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Method for synthesizing monodisperse polymer microspheres in a pure water medium

A polymer and monodisperse technology, which is applied in the field of synthesizing monodisperse polymer microspheres, can solve problems such as nucleation is easily disturbed, restricted, and microspheres are uneven, and achieve the effect of no pollution to the environment and avoiding impact

Active Publication Date: 2021-09-28
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing polymer microsphere synthesis systems mainly include emulsion polymerization, suspension polymerization and dispersion polymerization. Among them, emulsion polymerization can use pure water as the medium, but emulsion polymerization requires the use of emulsifiers, and the particle size control of microspheres is inflexible; suspension polymerization Pure water can also be used as the medium, but the particle size uniformity of the obtained microspheres is poor
Dispersion polymerization, as a mature polymer microsphere synthesis system, can synthesize monodisperse microspheres with a particle size of 0.1-15 mm. It has also been reported to prepare microspheres by dispersion polymerization in aqueous medium, but because the polymerization reaction requires heating conditions The reaction time is up to 24 hours, these conditions are limited in some biological applications
Moreover, since dispersion polymerization has special requirements on the solubility of monomers and polymers (monomers need to be dissolved in the dispersion medium, and polymers must be precipitated when they reach a certain chain length), when using aqueous media, the temperature has a great impact on the monomers. And the solubility of the polymer is particularly obvious, often resulting in uneven microspheres, or even no microspheres
The photoinitiation system can make the dispersion polymerization proceed rapidly at room temperature, but because the reaction speed is too fast, the nucleation is easily disturbed, and the growing microspheres cannot be stabilized in time, so it is difficult to obtain monodisperse microspheres

Method used

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  • Method for synthesizing monodisperse polymer microspheres in a pure water medium
  • Method for synthesizing monodisperse polymer microspheres in a pure water medium
  • Method for synthesizing monodisperse polymer microspheres in a pure water medium

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Embodiment 1

[0027] Embodiment 1 The method for synthesizing monodisperse polymer microspheres in a kind of pure water medium

[0028] Under normal temperature nitrogen atmosphere, 18g deionized water, 2.0g HPMA monomer (10wt% relative to the reaction system), 0.30g PVP (15% relative to the monomer), 0.005g BDMAT (0.25wt% relative to the monomer) , 0.040g Darocur1173 photoinitiator (2wt% with respect to monomer) and the sodium acetate (0.5wt% with respect to reaction system) of 0.10g add in the 50mL single-necked flask, magnetic stirring is even, then with ultraviolet light (ultraviolet light electrodeless lamp , the radiation wavelength is 365nm, and the light intensity is 50mW / cm 2 ) was irradiated from above the reactor for 4h. The reaction product was washed with deionized water after centrifugation, repeated 2-3 times, and then dried in a vacuum oven to obtain a white powder (ie, polymer microspheres). The conversion rate was calculated by the gravimetric method, and the yield was gr...

Embodiment 2

[0029] A method for synthesizing monodisperse polymer microspheres in a pure water medium in embodiment 2

[0030] Under a nitrogen atmosphere at room temperature, 18g deionized water, 1.0g HPMA monomer (5wt% relative to the reaction system), 0.20g PVP (10% relative to the monomer), 0.005g BDMAT (0.25wt% relative to the monomer) , 0.040g Darocur1173 photoinitiator (2wt% with respect to monomer) and the sodium acetate (0.5wt% with respect to reaction system) of 0.10g add in the 50mL single-necked flask, magnetic stirring is even, then with ultraviolet light (ultraviolet light electrodeless lamp , the radiation wavelength is 365nm, and the light intensity is 30mW / cm 2 ) was irradiated from above the reactor for 4h. The reaction product was washed with deionized water after centrifugation, repeated 2-3 times, and then dried in a vacuum oven to obtain a white powder (ie, polymer microspheres). The conversion rate was calculated by the gravimetric method, and the yield was greater...

Embodiment 3

[0031] A method for synthesizing monodisperse polymer microspheres in a pure water medium in embodiment 3

[0032] Under normal temperature nitrogen atmosphere, 18g deionized water, 2.0g HPMA monomer (10wt% relative to the reaction system), 0.30g PVP (15% relative to the monomer), 0.005g BDMAT (0.25wt% relative to the monomer) , 0.060g Darocur1173 photoinitiator (3wt% with respect to monomer) and the sodium acetate (1wt% with respect to reaction system) of 0.20g add in the 50mL single-necked flask, stir evenly with magnetic force, then use ultraviolet light (ultraviolet light electrodeless lamp, The radiation wavelength is 365nm, and the light intensity is 0.5mW / cm 2 ) was irradiated from above the reactor for 4h. The reaction product was washed with deionized water after centrifugation, repeated 2-3 times, and then dried in a vacuum oven to obtain a white powder (ie, polymer microspheres). The conversion rate was calculated by the gravimetric method, and the yield was greater ...

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Abstract

The invention belongs to the technical field of polymer microsphere preparation, and specifically relates to a method for synthesizing monodisperse polymer microspheres in a pure water medium. A reversible chain transfer agent and a photoinitiator enable the present invention to prepare polymer microspheres with uniform particle size distribution in pure water and low temperature conditions. On the one hand, it can avoid the problem of inability to form microspheres because the solubility characteristics of the monomer and the resulting polymer in water will be affected by temperature factors, and on the other hand, it also solves the problem that it is difficult to form monodisperse microspheres due to nucleation and growth too fast. question. at the same time. Since the present invention uses water instead of organic solvents as the dispersion medium, the influence of organic solvents on biological drugs can be avoided, and there is no pollution to the environment. In addition, since the present invention does not require heating, it is also beneficial to the synthesis of microspheres with biomedical loads.

Description

technical field [0001] The invention belongs to the technical field of polymer microsphere preparation, and in particular relates to a method for synthesizing monodisperse polymer microspheres in a pure water medium. Background technique [0002] Biological and medical technologies often require the use of polymer microspheres as carriers, such as biomolecular recognition, targeted drug delivery, drug sustained release, etc. In these application fields, the preparation process of microspheres often needs to be carried out in a non-organic solvent medium, and the synthesis process also needs to avoid excessively high temperatures, so as not to cause denaturation of biomedical components under the influence of organic solvents. Existing polymer microsphere synthesis systems mainly include emulsion polymerization, suspension polymerization and dispersion polymerization. Among them, emulsion polymerization can use pure water as the medium, but emulsion polymerization requires th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/20C08F2/38C08F2/48A61K9/16A61K47/32
CPCA61K9/1635A61K47/32C08F2/38C08F2/48C08F120/20
Inventor 曾兆华周慧敏杨建文
Owner SUN YAT SEN UNIV
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