technical field [0001] The invention relates to a carboxyl functionalized highly cross-linked monodisperse polymer microsphere and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] Carboxyl group-containing highly cross-linked monodisperse microspheres have a wide range of applications in many fields such as chromatographic separation media, solid phase extraction materials, and enzyme immobilization substrates. [0003] The methods for preparing carboxyl-containing monodisperse microspheres mainly include soap-free emulsion polymerization, seed swelling polymerization and precipitation polymerization. Chinese patent document CN102399340A discloses a method for preparing carboxylated polystyrene microspheres by soap-free emulsion polymerization. The microspheres obtained by this method are linear microspheres, which are not resistant to pressure and are not suitable for liquid chromatography systems under high ...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F220/06B01J13/14
CPCB01J13/14C08F212/36C08F220/06
Inventor 张书香丁园园刘真
Owner UNIV OF JINAN
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