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Eight-arm heteroarm star-shaped polymer and preparation method thereof

A technology of star polymers and heteroarms, which is applied in the field of preparation of eight-arm heteroarm star polymers, can solve the problem of poor controllability of molecular weight and molecular weight distribution of polymer arms, consistent initiation efficiency of initiation points, and multifunctional initiators. Difficulties and other problems, to achieve the effects of good molecular weight and molecular weight distribution control, mild reaction conditions, and high reaction efficiency

Active Publication Date: 2017-05-10
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest feature of the "arm first and then core method" is that the molecular weight of the linear polymer can be conveniently designed and controlled, so as to obtain a star polymer with a relatively consistent arm length, but its disadvantage is that the reaction usually takes a long time and is difficult. Carry out completely; The feature of "nucleus first and then arm method" is that the number of arms of the star polymer is determined by the number of functional initiator groups, and the star polymer can continue to initiate monomer polymerization to obtain star-embedded segment copolymer
However, the disadvantage of this method is that it is relatively difficult to synthesize a multifunctional initiator with a clear structure and high purity; in addition, it is difficult to ensure that the initiation efficiency of each initiation point is consistent, so this method has a significant impact on the molecular weight of the polymer arm. Poor control of parameters such as molecular weight distribution and molecular weight distribution

Method used

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  • Eight-arm heteroarm star-shaped polymer and preparation method thereof
  • Eight-arm heteroarm star-shaped polymer and preparation method thereof
  • Eight-arm heteroarm star-shaped polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Example 1: Preparation of eight-arm hybrid-arm star polymer (7PS-POSS-PCL)

[0080] (1) Preparation of seven-arm star polystyrene (7PS-POSS-OH) containing a single hydroxyl group

[0081] Using sec-butyllithium (sec-BuLi, 3.8 mL, 4.96 mmol) as the initiator and benzene (50 mL) as the solvent, the living anionic polymerization of styrene (7.8 mL, 68.1 mmol) was initiated at 30 °C, reaction 8 After 1 hour, a small amount of active chain solution was taken and terminated with methanol, and the remaining active chain continued to undergo addition reaction directly with VPOSS-OH (389.3 mg, 0.6 mmol) under vacuum conditions, and was terminated with methanol after 1 hour of reaction.

[0082] After the reaction, the product was subjected to rotary evaporation to remove the solvent, and precipitated in methanol, filtered and concentrated to obtain a white solid powder, which was dried in a vacuum oven at room temperature for 24 hours to obtain the crude product of 7PS-POSS-OH, ...

Embodiment 2

[0094] Example 2: Preparation of eight-arm hybrid-arm star polymer (7PS-POSS-PEG)

[0095] (1) Preparation of alkyne-terminated polyethylene glycol (Propargyl-PEG)

[0096] A certain amount of mPEG-OH (2.00 g, 1 mmol) and 40 mL of anhydrous toluene were added to a 100 mL branched flask, and water was removed azeotropically. After the end, the purified mPEG-OH was dissolved in anhydrous THF under an inert gas atmosphere, KH (0.24 g, 6 mmol) was added slowly, and the reaction was stirred for 1 h in an oil bath at 25 °C.

[0097] Add 3-bromopropyne (1.19 g, 10 mmol, 80% in Toluene) into the constant pressure dropping funnel with a syringe, and dilute with about 5 mL of THF. Then it was added dropwise into the branch bottle, and reacted in an oil bath at 45°C for 20 h after the dropwise addition was completed. After filtration and concentration, add 40 mL of CH 2 Cl 2 , with saturated NaHCO 3 The solution was extracted three times, and the organic phase was collected and wash...

Embodiment 3

[0102] Example 3: Preparation of eight-arm hybrid arm star polymer (7PS-POSS-PDMA)

[0103] (1) Preparation of seven-arm star polystyrene (7PS-POSS-OH) containing a single hydroxyl group

[0104] Using sec-butyllithium (sec-BuLi, 3.0 mL, 3.92 mmol) as the initiator and benzene (40 mL) as the solvent, the living anionic polymerization of styrene (8.16 mL, 78.4 mmol) was initiated at 30 °C for 10 After 1 hour, a small amount of active chain solution was taken and terminated with methanol, and the remaining active chain continued to undergo addition reaction directly with VPOSS-OH (259.5 mg, 0.4 mmol) under vacuum conditions, and was terminated with methanol after 1 hour of reaction.

[0105] After the reaction, the product was subjected to rotary evaporation to remove the solvent, and precipitated in methanol, filtered and concentrated to obtain a white solid powder, which was dried in a vacuum oven at room temperature for 24 hours to obtain the crude product of 7PS-POSS-OH, Us...

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Abstract

The invention discloses a preparation method of an eight-arm heteroarm star-shaped polymer. A polystyrene lithium compound is synthesized through a living anionic polymerization method, and then subjected to an addition reaction with monohydroxy heptaethylene polyhedral oligomeric silsesquioxane in benzene to obtain a seven-arm star-shaped polystyrene crude product; slightly excessive low addition products are removed by utilizing a fractional precipitation method, thus pure monohydroxy functional seven-arm star-shaped polystyrene can be obtained, and hydroxyls of the pure monohydroxy functional seven-arm star-shaped polystyrene are subjected to azide modification to obtain seven-arm star-shaped polystyrene containing azide groups. On the other hand, polycaprolactone, polyethylene glycol, polymethylacrylic acid-N, N-dimethylamino ethyl ester, and tert-butyl methacrylate of which the ends contain alkynyls are respectively synthesized, and subjected to cycloaddition reaction with alkynyls and azides at the generating end of the seven-arm star-shaped polystyrene containing the azide groups to obtain the product; the method has the characteristics of high reaction efficiency, mild reaction conditions and few side reactions. The star-shaped polymer prepared by the invention is controllable in structure and molecular weight, and relatively 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 an eight-arm hybrid-arm star polymer. Background technique [0002] Star polymer generally refers to a type of branched polymer composed of multiple linear branches connected to the same central core. The linear branches that make up the star polymer are called the "arms" of the star polymer, and the multifunctional group at the center is called the "core" of the star polymer. According to the chemical composition of the "arm" and the structure of the "core", star polymers can be roughly divided into homo-arm star polymers, hetero-arm star polymers and dendritic star polymers. Compared with linear polymers, polymers with multi-arm topology have the characteristics of smaller hydrodynamic volume, smaller radius of rotation, low crystallinity, and low melt viscosity, and these properties are related to the number of arms Molecular parameters su...

Claims

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Application Information

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IPC IPC(8): C08G81/02C08G63/08C08G65/337C08F112/08C08F120/34C08F120/18
CPCC08F112/08C08F120/18C08F120/34C08G63/08C08G65/337C08G81/024C08G2650/04C08G81/021C08G81/025C08G81/027
Inventor 何金林晏雪生倪沛红戴礼兴徐俊张明祖
Owner SUZHOU UNIV
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