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Chloroprene 'activity'/controllable radical polymerization method

A chloroprene and polymerization method technology, applied in the field of polychloroprene, can solve the problems of uncontrollable polymer molecular weight, no re-initiating monomer, obvious tendency of branching and cross-linking, etc.

Inactive Publication Date: 2013-01-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This traditional inactive or uncontrollable chloroprene emulsion polymerization method has the following disadvantages in the preparation of adhesive chloroprene rubber: the molecular weight of the polymer is uncontrollable, and the tendency of branching and crosslinking is obvious; the uniformity of the molecular weight of the polymer is poor, and the molecular weight distribution coefficient Relatively wide; the polymer has no active end, the active chain free radical will terminate the activity after chain transfer, and has no ability to re-initiate the monomer

Method used

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  • Chloroprene 'activity'/controllable radical polymerization method
  • Chloroprene 'activity'/controllable radical polymerization method
  • Chloroprene 'activity'/controllable radical polymerization method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] RAFT reagent (2-ethoxycarbonyl propane-2-dithiobenzoate) is a chain transfer agent, AIBN is an initiator, and the molar ratio of RAFT and AIBN is 4:1. The molar ratio of solvent benzene, monomer chloroprene and chain transfer agent RAFT is 200:1. The above components were sequentially added to a 50 mL round-bottom branched-tube flask, and a magnet was placed; after argon was introduced for 10 minutes, vacuum degassing-argon filling was repeated three times, and the tube was sealed in an oxygen-free atmosphere. The sealed round-bottom branched-tube flask was placed in an oil bath at a constant temperature for the reaction, and the reaction temperature was 60°C, and samples were taken during the reaction. The polymer was precipitated with a large amount of petroleum ether, and dried in a vacuum oven at room temperature to constant weight. Weighing to calculate the monomer conversion rate; GPC to test the relative molecular mass and molecular weight distribution of the po...

Embodiment 2

[0032] RAFT reagent (2-ethoxycarbonyl propane-2-dithiobenzoate) is a chain transfer agent, AIBN is an initiator, and the molar ratio of RAFT and AIBN is 4:1. The molar ratio of solvent toluene, monomer chloroprene and chain transfer agent RAFT is 400:1. The above components were sequentially added to a 50 mL round-bottom branched-tube flask, and a magnet was placed; after argon was introduced for 10 minutes, vacuum degassing-argon filling was repeated three times, and the tube was sealed in an oxygen-free atmosphere. The sealed round-bottom branched-tube flask was placed in an oil bath at a constant temperature for the reaction, and the reaction temperature was 60°C, and samples were taken during the reaction. The polymer was precipitated with a large amount of petroleum ether, and dried in a vacuum oven at room temperature to constant weight. Weighing, calculating the monomer conversion rate; GPC testing the relative molecular mass and molecular weight distribution of the po...

Embodiment 3

[0034]RAFT reagent (2-ethoxycarbonylpropane-2-dithiobenzoate) is a chain transfer agent, ABVN is an initiator, and the molar ratio of RAFT and ABVN is 4:1. The molar ratio of solvent toluene, monomer chloroprene and chain transfer agent RAFT is 800:1. The above components were sequentially added to a 50 mL round-bottom branched-tube flask, and a magnet was placed; after argon was introduced for 10 minutes, vacuum degassing-argon filling was repeated three times, and the tube was sealed in an oxygen-free atmosphere. The sealed round-bottom branched-tube flask was placed in an oil bath at a constant temperature for the reaction, and the reaction temperature was 55°C, and samples were taken during the reaction. The polymer was precipitated with a large amount of petroleum ether, and dried in a vacuum oven at room temperature to constant weight. Weighing, calculating the monomer conversion rate; GPC testing the relative molecular mass and molecular weight distribution of the poly...

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Abstract

A chloroprene 'activity' / controllable radical polymerization method is used for preparing polychloroprene controllable in molecular weight and narrow in molecular weight distribution. RAFT (reversible addition-fragmentation chain transfer) reagents serve as chain transfer agents to be used for chloroprene polymerization at the temperature of 30-70 DEG C, so that living polymerization of the chloroprene is realized. The molecular size of a polymerization product is adjusted by changing feed ratio of raw materials or controlling polymerization time, so that the chloroprene polymer molecular weight is accurately controlled, polymer is narrow in molecular weight distribution (PDI 1.4), and the actual molecular weight of the polymer is consistent with the theoretical polymer. A molecular chain of the chloroprene polymer generated in polymerization has an active end of an RAFT capped structure, and accordingly, the chloroprene polymer can continue to serve as macromolecular chain transfer agents and continue to transfer and initiate polymerization of a second monomer to prepare a block polymer.

Description

technical field [0001] The invention relates to a method for preparing polychloroprene with controllable molecular weight and narrow distribution by adopting Reversible Addition-Fragmentation Chain Transfer (RAFT) polymerization. Background technique: [0002] In the past two decades, the research on "living" / controlled radical polymerization has made great progress, and important "living" / controlled radical polymerization methods include nitroxide-mediated radical polymerization (NMP), atom transfer radical polymerization (ATRP) and reversible addition-fragmentation chain transfer (RAFT) polymerization, etc. Among these "living" / controllable free radical polymerization systems, reversible addition-fragmentation chain transfer polymerization was first reported in the literature in 1998. Rizzardo et al. added AIBN, BPO, etc. to the traditional free radical polymerization system initiated by High chain transfer constant and specific structure of chain transfer agents such as ...

Claims

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Application Information

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IPC IPC(8): C08F136/18C08F2/38C08F2/34C08F2/06C08F2/02
Inventor 石艳惠嘉付志峰
Owner BEIJING UNIV OF CHEM TECH
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