Brush copolymer and preparation method thereof

A copolymer and brush-shaped technology, which is applied in the field of preparation of brush-shaped copolymers, can solve problems such as poor uniformity of brush-shaped polymers, unclear structural components, and limited application development, and achieve good uniformity, clear structure and composition , good control effect

Active Publication Date: 2019-11-12
SUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the synthesis of brush-shaped copolymers with well-defined structure and composition and narrow molecular weight distribution is still a challenging work in the field of polymer synthesis
For the synthesis of brush copolymers by anionic polymerization, there are still many problems that limit its further development
On the one hand, the use of negative ion polymerization to synthesize topological polymers with complex structures requires a relatively complex device structure, and the time period for designing and firing devices is relatively long.
On the other hand, the selectivity of anionic polymerization to functional monomers is strong, and the limitations of functional group introduction limit its application development to a certain extent.
For the synthesis of brush copolymers by ring-opening metathesis polymerization, the structural components are less clear and the uniformity of brush polymers is poor

Method used

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  • Brush copolymer and preparation method thereof
  • Brush copolymer and preparation method thereof
  • Brush copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0097] Example 1: Preparation of a brush-shaped copolymer containing polystyrene and polyisoprene

[0098] (1) Preparation of hydroxyl-terminated polystyrene (PS-OH)

[0099] With sec-butyllithium ( sec -BuLi, 1.0 mL, 1.32 mmol) was used as the initiator and benzene (50 mL) was used as the solvent to initiate the living anion polymerization of styrene (8.4 mL, 73.3 mmol) at 25 °C. After 8 hours of reaction, ethylene oxide was added (3.0 mL, 59.4 mmol) for another 0.5 h and terminated with methanol.

[0100] After the reaction, the reaction solution was concentrated by rotary evaporation, precipitated in methanol three times, and then dried in a vacuum oven at 40°C for 24 hours to obtain a white solid powder, which was hydroxyl-terminated polystyrene PS-OH, with a yield of 99%.

[0101] (2) Preparation of norbornene-terminated polystyrene (PS-Nor)

[0102] Weigh PS-OH (2.97 g, 0.74 mmol) and N,N’-diisopropylcarbodiimide (1.53 g, 12.15 mmol), CH 2 Cl 2 (30 mL) was dissolve...

Embodiment 2

[0120] Example 2: Preparation of amphiphilic brush copolymer containing polystyrene and polyethylene glycol

[0121] (1) Preparation of norbornene-terminated polyethylene glycol (PEG-Nor)

[0122] Put the 100 mL branch flask (including stirring bar) and the constant pressure dropping funnel into a blast drying oven at 120°C to dry for 6 h, take them out and put them in a desiccator to cool to room temperature, and then put the whole set of glass devices into the double row Tube. Weigh PEG-OH (1.55 g, 0.78 mmol) and N,N’-diisopropylcarbodiimide (1.57 g, 12.42 mmol) in 30 mL of anhydrous CH 2 Cl 2 to ensure complete dissolution. in N 2 Under the protection of the atmosphere, quickly inject into the branched flask, and continue to N 2 Atmosphere protection. weigh exo - 5-Norbornene-2-carboxylic acid (0.54 g, 3.88 mmol) and 4-(dimethylamino)pyridine (0.17 g, 1.37 mmol) were dissolved in 20 mL of anhydrous CH 2 Cl 2 to ensure complete dissolution. in N 2 Under the protec...

Embodiment 3

[0131] Example 3: Preparation of polymer micelles loaded with hydrophobic doxorubicin molecules by dialysis

[0132] Take the amphiphilic brush copolymer P (PS) prepared by embodiment two 35 - co -P(PEG) 15 (10 mg) into a round bottom flask, add 2 mL tetrahydrofuran, measure 0.2 mL anticancer drug doxorubicin (DOX) in dimethyl sulfoxide (DMSO) solution (5 mg·mL -1 ) into the tetrahydrofuran solution, under continuous stirring, use a micro-injector at a slow speed (1 mL·h -1 ) was added deionized water (2 mL), after the injection was complete, stirred for 12 hours, and transferred to the -1 Dialyze in a dialysis bag for 24 hours under agitation. The volume of the dialyzed solution was adjusted to 10 mL to obtain polymer micelles loaded with hydrophobic doxorubicin molecules. The morphology and particle size of the polymer micelles were characterized by transmission electron microscopy (TEM) and dynamic light scattering (DLS). Figure 25 The transmission electron microgra...

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Abstract

The invention discloses a brush copolymer and a preparation method thereof. The preparation method comprises the following steps: synthesizing hydroxyl-terminated polystyrene and polyisoprene througha reactive anion polymerization method, and then carrying out esterification reaction on the hydroxyl-terminated polystyrene and the polyisoprene or hydroxyl-terminated polyethylene glycol and exo-5-norbornene-2-carboxylic acid to synthesize norbornene-terminated polystyrene, polyisoprene and polyethylene glycol macromonomers; and changing the feeding ratio and the feeding mode of the macromonomers to carry out ring-opening metathesis polymerization so as to obtain a two-block brush copolymer and a random brush copolymer which have different side chain ratios and arrangement sequences. The method has the characteristics of high reaction efficiency, mild reaction conditions and few side reactions, and the brush copolymer prepared by the method is controllable in structure and molecular weight and narrow in molecular weight distribution.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and in particular relates to a preparation method of a brush-shaped copolymer. Background technique [0002] Brush-shaped polymers, also known as polymer brushes, generally refer to a main chain composed of a repeating structural unit, and another molecular chain composed of repeating structural units is connected to the main chain in the form of side chains, and the adjacent branch chains The distance between them is equal, and the length of the branch chain is the same, and the shape is similar to a special class of grafted polymers of combs. According to the chemical composition of branched chains, brush polymers can be roughly divided into homopolymer brushes, mixed homopolymer brushes and copolymer brushes. However, the synthesis of brush polymers with well-defined compositions and structures is still a challenging work in the field of polymer synthesis. The methods currently used to synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/08C08G65/332C08F8/00C08F136/08C08F112/08
CPCC08G61/08C08G65/3324C08F8/00C08G2261/126C08G2261/1426C08G2261/148C08G2261/3324C08G2261/90C08F136/08C08F112/08
Inventor 何金林钱强雨倪沛红王彬张明祖
Owner SUZHOU UNIV
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