Method for preparing micro-sized monodisperse polyurea microsphere in static condition

A micron-scale, monodisperse technology, applied in the preparation of micron-scale monodisperse polymer microspheres, the field of preparation of micron-scale monodisperse polyurea microspheres, can solve the problem of low monomer conversion rate and microsphere yield, monodisperse microspheres Problems such as low production efficiency of spheres and continuous operation of equipment are needed to achieve the effects of high complete conversion of monomers, fast polymerization reaction rate and low cost

Inactive Publication Date: 2012-10-03
UNIV OF JINAN
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Problems solved by technology

[0004] At present, the preparation of polymer monodisperse microspheres by precipitation polymerization is based on the mechanism of free radical polymerization, which requires stirring or shaking. The amount of monomer used during polymerization generally does not exceed 2.0%, and the polymerization time is relatively long, generally 12~24h. Both monomer conversion rate and microsphere yield are low, resulting in extremely low preparation efficiency of polymer monodisperse microspheres and a large amount of residual monomer in the system after the polymerization is completed; stirring or shaking the polymerization system generally requires a special mixer or Oscillators have strict requirements on the material and shape of the agitator
The equipment required for stirring or shaking increases the production cost, and the equipment needs to work continuously during the polymerization process, which consumes a lot of energy

Method used

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  • Method for preparing micro-sized monodisperse polyurea microsphere in static condition
  • Method for preparing micro-sized monodisperse polyurea microsphere in static condition
  • Method for preparing micro-sized monodisperse polyurea microsphere in static condition

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Experimental program
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Effect test

Embodiment 1

[0039] At room temperature, first add 98.0 g of water / acetone mixed solvent with a mass ratio of 30 / 70 to a 120 mL glass reaction bottle, shake well and then add 2.0 g of 4,4′-dicyclohexylmethane diisocyanate (CAS No.: 5124-30-1) monomer, seal the reaction bottle, shake it well and put it in a constant temperature water bath at 30°C. After 80 minutes of reaction, the system starts to become cloudy, and then continue to react for 2 hours. After the reaction, take a certain amount of sample and add it to a centrifuge tube, centrifuge at 12000r / min for 5min with a high-speed centrifuge, take out the supernatant, wash the microspheres twice with acetone, and then dry them in an oven at 85°C for 10h Polyurea microspheres were obtained.

[0040] The productive rate of gained polyurea microsphere is 68.11%, and the average particle diameter of microsphere is 1.923 μ m, and the polydispersity coefficient of particle diameter is 1.028, and its scanning electron micrograph is as follows...

Embodiment 2

[0042] Add 98.0g of water / acetone mixed solvent with a mass ratio of 30 / 70 to a 120mL glass reaction bottle at room temperature, shake well and then add 2.0g of 1,6-hexamethylene diisocyanate (CAS No.: 822-06- 0) monomer, seal the reaction bottle, shake it well and put it in a constant temperature water bath with a temperature of 30°C. After 75 minutes of reaction, the system starts to become cloudy, and then continue to react for 2 hours. After the reaction, take a certain amount of sample and add it to a centrifuge tube, centrifuge at 12000r / min for 5min with a high-speed centrifuge, take out the supernatant, wash the microspheres twice with acetone, and then dry them in an oven at 85°C for 10h Polyurea microspheres were obtained.

[0043] The productive rate of gained polyurea microsphere is 69.43%, and the average particle diameter of microsphere is 2.101 μ m, and the polydispersity coefficient of particle diameter is 1.035, and its scanning electron micrograph is as follo...

Embodiment 3

[0045] At room temperature, first add 91.0 g of water / acetone mixed solvent with a mass ratio of 24 / 76 to a 120 mL glass reaction bottle, shake well and then add 9.0 g of isophorone diisocyanate (CAS No.: 4098-71-9 ), the reaction bottle was sealed and shaken evenly and placed in a constant temperature water bath at a temperature of 30°C. After 85 minutes of reaction, the system began to become cloudy, and then continued to react for 2 hours. After the reaction, take a certain amount of sample and add it to a centrifuge tube, centrifuge at 12000r / min for 5min with a high-speed centrifuge, take out the supernatant, wash the microspheres twice with acetone, and then dry them in an oven at 85°C for 10h Polyurea microspheres were obtained.

[0046] The productive rate of gained polyurea microsphere is 88.39%, and the average particle diameter of microsphere is 8.425 μ m, and the polydispersity coefficient of particle diameter is 1.007, and its scanning electron micrograph is as fo...

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Abstract

The invention relates to a method for preparing micro-sized monodisperse polymer microspheres in static condition. The method comprises the steps that diisocyanate monomers and a water-acetone mixed solvent are added into a reaction bottle, wherein the mass ratio of water to acetone ranges from 20/80 to 60/40, and the diisocyanate compound accounts for 0.5-13.0% of the total mass of the polymerization system; after the reaction bottle is sealed and the mixed solvent is shaken up, the reaction bottle is placed in thermostatic waterbath of 20-80 DEG C for polymerization; after polymerization, the products are centrifugalized and dried to obtain the micro-sized monodisperse polyurea microspheres. The method for preparing micro-sized monodisperse polymer microspheres in static condition has the advantages that one monomer is used for precipitation polymerization completely in static condition without any stirring or oscillation, so that the reaction time is short, the monomer can be transformed completely, the yield of microspheres is high, and the operation is simple; the method is conducive to scale production of monodisperse microspheres; and the produced microspheres have clean surfaces and a large amount of amido, and can be used in various fields of protein adsorption and separation, enzyme immobilization, chromatographic analysis and the like..

Description

technical field [0001] The invention relates to a method for preparing micron-sized monodisperse polymer microspheres, in particular to a method for preparing micron-sized monodisperse polyurea microspheres under standing conditions, and belongs to the field of functional polymer materials. Background technique [0002] Polymer monodisperse microspheres have become an important research content in the field of polymer science because of their important application value in standard metering, chromatographic analysis, enzyme immobilization, drug controlled release, liquid crystal display, photonic crystal and many other fields. The traditional methods for preparing polymer monodisperse microspheres include suspension polymerization, dispersion polymerization, emulsion polymerization, and glass membrane emulsification and post-polymerization techniques. All these methods must use surfactants or stabilizers in the preparation process, which seriously restricts the application o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/75C08G18/73C08G18/30
Inventor 孔祥正姜绪宝朱晓丽
Owner UNIV OF JINAN
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