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Method for preparing monodisperse submicron polystyrene spheres by intermediate-and low-temperature solvent thermal process

A technology of low-temperature solvothermal method and polystyrene balls, which is applied in the direction of pharmaceutical formulations, medical preparations of non-active ingredients, etc., can solve the problem of narrow particle size control range, large particle size, and increased difficulty in particle separation and purification and other problems, to achieve the effect of good monodispersity, simple preparation process, and easy mass production and scale-up

Active Publication Date: 2014-06-04
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the particle size distribution obtained by suspension polymerization and emulsion polymerization is wide, which is not suitable for preparing nanostructure materials as template materials, and its application in standard standards and biopharmaceuticals is also limited; the preparation of soap-free emulsion polymerization and seed swelling method Although polymer particles have good size monodispersity, there are shortcomings such as narrow particle size control range, harsh reaction conditions, time-consuming purification process, and energy consumption (soap-free emulsion polymerization and seed swelling method).
Dispersion polymerization is a special kind of precipitation polymerization carried out in an alcohol system. During the dispersion polymerization process, the particle size and distribution of the product are not as sensitive to the change of reaction parameters as soap-free emulsion polymerization, and the functional groups on the surface of the particles and the interface electricity The performance can also be adjusted, and the surface of the obtained particles is relatively smooth; in addition, compared with other methods, the degree of ionization of the functional groups on the surface of the particles is lower, and the electrostatic repulsion between the particles is smaller, which makes the separation and purification of the particles more difficult. Although the dispersion polymerization method has certain advantages in the preparation of monodisperse polymer particles, the particle size is often large (1-20 μm), which greatly limits the application range of the prepared monodisperse polymer particles.
When adopting the dispersion polymerization method to prepare polystyrene microspheres, the reaction is usually carried out in an open system, and an inert gas is required to discharge the air in the system, and the entire reaction process needs to be carried out under the protection of an inert gas to avoid Dissolved oxygen inhibits the polymerization of styrene monomer, and this method tends to have larger particle sizes of styrene microspheres due to the slower nucleation rate

Method used

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  • Method for preparing monodisperse submicron polystyrene spheres by intermediate-and low-temperature solvent thermal process
  • Method for preparing monodisperse submicron polystyrene spheres by intermediate-and low-temperature solvent thermal process
  • Method for preparing monodisperse submicron polystyrene spheres by intermediate-and low-temperature solvent thermal process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Concentration is that the styrene (St) monomer of 0.063mol / L is dissolved in the ethanol and the water mixed solution that mass ratio is 4 / 1, stirs, in solution, add the PVP that concentration is 5.0g / L as stabilizer, and Stir until the solution is clear, then add AIBA with 1% of the monomer mass as an initiator, and stir until it is completely dissolved; then transfer the resulting solution to a high-pressure reaction kettle, and put the kettle into an oven to maintain at 80°C After 5 hours, cool naturally in the air to room temperature, centrifuge the white emulsion in the kettle, disperse it with absolute ethanol and then centrifuge it, repeat this cycle for 3 times, and vacuum-dry the obtained solid in a vacuum oven at 50°C to obtain the product. Its scanning electron microscope picture is figure 1, The particle size is 112nm, and the dispersion coefficient σ is 12.5%.

Embodiment 2

[0043] Concentration is that the styrene (St) monomer of 0.1mol / L is dissolved in the ethanol and water mixed solution that mass ratio is 4 / 1, stirs, and in solution, add the PVP that concentration is 5.0g / L as stabilizer, and Stir until the solution is clear, then add AIBA with 1% of the monomer mass as an initiator, and stir until it is completely dissolved; then transfer the resulting solution to a high-pressure reaction kettle, and put the kettle into an oven to maintain at 80°C After 5 hours, cool naturally in the air to room temperature, centrifuge the white emulsion in the kettle, disperse it with absolute ethanol and then centrifuge it, repeat this cycle for 3 times, and vacuum-dry the obtained solid in a vacuum oven at 50°C to obtain the product. Its scanning electron microscope picture is figure 2 , The particle size is 225nm, and the dispersion coefficient σ is 5.3%.

Embodiment 3

[0045] Concentration is that the styrene (St) monomer of 0.48mol / L is dissolved in the ethanol and the water mixed solution that mass ratio is 4 / 1, stirs, in solution, add the PVP that concentration is 5.0g / L as stabilizer, and Stir until the solution is clear, then add AIBA with 1% of the monomer mass as an initiator, and stir until it is completely dissolved; then transfer the resulting solution to a high-pressure reaction kettle, and put the kettle into an oven to maintain at 80°C After 5 hours, cool naturally in the air to room temperature, centrifuge the white emulsion in the kettle, disperse it with absolute ethanol and then centrifuge it, repeat this cycle for 3 times, and vacuum-dry the obtained solid in a vacuum oven at 50°C to obtain the product. Its scanning electron microscope picture is image 3 , The particle size is 472nm, and the dispersion coefficient σ is 3.1%.

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Abstract

The invention relates to a method for preparing monodisperse submicron polystyrene spheres by intermediate-and low-temperature solvent thermal process, comprising the following steps: 1) dissolving a styrene monomer in a mixed solution of ethanol and water to obtain a styrene solution with the concentration of 0.063-1.25 mol / L; 2) adding polyvinylpyrrolidone in the styrene solution of the step 1), and then adding 2,2'-azobis (2-amidinopropane) dihydrochloride, stirring until it dissolves to obtain a reaction solution; 3) adding the reaction solution of the step 2) in an airtight container, reacting at 70-120 DEG C and cooling to obtain an emulsion; and 4) carrying out centrifugal separation on the emulsion of the step 3), and drying to obtain the monodisperse submicron polystyrene spheres. The monodisperse submicron polystyrene spheres prepared by using the solvent thermal-assisted dispersion polymerization technology have good monodispersity, uniform size, and high sphericity, and the method has the advantages of fast reaction speed, mild reaction conditions, simple operation, and easiness in mass production.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a method for preparing monodisperse submicron polystyrene spheres by a medium-low temperature solvothermal method. Background technique [0002] Monodisperse polymer particles are used as template materials for the synthesis of many inorganic functional nanostructure materials due to their unique spherical structure, single size distribution and good interfacial reactivity, such as core-shell structure materials and hollow structure spherical materials; They are also used as basic structural units to prepare various nanoporous functional devices, such as periodically arranged photonic crystals and macroporous materials. The development of these fields has greatly broadened the scope of application of monodisperse polymer colloidal particles, and also put forward higher requirements for the size and distribution of polymer colloidal particles, high dispersion and surface reactivit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F112/08C08F2/12A61K47/32
Inventor 陈运法武晓峰廖玉超
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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