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Multi-arm star-type polymer and preparation method thereof

A technology of polymers and multi-armed stars, applied in the field of multi-armed star polymers and its preparation, can solve the problems of low molecular weight of multi-armed star polymers, difficulty in adjusting and controlling the structure and size of the core, and achieve The effects of easy polymerization, convenient modification, and wide sources

Inactive Publication Date: 2009-11-11
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the number of arms of the multi-armed star-shaped polymer is more, free radicals are easy to couple and cross-link in the process of preparing the multi-armed star-shaped polymer by using ATRP reaction, so the molecular weight of the multi-armed star-shaped polymer prepared at present is not high ( 10 4 ~10 6 )
In addition, the existing multi-armed star polymers use single-structure dendrimers or hyperbranched polymers as the core, and the structure and size of the core are not easy to adjust and control.

Method used

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  • Multi-arm star-type polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Preparation of the core of the star-shaped multi-arm polymer

[0024] Add 0.659g of 2,2-bipyridine and 0.209g of cuprous chloride into a 100ml two-necked bottle, repeatedly vacuumize and fill with argon. Then 8ml of chlorobenzene, 3g of p-chloromethylstyrene and 2.42g of styrene were added in sequence. Under the protection of argon, react at 120°C for 4 hours. The reaction was quenched by the addition of tetrahydrofuran, and the product mixture was stirred for 2 hours, then chromatographed on neutral alumina. The solution obtained by chromatography was rotatively distilled and then precipitated with ethanol / water mixed solution with a volume ratio of 5:1. The obtained white precipitate was dried in vacuum for 24 hours and then stored in an inert atmosphere. The resulting chlorine-containing hyperbranched polystyrene copolymer totaled 5.15 g, and the yield was 95%. The measured number average molecular weight was 16270, and the molecular weight distribution was 3.4...

Embodiment 2

[0028] Add 0.2 g of the chlorine-containing hyperbranched polystyrene macromolecular initiator prepared in step 1) of Example 1, and 0.0416 g of cuprous chloride into a 100 ml three-necked flask, repeatedly vacuumize and fill with argon. Then 15ml of pyridine, 2.29g of acrylonitrile, and 0.1456g of pentamethyldiethylenetriamine were added in sequence. Under the protection of argon, react at 130°C for 4 hours. Then 15 ml of xylene was added dropwise. The reaction was continued until the 10th hour, when tetrahydrofuran was added to terminate the reaction, and the product mixture was stirred for 2 hours, then chromatographed on neutral alumina. The solution obtained by chromatography was rotatively distilled and then precipitated with ethanol / water mixed solution with a volume ratio of 5:1. The obtained white precipitate was dried in vacuum for 24 hours and then stored in an inert atmosphere. The obtained chlorine-containing star polymer was 1.87 g in total, and the yield was 6...

Embodiment 3

[0030] In a 100ml three-necked flask, add 0.2g of the chlorine-containing hyperbranched polystyrene type macromolecular initiator prepared in step 1) of Example 1, 0.1318g2, 2'-bipyridyl, 0.0416g cuprous chloride, and repeatedly vacuumize And filled with argon. Then 15ml of chlorobenzene and 4.5g of methyl methacrylate were added successively. Under the protection of argon, react at 100°C for 4 hours. Then 15 ml of 1,4-dioxane was added dropwise. Continue the reaction until the 10th hour, add tetrahydrofuran to terminate the reaction, stir the product mixture for 2 hours, and then precipitate it with a mixed solution of ethanol / water with a volume ratio of 5:1. The obtained white precipitate is dried in vacuum for 24 hours and stored in an inert atmosphere . The obtained chlorine-containing star polymer was 3.68 g in total, and the yield was 78.3%. The measured number average molecular weight was 1,007,000, and the molecular weight distribution was 2.74.

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Abstract

The invention discloses a multi-arm star-type polymer and a preparation method thereof. The method synthesizes the multi-arm star-type polymer by a method with the following two steps of step one: taking a complex formed by a polydentate nitrogen-contained compound and a transitional metal halide as a catalytic system so as to catalyze the polymerization of atom transfer free radicals and self-condensing vinyl of a monomer, thus preparing and obtaining the halogen atom-contained hyperbranched polystyrene macromolecular initiator taken as the star-type polymer core; and step two: taking the complex formed by the the polydentate nitrogen-contained compound and the transitional metal halide as the catalytic system and taking the prepared halogen atom-contained hyperbranched polystyrene macromolecular as the initiator to initiate the polymerization of the atom transfer free radicals of the monomer, thus preparing and obtaining the multi-arm star-type polymer with controllable core structure, core size, core property, arm number, arm length and arm property and adjustable molecular weight within wider range.

Description

technical field [0001] The invention relates to a multi-arm star polymer and a preparation method thereof. Background technique [0002] Star polymers are one of the research hotspots in the field of polymer materials in recent years. It is a class of star-shaped macromolecules with a single branch point as the core and multiple molecular chains drawn around. Star polymers have a highly branched structure, so they exhibit many different properties from linear polymers, such as: molecular chains are not easily entangled, the viscosity of solution and bulk is significantly lower than that of linear polymers with the same molecular weight, and the molecular structure is similar to that of linear polymers. Spherical, with a large number of functional groups at the end of the molecular chain for further modification. The unique topology of star-shaped polymers endows them with unique physical and chemical properties, and the flexible and adjustable functional groups greatly exp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F257/02C08F2/04C08F4/26C08F4/10
Inventor 李化毅张君张辽云胡友良李金阁曾婉李倩
Owner INST OF CHEM CHINESE ACAD OF SCI
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