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The preparation method of polymethyl methacrylate

A technology for polymethyl methacrylate and polymerization reaction, which is applied in the field of preparation of polymethyl methacrylate, can solve the problems of harsh polymerization reaction conditions and complicated preparation of initiators, and achieve high yield of polymerization products, simple preparation, The effect of mild polymerization conditions

Inactive Publication Date: 2016-01-06
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Yet, the shortcoming of the polymerization method of this methacrylate is: the polymerization reaction condition is harsher, needs to operate under anhydrous, anaerobic condition
Initiator preparation is more complex

Method used

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  • The preparation method of polymethyl methacrylate
  • The preparation method of polymethyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 20ml of refined tetrahydrofuran, 0.1g of diphenyl sulfoxide, 0.1g of epichlorohydrin and 0.5ml of 1MBF in a three-necked flask equipped with a stirring bar. 3 solution, stirred at room temperature for 25 minutes, then added 0.5ml1MBF 3 solution, 0.13gAlCl 3 Add the solution dissolved in 5.15g of methyl methacrylate into a three-necked flask, keep the system temperature at 30°C, and after 72 hours of reaction, add 20ml of acetone, and add 2ml of an aqueous solution with a mass fraction of 10% NaOH under stirring. The reaction was terminated after stirring at 20°C for 50 minutes. When the system was cooled to room temperature, 50 ml of methanol was added to precipitate the polymer. The polymer is then isolated. Dry under vacuum at 40 °C. The resulting polymer yield was 93%. In the gel permeation chromatography (GPC) test using polystyrene as a standard sample and tetrahydrofuran (THF) as a mobile phase, polymethyl methacrylate was obtained with a number average mo...

Embodiment 2

[0025] Add 15ml of refined tetrahydrofuran, 0.1g of diphenyl sulfoxide, 0.1g of propylene oxide and 0.5ml of 1MBF in a three-necked flask equipped with a stirring bar. 3 solution, stirred at room temperature for 25 minutes, then added 0.5ml1MBF 3 solution, 0.11gAlCl 3 Add the solution dissolved in 5.06g of methyl methacrylate into a three-necked flask, keep the system temperature at 30°C, and after reacting for 96 hours, add 20ml of acetone, and add 2ml of NaHCO solution dropwise under stirring. 3 The mass fraction is 10% aqueous solution, and the reaction is terminated after stirring at 50° C. for 30 minutes. When the system was cooled to room temperature, 50 ml of methanol was added to precipitate the polymer. The polymer is then isolated. Dry under vacuum at 40 °C. The resulting polymer yield was 62.4%. In the gel permeation chromatography (GPC) test using polystyrene as a standard sample and tetrahydrofuran (THF) as a mobile phase, polymethyl methacrylate was obtained ...

Embodiment 3

[0027] Add 20ml of refined tetrahydrofuran, 0.1g of diphenyl sulfoxide, 0.15g of epoxy styrene and 0.5ml of 1MBF in a three-necked flask equipped with a stirring bar. 3 Solution, after stirring at room temperature for 25 minutes, 0.26gAlCl 3 A solution dissolved in 5.16 g of methyl methacrylate was added to a three-necked flask. Keep the system temperature at 30°C. After reacting for 96 hours, add 20ml of acetone, add 2ml of an aqueous solution containing KOH with a mass fraction of 10% dropwise under stirring, and stop the reaction after stirring at 20°C for 60 minutes. When the system was cooled to room temperature, 50 ml of methanol was added to precipitate the polymer. The polymer is then isolated. Dry under vacuum at 40 °C. The resulting polymer yield was 37.1%. In the gel permeation chromatography (GPC) test using polystyrene as a standard sample and tetrahydrofuran (THF) as a mobile phase, polymethyl methacrylate was obtained with a number average molecular weight of...

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Abstract

The invention relates to a preparation method of polymethyl methacrylate. The preparation method is as follows: adding a catalyst and refined methyl methacrylate into diphenylsulfoxide ionic compound liquor; controlling a temperature to 0 DEG C-50 DEG C in the presence of an anhydrous organic solvent, polymerizing and ending polymerization reaction; then, adding a precipitator into the liquor to separate out polymethyl methacrylate. The polymethyl methacrylate prepared by the method disclosed by the invention is white solid, and the method is beneficial to processing follow-up products of the polymethyl methacrylate; number-average molecular weight of the prepared polymethyl methacrylate is greater than 5000, and molecular weight dispersion index of the prepared polymethyl methacrylate is smaller than 2.0; and a used initiator is simple to prepare, gentle in polymerization condition and high in polymerization product yield.

Description

technical field [0001] The invention relates to a preparation method of polymethyl methacrylate. Background technique [0002] Polymethyl methacrylate (PMMA) has excellent properties such as low density, high mechanical strength, low melting point, and high light transmittance, making it an important polymer. There are also many studies on its polymerization method. In addition to the polymethyl methacrylate produced by the traditional free radical polymerization method, the living polymer polymerization method 'group transfer polymerization' can synthesize polymethyl methacrylate polymer. . Compared with the traditional free radical polymerization method, the molecular weight distribution of the polymer obtained by this polymerization method is narrow, the molecular weight size is controllable, and the molecular structure can be designed. This polymerization method is characterized by (1) low polymerization reaction temperature. (2) The amount of catalyst is less. (3) L...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14
Inventor 周立民杨景廖广鑫肖乐福
Owner WUHAN INSTITUTE OF TECHNOLOGY