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Preparation method of polymethylmethacrylate with high molecular weight and narrow molecular weight distribution

A polymethyl methacrylate technology with narrow molecular weight distribution, applied in the field of chemical materials, can solve the problems of not many living radical polymerization, high emulsifier concentration, low monomer concentration, etc., and achieves good control characteristics and narrow molecular weight. The effect of distribution and improvement of purity

Inactive Publication Date: 2013-12-04
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at the same time, it also has the disadvantages of high emulsifier concentration and low monomer concentration in the polymerization system
[0006] At present, microemulsion polymerization has been widely used in traditional free radical polymerization, but there are not many implementations in living free radical polymerization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 0.0187g RAFT reagent S, S'-di(α,α'-methyl-α"-acetic acid) trithiocarbonate to 4.35g MMA and mix well to form an oil solution; Methyl ammonium bromide is dissolved in 50g of water to form an aqueous solution; the oil solution and the aqueous solution are mixed evenly to form a uniform translucent pre-emulsion. The pre-emulsion is stirred and heated to 70 ° C, and the system is fed with nitrogen for 30 minutes to remove oxygen. Then add 0.02175g of initiator AIBN into the system, and the initiation system starts to polymerize. After about ten minutes of stabilization, the microemulsion gradually turns from light yellow translucent to very light translucent blue, indicating that the reaction has started and ends after 5 hours. After reacting, slowly cooling to room temperature and discharging, polymethyl methacrylate with high molecular weight and narrow molecular weight distribution can be obtained.

Embodiment 2

[0031] Add 0.0375g RAFT reagent S, S'-di(α,α'-methyl-α"-acetic acid) trithiocarbonate to 4.35g MMA and mix well to form an oil solution; Methyl ammonium bromide is dissolved in 50g of water to form an aqueous solution; the oil solution and the aqueous solution are mixed evenly to form a uniform translucent pre-emulsion. The pre-emulsion is stirred and heated to 70 ° C, and the system is fed with nitrogen for 30 minutes to remove oxygen. Then add 0.02175g of initiator AIBN into the system, and the initiation system starts to polymerize. After about ten minutes of stabilization, the microemulsion gradually turns from light yellow translucent to very light translucent blue, indicating that the reaction has started and ends after 5 hours. After reacting, slowly cooling to room temperature and discharging, polymethyl methacrylate with high molecular weight and narrow molecular weight distribution can be obtained.

Embodiment 3

[0033] Add 0.0750g RAFT reagent S, S'-di(α,α'-methyl-α"-acetic acid) trithiocarbonate to 4.35g MMA and mix well to form an oil solution; Methyl ammonium bromide is dissolved in 50g of water to form an aqueous solution; the oil solution and the aqueous solution are mixed evenly to form a uniform translucent pre-emulsion. The pre-emulsion is stirred and heated to 80 ° C, and the system is fed with nitrogen for 30 minutes to remove oxygen. Then add 0.02175g of initiator AIBN into the system, and the initiation system starts to polymerize. After about ten minutes of stabilization, the microemulsion gradually changes from light yellow translucent to very light translucent blue, indicating that the reaction has started and ends after 2 hours. After reacting, slowly cooling to room temperature and discharging, polymethyl methacrylate with high molecular weight and narrow molecular weight distribution can be obtained.

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Abstract

The invention belongs to the field of chemical materials and discloses a preparation method of polymethylmethacrylate with high molecular weight and narrow molecular weight distribution, which includes mixing an RAFT chain transfer agent and a methyl methacrylate monomer to form even oil solution, adding the even oil solution into emulsifier water solution to obtain pre-emulsion, introducing nitrogen to for deoxidization, heating the pre-emulsion to the temperature ranging from 65 DEG C to 80 DEG C and adding initiator to trigger polymerization which lasts for 2 to 6 hours to obtain polymethylmethacrylate with high molecular weight and narrow molecular weight distribution. The preparation method successfully applying reversible addition / breaking chain transfer free radical polymerization technology to a micro emulation system, has better control characteristic on micro emulation polymerization of methyl methacrylate, improves emulation stability in the polymerization process, and ensures that the prepared polymer has higher molecular weight and narrower molecular weight distribution. Simultaneously, content of emulsifier in the polymer is lower, and purity of the polymer is greatly improved.

Description

technical field [0001] The invention belongs to the field of chemical materials, in particular to a method for preparing polymethyl methacrylate with high molecular weight and narrow molecular weight distribution. Background technique [0002] Free radical polymerization has been widely used because of its wide range of applicable monomers and mild polymerization conditions. The free radical polymerization process has the following characteristics: slow initiation, fast growth, and fast termination. However, conventional radical polymerization cannot synthesize polymers with narrow molecular weight distribution (molecular weight distribution index less than 1.5). [0003] Since the 1990s, breakthroughs have been made in the research of living radical polymerization technology. Nitroxide-Mediated Living Radical Polymerization (NMP), Atom Transfer Radical Polymerization (ATRP) and Reversible addition-fragmentation chain transfer appeared. Polymerization, RAFT) and other eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F2/38C08F2/24
Inventor 吕满庚马剑英
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI