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Reversible Complexation Polymerization in Light-Controlled Aqueous Solution and Preparation of Polymer Nanoparticles

A nanoparticle and polymer technology, applied in the field of polymer preparation, achieves the effects of narrow molecular weight distribution, mild reaction conditions and simple polymerization components

Active Publication Date: 2021-03-30
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, how to apply light-controlled RCMP technology to aqueous solution for polymerization has not been reported in the literature.

Method used

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  • Reversible Complexation Polymerization in Light-Controlled Aqueous Solution and Preparation of Polymer Nanoparticles
  • Reversible Complexation Polymerization in Light-Controlled Aqueous Solution and Preparation of Polymer Nanoparticles
  • Reversible Complexation Polymerization in Light-Controlled Aqueous Solution and Preparation of Polymer Nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: the preparation of poly(ethylene glycol monomethyl ether) methacrylate (PPEGMA)

[0048] Massive ratio [PEGMA] 0 / [CP-I] 0 =50 / 1, PEGMA (1.09g, 2.18mmol), CP-I (8.5mg, 0.04mmol), H 2 O (1.0mL), add a 5mL clean ampoule bottle, put a clean stirring bar. The mixed solution is a colorless and transparent homogeneous solution. Place the ampoule bottle in liquid nitrogen to freeze the solution, then pump air for 20-30 seconds, then pass in argon gas, let it thaw and dissolve at room temperature, and undergo three gas replacements. , remove the oxygen in the ampoule, and make it under argon atmosphere, quickly move the ampoule to the nozzle of the spray gun, and seal the ampoule with an outer flame. Place the sealed ampoule on the pre-installed blue LED light strip (wavelength 464nm, 15mW / cm 2 ) in the lamp tray, a stirrer is placed at the bottom of the tray, and an electric fan is placed next to the lamp tray to keep the polymerization temperature at room te...

Embodiment 2

[0050] Embodiment 2: Preparation of polymer nanoparticles PPEGMA-b-PBnMA (chain extension experiment)

[0051] Massive ratio [PEGMA] 0 / [CP-I] 0 =10 / 1, PEGMA (0.55g, 1.09mmol), CP-I (19.1mg, 0.11mmol), H 2 O (1.0mL), put into a 5mL clean ampoule bottle, put a clean stirring bar, according to the conditions of Example 1, in an argon protective atmosphere, after reacting for 6h under the same light conditions, the tube was broken , take out a certain amount of reaction solution and leave it for testing, then use the obtained PPEGMA as a macromolecular initiator, directly mix BnMA (0.37mL, 2.18mmol), H 2 O (3.50 mL) was mixed with the reaction, transferred to a new ampoule, and the ampoule was placed under argon atmosphere and sealed with a flame. Let the sealed ampoule continue to light up under the blue LED light strip (wavelength 464nm, 15mW / cm 2 ) reaction under irradiation. At first, the oil-soluble BnMA was incompatible with the polymerization system. After a certain p...

Embodiment 3

[0055] Embodiment 3: kinetic experiment

[0056] Massive ratio [PEGMA] 0 / [CP-I] 0 =50 / 1, PEGMA (1.09g, 2.18mmol), CP-I (8.5mg, 0.04mmol), H 2 O (1.0mL), add a 5mL clean ampoule bottle, put a clean stirring bar. The mixed solution is a colorless and transparent homogeneous solution. Place the ampoule bottle in liquid nitrogen to freeze the solution, then pump air for 20-30 seconds, then pass in argon gas, let it thaw and dissolve at room temperature, and undergo three gas replacements. , remove the oxygen in the ampoule, and make it under argon atmosphere, quickly move the ampoule to the nozzle of the spray gun, and seal the ampoule with an outer flame. By measuring the conversion rate of monomer under different reaction times (6h, 8h, 12h, 16h, 24h), obtain as follows Figure 4 The polymerization kinetics diagram shown. Figure 4 In (a), from right to left, the polymerization time increases sequentially, and the molecular weight and molecular weight distribution correspo...

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Abstract

The invention relates to a visible light induced iodine-regulation reversible deactivated radical polymerization method of water-soluble monomers in a water solution and a preparation method of polymernano particles. The reversible deactivated radical polymerization method comprises the following steps: in a protective atmosphere, water-soluble methacrylate monomers and an alkyl iodide initiator are added into water; a reaction is carried out at 20-30 DEG C, wherein the light wavelength to be 390-590 nm; a water-soluble methyl acrylate polymer is obtained after the reaction is completed; and oil-soluble methacrylate monomers are added for carrying out a chain extension reaction, so that an amphiphilic block copolymer is obtained, and the amphiphilic block copolymer can be subjected to in-situ self-assembly in the water solution to form spherical micelle nanoparticles. According to the invention, polymerization is directly carried out in water, polymerization components are simple, polymerization conditions are mild, and polymerization of the methacrylate monomers and preparation of the polymer nano particles can be realized without additional catalysts. The molecular weight distribution of the prepared polymer is narrow, the stable spherical polymer nano particles are obtained, and the polymerization process has a characteristic of active free radical polymerization.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to the reversible complexation polymerization of light-controlled aqueous solution and the preparation of polymer nanoparticles. Background technique [0002] In recent years, the RDRP (Reversible Deactivation Radical Polymerization) method has developed rapidly and has become a powerful tool for the synthesis of polymers with specific structures and designable molecular weights. So far, various RDRP methods such as nitroxide-stabilized living radical polymerization (NMP), atom transfer radical polymerization (ATRP), reversible addition-fragmentation chain transfer (RAFT) polymerization, and reversible complexation polymerization (RCMP) have been An efficient way to prepare "living" polymers. RCMP is a RDRP technology that regulates the concentration of free radicals through the reversible complexation of alkyl iodides and external organic amines, NaI, iodine salts and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/28C08F2/48C08F2/10C08F293/00
CPCC08F2/10C08F2/48C08F120/28C08F293/005C08F2438/00
Inventor 程振平倪媛媛张丽芬朱秀林
Owner SUZHOU UNIV