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Preparation method for polymeric nanometer microsphere

A nano-microsphere and polymer technology, which is applied in the field of preparation of polymer nano-microspheres, can solve the problems of complicated post-processing steps, difficulty in obtaining surface-functionalized nano-microspheres, and difficulty in controlling the preparation process, and the method is simple and easy to achieve. performance, improved stability and uniformity, narrow particle size distribution

Active Publication Date: 2014-01-01
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the surface functionalization of nanospheres generally requires chemical reactions related to surface modification or the design of initiators during polymerization. The preparation process is difficult to control, and the post-processing steps are cumbersome. Nanospheres

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  • Preparation method for polymeric nanometer microsphere
  • Preparation method for polymeric nanometer microsphere
  • Preparation method for polymeric nanometer microsphere

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preparation example Construction

[0028] The embodiment of the present invention discloses a method for preparing polymer nanospheres, comprising the following steps:

[0029] (A) select the trithiocarbonate compound represented by formula (I) as a chain transfer agent, and synthesize a gradient copolymer through RAFT active polymerization;

[0030] (B) dissolving the gradient copolymer in an organic solvent, and then adding water to form a polymer micelle solution; the organic solvent is miscible with water;

[0031] (C) adding the polymer micelle solution to an aqueous solution of an inorganic salt, and performing solvent replacement to obtain polymer nanospheres; the volume ratio of the polymer micelle solution to the aqueous solution of an inorganic salt is 0.01 to 1;

[0032]

[0033] Wherein, Z is a group with a carboxyl group at the end, and R is a leaving group.

[0034] The present invention makes full use of the convenience of the reversible addition-fragmentation chain transfer polymerization (R...

Embodiment 1

[0044] After feeding nitrogen into the dry reactor for 20 minutes, add styrene monomer and RAFT reagent S-1-carboxypropyl-S'-benzyl trithiocarbonate, the monomer and RAFT reagent molar ratio is 300: 1. Please clarify which catalyst is stirred and dissolved, then heat the reactor to 120°C, and after 12 hours of reaction, use a syringe pump to add 2.5 times the equivalent of styrene monomer into the reactor The copolymerization reaction was carried out, and the copolymerization reaction was carried out for 14 hours. Inject 8% of the total amount of methyl methacrylate at a constant speed for the first 6 hours, then inject 65% of methyl methacrylate instantaneously, and inject 27% of methyl methacrylate at a constant speed for the last 8 hours. Purify the polymer. By NMR spectroscopy ( 1 H NMR) and gel permeation chromatography (GPC) to characterize the gradient copolymers. The polymer had a final molecular weight of 47,000, a molecular weight distribution of 1.38, and a methy...

Embodiment 2

[0050] After feeding nitrogen into the dry reactor for 20 minutes, add styrene monomer and RAFT reagent S-1-carboxypropyl-S'-benzyl trithiocarbonate, the monomer and RAFT reagent molar ratio is 300: 1. After stirring and dissolving, heat the reactor to 120°C. After 12 hours of reaction, use a syringe pump to add methyl methacrylate 2.5 times the equivalent of styrene monomer into the reactor for copolymerization. The copolymerization is carried out for 14 hours. Hour. Inject 8% of the total amount of methyl methacrylate at a constant speed for the first 6 hours, then inject 65% of methyl methacrylate instantaneously, and inject 27% of methyl methacrylate at a constant speed for the last 8 hours. After purification, a gradient copolymer was obtained.

[0051] The gradient copolymer was dissolved in tetrahydrofuran at a concentration of 0.5% (w / v), then deionized water was added dropwise under stirring at 300 rpm, and the final water content was 10% (w / w).

[0052] The above-m...

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Abstract

The invention provides a preparation method for a polymeric nanometer microsphere. The preparation method comprises the following steps: with trithiocarbonate represented by a formula (I) as a chain transferring agent, carrying out RAFT living polymerization to synthesize a gradient copolymer; dissolving the gradient copolymer in an organic solvent and then adding water to form a polymeric micelle solution, wherein the organic solvent and water are intermiscible; and adding the polymeric micelle solution into an aqueous solution of an inorganic salt and carrying out solvent displacement so as to obtain the polymeric nanometer microsphere, wherein a volume ratio of the polymeric micelle solution to the aqueous solution of the inorganic salt is 0.01 to 1. The polymeric nanometer microsphere prepared by using the method has good stability and uniformity, narrow particle size distribution and photoresponse characteristics and the surface of the microsphere is rich in carboxyl groups, thereby facilitating application of the polymeric nanometer microsphere as a good carrier for drugs and proteins. Moreover, the method provided by the invention has the advantages of simpleness, easy practicability, good repeatability, low energy consumption, extensive applicability and easy realization of industrialization.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a method for preparing polymer nanospheres. Background technique [0002] Polymer nanospheres refer to polymer microspheres with a size less than 100 nm and uniform distribution. In recent years, due to the application value of polymer nanospheres in electronic device engineering, biomedical engineering, especially nanomedicine such as drug carriers, immunodiagnosis and other fields, their preparation methods have attracted much attention. [0003] Polymerization by monomer is a common means to prepare polymeric microspheres. However, in many fields of nanomedicine, it is generally required that the nano-microsphere system does not contain small molecular impurities such as surfactants and the particle size is less than 100nm. Soap-free emulsion polymerization and precipitation polymerization are generally used to prepare monodisperse microspheres with a size larger than 100 na...

Claims

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Application Information

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IPC IPC(8): C08J3/14C08F220/14C08F212/08C08F2/38C08F220/18C08F226/06
Inventor 郑超黄海瑛何天白
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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