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High-specific surface polymer microsphere resin with even particle size and preparation method thereof

A high specific surface area, polymer technology, applied in the direction of microsphere preparation, microcapsule preparation, alkali metal compounds, etc., can solve the problem that the particle size of synthetic resin microspheres cannot be effectively controlled, the synthesis steps are shortened, and it is difficult to meet actual needs, etc. problem, to achieve the effect of facilitating large-scale production, simple steps and strong repeatability

Inactive Publication Date: 2010-07-14
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the fact that the existing preparation method of microsphere resin cannot effectively control the particle size of synthetic resin microspheres, and it is difficult to meet the actual demand for the synthesis of monodisperse microspheres with different particle sizes, the present invention provides a uniform particle size high specific surface area Polymer microsphere resin and its preparation method, through the membrane emulsification-suspension polymerization method, using monomer polymerization with active groups to shorten the synthesis steps, to obtain high specific surface area polymer microspheres with uniform particle size and controllable size

Method used

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  • High-specific surface polymer microsphere resin with even particle size and preparation method thereof
  • High-specific surface polymer microsphere resin with even particle size and preparation method thereof

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Embodiment 1

[0035] The mass ratio of chloromethylstyrene, divinylbenzene, n-heptane and benzoyl peroxide in the oil phase is 95:5:60:2, 50g in total. In the aqueous phase, 3 g of polydiene dimethyl ammonium chloride and 2 g of polyvinyl alcohol were dissolved in 450 g of water. The selected SPG membrane has a pore size of 0.5 μm and forms an emulsion under a nitrogen pressure of 0.2 MPa. Transfer the emulsion into a three-necked bottle, stir slowly, and raise the temperature to 70°C under the protection of nitrogen to initiate the reaction, polymerize for 6 hours, then gradually raise the temperature to 95°C, and react for 12 hours. Centrifuge the obtained chlorine balls, wash with water, ethanol, and acetone, add dichloroethane to swell for 6 hours after drying, and react at 80°C under the catalysis of ferric chloride (the mass ratio of catalyst addition to microsphere resin is 1:5) Resin microspheres were obtained after 12 hours, and the finished product was obtained by washing with et...

Embodiment 2

[0038] The mass ratio of chloroacetylated styrene, divinylbenzene, toluene and azobisisobutyronitrile in the oil phase is 90:10:100:1, totaling 50 g. Add 2g of gelatin to the water phase, dissolve in 450g of water. The selected SPG membrane has a pore size of 1 μm and forms an emulsion under a nitrogen pressure of 0.1 MPa. Transfer the emulsion into a three-necked bottle, stir slowly, and raise the temperature to 70°C under the protection of nitrogen to initiate the reaction, polymerize for 4 hours, then gradually raise the temperature to 80°C, and react for 5 hours. Centrifuge the obtained chlorine balls, wash with water, ethanol, and acetone, add nitrobenzene to swell after drying, and react under the catalysis of aluminum chloride (the mass ratio of catalyst addition to microsphere resin is 1:6) at 85°C for 16 hours to obtain Resin microspheres, washed with ethanol and acetone to obtain finished products.

[0039] The particle size of the resin microspheres is about 3.7 μ...

Embodiment 3

[0041] The mass ratio of chloroacetylated styrene, divinylbenzene, n-dodecane and azobisisobutyronitrile in the oil phase is 80:20:50:1, 50 g in total. Add 4 g of hydroxyethyl cellulose to the water phase and dissolve in 450 g of water. The selected SPG membrane has a pore size of 1 μm and forms an emulsion under a nitrogen pressure of 0.08 MPa. Transfer the emulsion into a three-necked bottle, stir slowly, and raise the temperature to 70°C under the protection of nitrogen to initiate the reaction, polymerize for 4 hours, then gradually raise the temperature to 80°C, and react for 8 hours. Centrifuge the obtained chlorine balls, wash them with water, ethanol, and acetone, add nitrobenzene to swell after drying, and react under the catalysis of zinc chloride (the mass ratio of catalyst addition to microsphere resin is 1:4) at 85°C for 14 hours to obtain Resin microspheres, washed with ethanol and acetone to obtain finished products.

[0042] The particle size of the resin mic...

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PUM

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Abstract

The invention discloses a high-specific surface polymer microsphere resin with even particle size and a preparation method thereof. In the method, a high-specific surface resin microsphere is prepared by the following steps of: dispersing vinylbenzylchloride and the like as monomers by a membrane emulsification method and polymerizing at a certain temperature and condition. The monodisperse polymer microsphere resin within the range of 1-60 Mum can be synthetized by the method, wherein the specific surface is 800-1200m2 / g. The invention has simple steps and environmental pollution reduction, easy control of process flow, strong repeatability, thereby being beneficial to scale production. The resin microsphere prepared by the method has very high specific surface, thereby being beneficial to carrying out enrichment separation and analysis on water-soluble organic pollutants in a water body and having wide application prospect.

Description

Technical field: [0001] The invention relates to a polymer microsphere resin and a preparation method thereof, in particular to a polymer microsphere resin with uniform particle size and high specific surface area and a preparation method thereof. Background technique: [0002] The analysis and detection of water-soluble organic pollutants is an important issue in current environmental monitoring. The development of suitable solid-phase extraction and liquid chromatography packing is the core of the enrichment, separation and analysis of such substances. Relying on its high specific surface area, polymer resin adsorbents are much better at extracting polar compounds from water samples than traditional silicon-based and carbon-based adsorbents, but the hydrophobicity of such adsorbents leads to their enrichment Poor ability. Although the adsorbents modified with hydrophilic groups increase the force on the analyte through hydrogen bonding, electrostatic and hydrophilic inter...

Claims

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Application Information

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IPC IPC(8): B01J13/14B01J20/26B01J20/28B01J20/30
Inventor 李爱民周庆张满成钟声唐松林双陈冬薛玉志王津南徐伟
Owner NANJING UNIV
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