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A method for preparing micron-sized monodisperse polymer microspheres at room temperature

A monodisperse microsphere, micron-scale technology, applied in the direction of microsphere preparation, microcapsule preparation, etc., can solve the problems of limited application and difficult removal, and achieve the effect of simple and reliable method, short time consumption and high yield of microspheres

Inactive Publication Date: 2019-05-10
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the preparation process of this method, polyvinylpyrrolidone needs to be added as a stabilizer and catalyst, which is difficult to remove after polymerization, which limits the application of this method in biomedicine

Method used

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  • A method for preparing micron-sized monodisperse polymer microspheres at room temperature
  • A method for preparing micron-sized monodisperse polymer microspheres at room temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1560 μL of toluene diisocyanate and 2365 μL of trimethylolpropane tris(3-mercaptopropionate) were added to 10 mL of triethylamine in acetonitrile solution at a concentration of 0.00158 g / L, and mixed well; then the two parts of the solution Put it in a reaction container and mix it evenly, seal it; let it stand at room temperature for 2 hours to react; the obtained product is washed successively with acetone and n-hexane, centrifugally precipitated, and vacuum-dried to obtain monodisperse microspheres. The average particle size of the obtained product is 2.259 μm, the polydispersity coefficient is 1.049, and the yield of microspheres is 98.7% ( figure 1 ).

Embodiment 2

[0032] 1025 μL of toluene diisocyanate and 1580 μL of trimethylolpropane tris(3-mercaptopropionate) were added to 10 mL of triethylamine in acetonitrile solution at a concentration of 0.00105 g / L, and mixed well; then the two parts of the solution Put it in a reaction container and mix it evenly, seal it; let it stand at room temperature for 2 hours to react; the obtained product is washed successively with acetone and n-hexane, centrifugally precipitated, and vacuum-dried to obtain monodisperse microspheres. The average particle size of the obtained product was 2.259 μm, the polydispersity coefficient was 1.023, and the yield of microspheres was 96.6%.

Embodiment 3

[0034] 1085 μL of toluene diisocyanate and 1517 μL of trimethylolpropane tris(3-mercaptopropionate) were added to 10 mL of triethylamine in acetonitrile solution at a concentration of 0.00107 g / L, and mixed well; then the two parts of the solution Put it in a reaction container and mix it evenly, seal it; let it stand at room temperature for 2 hours to react; the obtained product is washed successively with acetone and n-hexane, centrifugally precipitated, and vacuum-dried to obtain monodisperse microspheres. The average particle size of the obtained product was 2.263 μm, the polydispersity coefficient was 1.034, and the yield of microspheres was 97.2%.

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Abstract

The invention relates to a method for preparing a micron monodisperse polymeric microsphere under a room temperature condition. According to the invention, the monodisperse polymeric microsphere is prepared by utilizing the reaction of mercaptan and isocyanate through precipitation polymerization without surface active agent or stabilizer. The method comprises the following steps: uniformly mixing mercaptan monomer with isocyanate monomer; under an effect of a basic catalyst, standing by and reacting for 1-8 hours under room temperature; washing the acquired product with a solvent; centrifugally precipitating; drying, thereby acquiring the monodisperse polymeric microsphere. The preparation method provided by the invention is simple and reliable; the reaction is performed under the room temperature; no sealing or stirring is required; the time consumption is short; the monomer dosage is large; the microsphere yield is high.

Description

technical field [0001] The invention relates to a method for preparing micron-sized monodisperse polymer microspheres at room temperature, and belongs to the technical field of polymer materials. Background technique [0002] Micron-sized monodisperse polymer microspheres have been used in biomedicine, enzyme immobilization, liquid crystal display, dyes, photonic crystals, and chromatographic separation, and have broad application prospects. [0003] At present, the preparation methods of micron-sized monodisperse polymer microspheres mainly include emulsion polymerization, seed swelling polymerization, dispersion polymerization, precipitation polymerization, glass membrane emulsification and microfluidic technology. In addition to precipitation polymerization, the above methods all need to add certain stabilizers or dispersants and other related additives. These components are difficult to remove, which limits the application of microspheres in biomedicine and other fields....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/76C08G18/38B01J13/14
CPCB01J13/14C08G18/3876C08G18/7614
Inventor 孔祥正郭峰豪陈志勇
Owner UNIV OF JINAN
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