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Method for preparing high cross-linking monodisperse polymer micro-sphere

A monodisperse, polymer technology, applied in the field of preparation of high cross-linking, monodisperse polymer microspheres, can solve problems such as unstable reaction of the polymerization system, inability to proceed, rough surface of polymer microspheres, etc., to achieve the method Simple, easy to handle, good thermal stability results

Inactive Publication Date: 2008-04-30
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cross-linked polymer microspheres can also be obtained by dispersion polymerization, but the cross-linking agent concentration relative to the monomer is lower than 5wt%. When the cross-linking agent concentration is further increased, the surface of the obtained polymer microspheres is rough, or polymerization The system is unstable and flocculation occurs so that the reaction cannot go on

Method used

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  • Method for preparing high cross-linking monodisperse polymer micro-sphere
  • Method for preparing high cross-linking monodisperse polymer micro-sphere
  • Method for preparing high cross-linking monodisperse polymer micro-sphere

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The dispersant PVP (1.0 g) was dissolved in absolute ethanol (63 g) in a container, and stirred to dissolve. Under the protection of nitrogen, the temperature was raised to 70°C. After passing nitrogen for half an hour, styrene (10.0 g) dissolved with initiator AIBN (0.3 g) was added, and the stirring speed was adjusted to 120 rpm. After 4 hours of reaction, Dehydrated ethanol (22 g) dissolved in divinylbenzene (1.0 g) was slowly added at a rate of 0.13 mL / min, and the total reaction time was 12 h. After the reaction, the product was diluted with a large amount of absolute ethanol, centrifuged, and the dispersion medium and stabilizer were removed. The solid was washed 5 times with absolute ethanol and 3 times with water, and vacuum-dried at room temperature to constant weight. The yield was 83.2%.

[0027] The obtained polymer microspheres had a particle size of 1.75 μm, a particle size distribution of 1.005, a swelling ratio of 1.07, a WLR value of 6.2 wt%, and a ther...

Embodiment 2

[0029] The dispersant PVP (1.0 g) was dissolved in anhydrous methanol (63 g) in a container, and stirred to dissolve. Under the protection of nitrogen, the temperature was raised to 30°C. After passing nitrogen for half an hour, styrene (10.0 g) dissolved with initiator AIBN (0.3 g) was added, and the stirring speed was adjusted to 140 rpm. After 4 hours of reaction, Slowly add anhydrous methanol (22 g) dissolved in divinylbenzene (2.0 g) at a rate of 0.18 mL / min, and the total reaction time is 24 h. After the reaction, the product was diluted with a large amount of absolute ethanol, centrifuged, and the dispersion medium and stabilizer were removed. The solid was washed 5 times with absolute ethanol and 3 times with water, and vacuum-dried at room temperature to constant weight. The yield was 85.7%.

[0030] The obtained polymer microspheres had a particle size of 2.47 μm, a particle size distribution of 1.008, a swelling ratio of 1.03, a WLR value of 4.5 wt%, and a thermal d...

Embodiment 3

[0032] The dispersant PVP (2.0 g) was dissolved in absolute ethanol (63 g) in a container, and stirred to dissolve. Under the protection of nitrogen, the temperature was raised to 80°C. After passing nitrogen for half an hour, styrene (10.0 g) dissolved with initiator AVBN (0.5 g) was added, and the stirring speed was adjusted to 150 rpm. After reacting for 4 hours, Dehydrated ethanol (22 g) dissolved in divinylbenzene (3.0 g) was slowly added at a rate of 0.13 mL / min, and the total reaction time was 12 h. After the reaction, the product was diluted with a large amount of absolute ethanol, centrifuged, and the dispersion medium and stabilizer were removed. The solid was washed 5 times with absolute ethanol and 3 times with water, and vacuum-dried at room temperature to constant weight. The yield was 88.5%.

[0033] The obtained polymer microspheres had a particle size of 3.23 μm, a particle size distribution of 1.006, a swelling ratio of 1.02, a WLR value of 3.9 wt%, and a the...

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Abstract

The invention relates to a preparation method for polymer microspheres having good solvent resistance and thermal stability, controllable particle diameter, monodisperse, smooth surface, and high cross linking degree, and belongs to the micro nanometer functional material field. The invention takes styrene below 20 wt percent as a monomer, takes 60 to 92 wt percent of low molecular weight fat (poly) alcohol as dispersion medium, takes azo diisobutyronitrile (AIBN) or azo-bis-iso-heptonitrile (AVBN) below 6 wt percent (based on the concentration of the monomer styrene) as initiating agent, takes 1 to 50 wt percent (based on the concentration of the monomer styrene) of periston (PVP) as dispersing agent, and takes divinyl benzene below 60 wt percent (based on the concentration of the monomer styrene) as the dispersion polymerization system of cross linking agent, the cross linking degree of the prepared polymer microspheres can reach 60 wt percent, the swelling ratio is 1.02, and the mass loss is only 1.77 wt percent after Soxhlet extraction. The thermogravimetric analysis result shows that the prepared polymer microspheres have good thermal stability, the mass loss is 5 percent, and the thermal decomposition temperature is above 344 DEG C.

Description

technical field [0001] The invention belongs to the field of micro-nano functional materials, and relates to a method for preparing high-crosslinking and monodisperse polymer microspheres with good solvent resistance and thermal stability. Background technique [0002] Since Vanderhoff and Brodford of the Institute of Emulsion Polymer Research of Lehigh University in the United States announced the preparation method of highly uniform polystyrene microspheres in 1955, polymer microspheres have become a new research field. Monodisperse polymer microspheres have special properties such as small size, large specific surface area, special shape (spherical), monodispersity, strong adsorption, and enrichment of surface functional groups. As functional polymer materials, they have great potential in many fields. Widely used, such as quantitative reference material, biomedical detection, packing material of high performance liquid chromatography, catalyst carrier, information storag...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F4/04C08F2/44C08F2/04
Inventor 佟斌曹茉莉支俊格董宇平孙洪波石建兵赵玮申进波
Owner BEIJING INSTITUTE OF TECHNOLOGYGY