Method for preparing micro-sized monodisperse polyuria microspheres

A monodisperse, micron-scale technology, which is applied in the field of high-yield preparation of micron-scale monodisperse polymer microspheres and precipitation polymerization to prepare monodisperse polyurea microspheres, which can solve the problems of long polymerization time, low yield of microspheres, residual monomer Difficult separation and other problems, to achieve the effect of single raw material and simple process

Inactive Publication Date: 2013-10-02
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of various problems such as low monomer content and conversion rate, low microsphere yield, long polymerization time, and difficult separation of residual monomers in the preparation process of the prior art, the present invention provides a high-yield micron-sized monodisperse polyurea microsphere preparation method

Method used

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  • Method for preparing micro-sized monodisperse polyuria microspheres
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  • Method for preparing micro-sized monodisperse polyuria microspheres

Examples

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Effect test

Embodiment 1

[0038] At room temperature, first add 94.0 g of water / acetone mixed solvent with a mass ratio of 3 / 7 to a 120 mL glass reaction bottle, shake well and then add 6.0 g of monomeric isophorone diisocyanate (CAS No.: 4098-71 -9), the reaction bottle was sealed and placed in a constant temperature water bath shaker at a temperature of 30° C., and the system began to become cloudy after reacting at a vibration frequency of 120 times / min for 56 minutes, 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 80°C for 12h Polyurea microspheres were obtained.

[0039] The productive rate of gained polyurea microsphere is 84.21%, and the average particle diameter of microsphere is 9.024 μ m, and the polydispersity coefficient of particle diameter is 1.004, ...

Embodiment 2

[0041] At room temperature, first add 98.4 g of water / acetone mixed solvent with a mass ratio of 3 / 7 to a 120 mL glass reaction bottle, shake well and then add 1.6 g of 4,4′-dicyclohexylmethane diisocyanate (CAS No.: 5124-30-1) monomer, seal the reaction bottle and place it in a constant temperature water bath shaker at a temperature of 30°C. After reacting for 47 minutes at a vibration frequency of 120 times / min, 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 80°C for 12h Polyurea microspheres were obtained.

[0042] The productive rate of gained polyurea microsphere is 60.23%, and the average particle diameter of microsphere is 4.023 μ m, and the polydispersity coefficient of particle diameter is 1.060...

Embodiment 3

[0044] At room temperature, first add 98.4g of water / acetone mixed solvent with a mass ratio of 3 / 7 to a 120mL glass reaction bottle, shake well and then add 1.6g of 1,6-hexamethylene diisocyanate (CAS No.: 822-06- 0) Monomer, seal the reaction bottle and place it in a constant temperature water bath shaker at a temperature of 30°C. After reacting for 45 minutes at a vibration frequency of 120 times / min, 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 80°C for 12h Polyurea microspheres were obtained.

[0045] The productive rate of gained polyurea microsphere is 65.73%, and the average particle diameter of microsphere is 4.192 μ m, and the polydispersity coefficient of particle diameter is 1.015, and its ...

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Abstract

The invention relates to a method for preparing micro-sized monodisperse polyuria microspheres. The method comprises the following steps of: adding a mixed solvent of water and acetone and a diisocyanate compound monomer to a reaction flask at room temperature, wherein the weight ratio of the water to the acetone is 2 / 8-6 / 4, and the diisocyanate compound monomer accounts for 0.5-10.0 percent of the total weight of a mixed system; hermetically shaking up; putting in a constant-temperature water-bath vibrator; performing a polymerization reaction under the conditions that the vibration frequency is 70-150 times per minute and the temperature is 20-80 DEG C; and performing centrifugal separation and drying on a product after polymerization is ended to obtain the micro-sized monodisperse polyuria microspheres. According to the method for preparing the micro-sized monodisperse polyuria microspheres, precipitation polymerization is performed under the vibration condition by using only one monomer, thereby, the process is simple, the raw materials are single, the consumed reaction time is short, the monomer can be completely converted, and the yield of the microspheres can reach at least 86 percent. All the microspheres are clean in surface and contain a large amount of amido and can be used for the field of protein adsorption and separation, enzyme immobilization and chromatographic analysis.

Description

technical field [0001] The invention relates to a method for preparing micron-sized monodisperse polymer microspheres with high yield, in particular to a method for preparing monodisperse polyurea microspheres by precipitation polymerization, which belongs to the field of functional polymer materials. Background technique [0002] Polymer monodisperse microspheres refer to polymer spherical microparticles whose diameters range from nanometers to micrometers and whose particle sizes are highly consistent. Such microspheres have been widely used in liquid crystal display, drug controlled release, chromatographic analysis, enzyme immobilization, photonic crystal and other fields. The traditional methods for preparing monodisperse microspheres include emulsion polymerization, dispersion polymerization, suspension polymerization, glass membrane emulsification and post-polymerization techniques, etc. However, all these methods must use surfactants or stabilizers in the preparatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/02
Inventor 姜绪宝孔祥正朱晓丽
Owner UNIV OF JINAN
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