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A low-temperature synthesis method of monodisperse polymer microspheres

A synthetic method and polymer technology, which is applied in the chemical industry and can solve problems such as denaturation and failure

Active Publication Date: 2015-09-23
HEBEI ZHISHENG GREEN TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention proposes a low-temperature synthesis method of monodisperse polymer microspheres, which solves the problem in the prior art that heat-induced polymerization of polypeptides and proteins and other non-temperature-resistant components are prone to denaturation and failure under long-term heating

Method used

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  • A low-temperature synthesis method of monodisperse polymer microspheres
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  • A low-temperature synthesis method of monodisperse polymer microspheres

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preparation example Construction

[0034] A low-temperature synthesis method of monodisperse polymer microspheres, characterized in that it comprises steps:

[0035] 1) Dissolving the free radical polymerization monomer, stable dispersant, reversible addition-fragmentation chain transfer agent RAFT, and photoinitiator in the reaction medium;

[0036] 2) After introducing nitrogen gas to remove oxygen, under the stirring state, react under light at 0-90° C. to prepare the monodisperse polymer microspheres.

Embodiment 1

[0038] Such as figure 1 and figure 2As shown, the ethanol / water mixture with a mass ratio of 40 / 60 was placed in a quartz reactor as a reaction medium, and then 10% (relative to the reaction medium) methyl methacrylate (MMA) monomer, 15% polyethylene Pyrrolidone (PVP) stabilizer, 0.5% reversible addition-fragmentation chain transfer agent RAFT (BDMAT), 2% 2-hydroxyl-2-methyl-1-phenylacetone-1 (Ciba company trade name is Darocur1173) The photoinitiator is dissolved in the reaction medium. The reaction mixture was purged with nitrogen for 15 minutes to drive off oxygen and then sealed. Under magnetic stirring, the reaction mixture was irradiated from the top of the reactor with an LED light source with a wavelength of 365 nm (power 3 watts) for 3 hours, and then the light source was turned off. The reaction product was precipitated by a centrifuge, the clear liquid was removed, washed several times with the ethanol / water mixture (40 / 60) in the same ratio as the reaction medi...

Embodiment 2

[0042] Such as Figure 4 As shown, the concentration of the reversible addition-fragmentation chain transfer agent RAFT (BDMAT) used in this example is 0.25%, and the rest of the reagents, their dosages, and implementation steps are the same as in Example 1. The yield obtained was 95%. The shape of the product was observed by SEM, and it was a uniform spherical shape. The weight-average diameter (Dw) of all microspheres obtained from the SEM pictures was 1.00m, and the standard deviation rate (CV) was 1.61.

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Abstract

The invention provides a low temperature synthesis method for a monodisperse polymer microsphere. The method includes the steps of 1) dissolving a free radical polymerization monomer, a stable dispersant, a reversible addition-fragmentation chain transfer agent (RAFT) and a photoinitiator in a reaction medium to obtain a mixture; and 2) feeding nitrogen to deoxidize and subjecting the mixture to a light reaction at a temperature between 0 DEG C to 90 DEG C in a stirring state to obtain the monodisperse polymer microsphere. According to the method, on a basis of light dispersion polymerization, a controllable / 'living' radical polymerization mechanism is introduced, and a control reagent of a free radical polymerization is added, so that a photopolymerization which is overquick previously is slowed down, a highly monodisperse polymer microsphere is obtained, and the problem that denaturation and effectiveness losing of heat labile components such as polypeptide and protein caused by a thermal-initiation polymerization under the long time heating in prior art are prone to occur is solved.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a low-temperature synthesis method of monodisperse polymer microspheres. Background technique [0002] Polymer functional microspheres are widely used in biomedicine, electronic information, coating ink, chromatographic separation and other fields. In recent years, with the rapid development of the field of biomedicine, higher requirements have been put forward for the preparation technology of polymer microspheres. [0003] Polymer microspheres can be prepared by methods such as emulsion polymerization, miniemulsion polymerization, microemulsion polymerization, dispersion polymerization, precipitation polymerization, and suspension polymerization. Among them, the dispersion polymerization method is a commonly used microsphere preparation method. Compared with other methods, its main advantage is that microspheres from nanometer to micrometer can be obtained, and the o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/48C08F2/38
Inventor 陈智曾兆华
Owner HEBEI ZHISHENG GREEN TECH
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