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Method for preparing PMMA with high molecular weight and narrow molecular weight distribution

A technology with narrow molecular weight distribution and high molecular weight, applied in the field of polymethyl methacrylate, can solve the problems of long reaction time, high energy consumption, expensive RAFT reagent, etc., and achieve the effects of high utilization rate, mild conditions and simple operation.

Inactive Publication Date: 2019-01-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The patent document with the patent publication number US4711938 discloses a method of regulating polymerization by regulating the low conversion rate, and regulating the molecular weight and distribution by reducing the viscosity of the system, but the reaction time of this process is long and the energy consumption is large.
Moreover, the synthesis of RAFT reagents is more complicated, and the price of RAFT reagents is more expensive, and there is no industrialized product yet

Method used

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  • Method for preparing PMMA with high molecular weight and narrow molecular weight distribution
  • Method for preparing PMMA with high molecular weight and narrow molecular weight distribution
  • Method for preparing PMMA with high molecular weight and narrow molecular weight distribution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Add 0.1900g of iodine, 0.1850g of azobisisobutyronitrile, 50g of methyl methacrylate, and 0.8598g of hexamethylphosphoric triamide into a 50ml single-necked flask with magnetic stirring to form a uniform solution. The air in it was "pumped-dissolved" four times. Under the condition of avoiding light, the temperature was raised to 70°C in an oil bath. After 16 hours of reaction, it was slowly cooled to room temperature and discharged to obtain a number average molecular weight of 30500 and a dispersion coefficient. 1.26 polymethyl methacrylate. The GPC curve of the polymer is as image 3 (1) shown.

Embodiment 2

[0066] Add 0.1900g of iodine, 0.1850g of azobisisobutyronitrile, 60g of methyl methacrylate, and 1.1464g of hexamethylphosphoric triamide into a 100ml single-necked flask with magnetic stirring to form a homogeneous solution. The air in it was "pumped-dissolved" four times. Under the condition of avoiding light, the temperature was raised to 75°C in an oil bath, and after 18 hours of reaction, it was slowly cooled to room temperature and discharged, and the number average molecular weight was 50800, and the dispersion coefficient was 1.28. of polymethyl methacrylate. The GPC curve of the polymer is as image 3 (2) shown.

Embodiment 3

[0068] Add 0.1900g of iodine, 0.1850g of azobisisobutyronitrile, 90g of methyl methacrylate, and 1.7196g of hexamethylphosphoric triamide into a 100ml single-necked flask with magnetic stirring to form a homogeneous solution. The air in it was "pumped-dissolved" four times. Under the condition of avoiding light, the temperature was raised to 75°C in an oil bath. After 20 hours of reaction, it was slowly cooled to room temperature and then discharged. The number average molecular weight was 60700, and the dispersion coefficient was 1.31. of polymethyl methacrylate. The GPC curve of the polymer is as image 3 (3) shown.

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Abstract

The invention discloses a method for preparing PMMA with high molecular weight and narrow molecular weight distribution. According to the method, firstly, an iodine compound is obtained by an in-situreaction of an azo initiator and an iodine simple substance, and a combined action of the generated iodine compound and a phosphoramide additive regulates and controls the reaction to obtain the PMMAwith the high molecular weight and the narrow molecular weight distribution. The reaction is mild in condition, is simple to operate, and is high in utilization rate of raw materials; and the conversion rate of converting elemental iodine into the iodine compound is 98% or above, the monomer conversion rate is in a range of 80-98%, the number average molecular weight of the prepared poly(methyl methacrylate) is between 30000 and 120000, the weight average molecular weight is between 37000 and 170000, and the molecular weight is distributed in the range of 1.2-1.6.

Description

technical field [0001] The invention relates to the technical field of preparation of engineering materials, in particular to a polymethyl methacrylate with high molecular weight and narrow distribution prepared by a living free radical polymerization method. Background technique [0002] High molecular weight polymethyl methacrylate, commonly known as plexiglass, is called methyl methacrylate resin in the plastic industry. It has unique light transmittance and good aging resistance. PMMA is colorless and transparent. Its light transmittance is the best among plastics. It has a wide range of light transmission and has good anti-craze and impact Toughness: small mass, toughness, high mechanical degree at normal temperature, excellent surface gloss, good tinting strength, good dimensional stability, good electrical conductivity, no flame when non-toxic burning, and monomer methyl methacrylate is easy to mix with Other ethylene monomers are copolymerized to obtain products wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F2/38C08F4/04
CPCC08F2/38C08F4/04C08F120/14
Inventor 石艳王延安李彬付志峰
Owner BEIJING UNIV OF CHEM TECH
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