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A method for preparing monodisperse cross-linked polymer microspheres with high yield

A cross-linked polymer, monodisperse technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of long polymerization time, monomer conversion rate and low yield of microspheres, etc. Yield improvement, high cross-linking effect

Inactive Publication Date: 2019-03-15
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problems of low monomer dosage, monomer conversion rate, microsphere yield and long polymerization time in the preparation of monodisperse cross-linked polymer microspheres in the prior art, the present invention provides a rapid and high-yield preparation of monodisperse cross-linked polymer microspheres. A method for dispersing cross-linked polymer microspheres; that is, using acetonitrile or water and acetonitrile as a solvent, using polyamine or polyol as a cross-linking monomer to react with diisocyanate to prepare monodisperse cross-linked polymer microspheres by precipitation polymerization

Method used

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  • A method for preparing monodisperse cross-linked polymer microspheres with high yield
  • A method for preparing monodisperse cross-linked polymer microspheres with high yield
  • A method for preparing monodisperse cross-linked polymer microspheres with high yield

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Experimental program
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Effect test

Embodiment 1

[0040] At room temperature, first add 90.0g of water / acetonitrile mixed solvent with a mass ratio of 25 / 75 to a 120mL glass reaction bottle, then add 2.48g of triethylenetetramine and 7.52g of isophorone diisocyanate respectively, and shake it evenly The reaction bottle was sealed and placed in a constant temperature water bath at 30°C. After 4 minutes of reaction, the system became cloudy, and then continued to react for 0.5 hours. After the reaction, the product was centrifuged with a high-speed centrifuge at 8,000 rpm for 5 minutes, the microspheres were washed twice with acetonitrile, and then dried in an oven at 100°C for 5 hours to obtain monodisperse cross-linked polyurea microspheres.

[0041] The obtained polyurea is 100% cross-linked, and the yield of polyurea microspheres is 88.23%. Scanning electron microscope pictures of microspheres as figure 1 As shown, the average particle size of the microspheres thus measured was 4.5 μm, and the polydispersity coefficient o...

Embodiment 2

[0043] Add 80.0g of acetonitrile to a 120mL glass reaction bottle at room temperature, then add 5.91g of triethylenetetramine and 14.09g of toluene diisocyanate respectively, shake evenly, seal the reaction bottle and place it in a constant temperature water bath at 30°C. After 10 minutes of reaction, the system became cloudy, and then continued to react for 1 hour. After the reaction, the product was centrifuged with a high-speed centrifuge at 8,000 rpm for 5 minutes, the microspheres were washed twice with acetonitrile, and then dried in an oven at 100°C for 5 hours to obtain monodisperse cross-linked polyurea microspheres.

[0044] The obtained polyurea is 100% cross-linked, and the yield of polyurea microspheres is 93.51%. The average particle size of the microspheres is 8.5 μm, and the polydispersity coefficient of the particle size is 1.007.

Embodiment 3

[0046] At room temperature, first add 75.0g of water / acetonitrile mixed solvent with a mass ratio of 10 / 90 to a 120mL glass reaction bottle, and then add 5.75g of triethylenetetramine and 19.25g of isophorone diisocyanate respectively, and shake it evenly The reaction bottle was sealed and placed in a constant temperature water bath at 70°C. After 3 minutes of reaction, the system became cloudy, and then continued to react for 0.5 hours. After the reaction, the product was centrifuged with a high-speed centrifuge at 8,000 rpm for 5 minutes, the microspheres were washed twice with acetonitrile, and then dried in an oven at 100°C for 5 hours to obtain monodisperse cross-linked polyurea microspheres.

[0047] The cross-linked product in the obtained polyurea accounts for 97.4%, and the yield of polyurea microspheres is 94.84%. The average particle size of the microspheres is 9.5 μm, and the polydispersity coefficient of the particle size is 1.008.

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Abstract

The invention relates to a method for preparing monodisperse crosslinked polymer microsphere with high yield. Taking acetonitrile or mixed solvent of water and acetonitrile as the reaction medium, with diisocyanate compounds and polyhydric alcohols or polyamine as monomer, precipitation polymerization is made in static conditions without stirring, following by centrifugal separation, washing and frying of the product to obtain monodisperse crosslinked polymer microspheres. The invention has short reaction time, high monomer loading capacity and microspheres yield, which is helpful in scale production of monodisperse microspheres. The polymer from the invention is highly crosslinked, and the microspheres have high solvent resistance and heat resistance. At the same time, monodisperse microspheres are prepared without any stabilizer and initiator. After the polymerization is completed, the monomer is completely transformed and the resulting microspheres are very clean, which can be applied to chromatographic analysis, protein adsorption and separation and other fields.

Description

technical field [0001] The invention relates to a method for preparing monodisperse polymer microspheres, in particular to a method for preparing monodisperse crosslinked polymer microspheres with high yield, and belongs to the field of functional polymer materials. Background technique [0002] Monodisperse polymer microspheres refer to polymer spherical particles with diameters ranging from nanometers to micrometers and highly consistent particle sizes. Cross-linked polymers have a three-dimensional network structure, and compared with linear polymers, they have higher mechanical strength, thermal stability, abrasion resistance, solvent resistance and creep resistance. Due to the excellent properties of cross-linked polymers, cross-linked polymer microspheres have higher application value than linear polymer microspheres, and are widely used in chromatographic analysis, liquid crystal display, drug controlled release, enzyme immobilization, photonic crystals and other fiel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/32C08G18/75C08G18/76B01J13/14
CPCB01J13/14C08G18/3206C08G18/3228C08G18/755C08G18/7614
Inventor 姜绪宝孔祥正朱晓丽
Owner UNIV OF JINAN
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