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Method for preparing monodisperse polymer microspheres

A polymer, monodisperse technology, applied in the field of preparation of monodisperse polymer microspheres, can solve the problems of complicated steps, difficult control, polydispersity, etc. The effect of mass and heat transfer

Inactive Publication Date: 2012-10-17
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional preparation methods include emulsion polymerization and suspension polymerization, but the former can only prepare particles with a particle size of less than 1 μm, while the polymer microspheres prepared by the latter have a particle size of 100-1000 μm, and the polydispersity
Since the 1970s, scholars at home and abroad have developed many new technologies for synthesizing polymer microspheres, the most important of which is the seed swelling method, which can prepare monodisperse polymer microspheres with a particle size of 1-100 μm as required , but the steps of the seed swelling method are cumbersome, the control is difficult, and the cycle is long

Method used

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  • Method for preparing monodisperse polymer microspheres
  • Method for preparing monodisperse polymer microspheres
  • Method for preparing monodisperse polymer microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh 10g of stabilizer PVP and dissolve it in the system of absolute ethanol and deionized water (732.5g), wherein the mass ratio of absolute ethanol to deionized water is 95:5, stir well and add to the impinging flow reactor, heat up to 70 degrees Celsius; 250g styrene solution (total amount is calculated as 1000g) dissolved with 7.5g initiator AIBN is added to the impingement flow reactor at one time, and the cooling is terminated after reacting at 70 degrees Celsius for 24 hours; then the obtained emulsion is passed through Ultracentrifuge at 5000r / min-7000r / min for centrifugal sedimentation, pour off the supernatant, add absolute ethanol, ultrasonically clean, repeat this several times, and dry the cleaned microspheres at 40-60 degrees Celsius to constant weight , the polystyrene microsphere powder under impinging flow conditions can be obtained; in a series of experiments, while keeping other experimental conditions unchanged, the monomer dosage was increased from ...

Embodiment 2

[0029] Weigh 10g of stabilizer PVP and dissolve it in the system of absolute ethanol and deionized water, wherein the mass ratio of absolute ethanol to deionized water is 95:5, stir evenly and add to the impinging flow reactor, and heat up to 70 degrees Celsius; Add 250g styrene solution (the total amount is 1000g) dissolved with 2.5g initiator AIBN into the impingement flow reactor at one time, react at 70 degrees Celsius for 24h and then cool to terminate; then pass the obtained emulsion through an ultracentrifuge 5000r / min-7000r / min for centrifugal sedimentation, pouring off the supernatant, adding absolute ethanol, ultrasonic cleaning, repeated operations several times, drying the cleaned microspheres at 40-60 degrees Celsius to constant weight, you can get Polystyrene microsphere powder under impinging flow conditions; in a series of experiments, while keeping other conditions unchanged, the amount of initiator AIBN was increased from 2.5g to 10g, and polystyrene microsph...

Embodiment 3

[0032] Weigh 5.0g stabilizer PVP and dissolve it in the system of absolute ethanol and deionized water, wherein the mass ratio of absolute ethanol to deionized water is 95:5, stir evenly and add it to the impinging flow reactor, and heat up to 70 degrees Celsius ; 250g styrene solution (total amount is calculated as 1000g) that is dissolved with 7.5g initiator AIBN is added in the impingement flow reactor at one time, and cooling is terminated after reacting at 70 degrees Celsius for 24 hours; then the obtained emulsion is passed through an ultracentrifuge Centrifugal sedimentation at 5000r / min-7000r / min, pour off the supernatant, add absolute ethanol, ultrasonically clean, repeat the operation several times, and dry the cleaned microspheres at 40-60 degrees Celsius to constant weight. Obtain the polystyrene microsphere powder under impinging flow condition; In a series of experiments, keep other conditions unchanged, the amount of stabilizer is increased from 5.0g to 12.5g, an...

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Abstract

The invention relates to a method for preparing monodisperse polymer microspheres. The method comprises the following process steps: adding a dispersion medium with a stabilizing agent dissolved inside to an impinging stream reactor, heating the dispersion medium, adding a monomer with an initiating agent dissolved inside in one step, carrying out constant-temperature polymerization reaction, obtaining polymer microsphere emulsion after stopping cooling, then using an ultracentrifuge to carry out centrifugal sedimentation, adding absolute ethyl alcohol after removing supernatant, carrying out ultrasonic washing multiple times and drying the washed microspheres to constant weight, thus obtaining the monodisperse polymer microspheres. Compared with the prior art, the method has the following advantages: the prepared polymer microspheres have good apparent morphology, good smoothness and monodispersity and uniform grain sizes; the process is simple to operate; the grain sizes of the microspheres can be well controlled according to the formula; and the grain size range applicability is better.

Description

technical field [0001] The invention belongs to the field of polymer microsphere materials, and in particular relates to a preparation method of monodisperse polymer microspheres. Background technique [0002] Polymer microsphere materials are widely used in chromatographic fillers, analytical chemistry, medical immunity, bioengineering, coatings, microelectronics and other fields. Therefore, the preparation of monodisperse, uniform particle size polymer microspheres is a hot spot in the field of microsphere materials. . [0003] In terms of microsphere preparation technology, the preparation method and preparation system have been gradually improved, and the preparation method of uniform-sized polymer microspheres has basically been established. The traditional preparation methods include emulsion polymerization and suspension polymerization, but the former can only prepare particles with a particle size of less than 1 μm, while the latter prepares polymer microspheres wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F120/14C08F120/18C08F2/01
Inventor 樊庆春吴田段菲红李文胡芽
Owner WUHAN INSTITUTE OF TECHNOLOGY
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