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Method for synthesizing micron grade polymer microsphere by suspension polymerization

A suspension polymerization method, suspension polymerization technology, applied in the field of suspension polymerization synthesis of micron-sized polymer microspheres, can solve the problems of harsh reaction conditions, complicated preparation process, purity of polymerization products and troublesome post-processing, etc., to achieve monodispersity and shape Good, simple post-processing, effective in solving pollution

Inactive Publication Date: 2006-07-19
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Synthesizing monodisperse polymer microspheres is very difficult, the reaction conditions are harsh, the preparation process is complicated, and the reaction control requirements are extremely strict
The traditional synthesis methods of polymer microspheres include emulsion polymerization and suspension polymerization. The emulsion polymerization can only prepare microspheres smaller than 500nm. Although the microspheres prepared by the suspension polymerization method have a particle size of 100-1000μm, they are polydisperse. Yes, it is difficult to obtain monodisperse microspheres even after multiple sieves. Dispersion polymerization and seed polymerization developed in the 1970s can prepare monodisperse polymer microspheres with a particle size of 1-100 μm. It is a better method for preparing monodisperse polymer microspheres at present, but the reaction medium of dispersion polymerization needs to use organic solvents such as ethanol, etc., and also needs to add stabilizers such as polyvinylpyrrolidone, etc. cause trouble

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] In a 250ml three-necked flask with stirring, add 5% (wt%) glucose / water solution, styrene monomer 20%, crosslinking agent divinylbenzene 0.3%, initiator azobisisobutyronitrile 0.5%, poly Vinyl alcohol 2% (wt %), heat up to 70 degrees while stirring in a constant temperature water bath, control a certain stirring speed, N 2 After 9 hours of reaction under the atmosphere, it was separated by an ultracentrifuge, and the lower layer of microspheres was washed with ethanol to remove unreacted monomers, separated by ultracentrifugation, and the product was dried at 105 degrees to obtain cross-linked polystyrene microspheres.

Embodiment 2

[0010] In a 250ml three-necked flask with stirring, add 7% (wt%) glucose / water solution, 25% styrene monomer, 0.7% crosslinking agent divinylbenzene, 1% initiator azobisisobutyronitrile, poly Vinyl alcohol 3% (wt %), heat up to 80 degrees while stirring in a constant temperature water bath, control a certain stirring speed, N 2 After 10 hours of reaction under the atmosphere, it was separated by an ultracentrifuge, and the lower layer of microspheres was washed with ethanol to remove unreacted monomers, separated by ultracentrifugation, and the product was dried at 105 degrees to obtain cross-linked polystyrene microspheres.

Embodiment 3

[0012] In a 250ml three-necked flask with stirring, add 10% (wt%) glucose / water solution, 30% styrene monomer, 1% crosslinking agent divinylbenzene, 1.5% initiator azobisisobutyronitrile, poly Vinyl alcohol 4.5% (wt%), in constant temperature water bath, be warmed up to 85 degrees while stirring, control a certain stirring speed, N 2 The reaction was completed after 14 hours under the atmosphere, and then separated by an ultracentrifuge. The lower layer of microspheres was washed with ethanol to remove unreacted monomers, separated by ultracentrifugation, and the product was dried at 105 degrees to obtain cross-linked polystyrene microspheres.

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Abstract

The disclosed synthesis method for micron-level polymer microsphere comprises: using 5-10wt% glucose / water as medium system, 2-4.5wt% polyvinyl alcohol as stabilizer, 20~30wt% styrene, 0.3~1wt% divinylbenzens, and 0.5~1.5wt% azo-diisobutyronitrile; taking the suspension polymerization reaction in N2 atmosphere for 9-14h at 70-85Deg. Wherein, the product has particle size within 10-20nm and dispersion coefficient within 0.020-0.046. This invention simplifies the post-treatment, and solves the pollution of organic solvent efficiently.

Description

technical field [0001] The invention relates to a method for synthesizing micron-sized polymer microspheres by suspension polymerization. Background technique [0002] Synthesizing monodisperse polymer microspheres is very difficult, the reaction conditions are harsh, the preparation process is complicated, and the reaction control requirements are extremely strict. The traditional synthesis methods of polymer microspheres include emulsion polymerization and suspension polymerization. The emulsion polymerization can only prepare microspheres smaller than 500nm. Although the microspheres prepared by the suspension polymerization method have a particle size of 100-1000μm, they are polydisperse. Yes, it is difficult to obtain monodisperse microspheres even after multiple sieves. Dispersion polymerization and seed polymerization developed in the 1970s can prepare monodisperse polymer microspheres with a particle size of 1-100 μm. It is a better method for preparing monodisperse...

Claims

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Application Information

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IPC IPC(8): C08F2/18C08F212/08C08F4/04
Inventor 李红
Owner GUANGDONG UNIV OF TECH
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