Method for preparing polymethyl methacrylate by single electron transfer living radical emulsion polymerization

A technology of polymethyl methacrylate and methyl methacrylate, which is applied in the chemical industry, can solve the problems of undiscovered single-electron active radical polymerization, the need for more expensive nitrogen-containing ligands, and sensitivity to oxygen, etc., to achieve Effects of high molecular weight, fast polymerization rate, and high initiation efficiency

Active Publication Date: 2013-01-02
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Of course, the SET-LRP method also has disadvantages, such as being sensitive to oxygen and requiring more expensive nitrogen-containing ligands, etc.
[0006] At present, emulsion polymerization has been successfully applied to living radical polymerization, however, the implementation of single-electron living radical polymerization has not yet been discovered.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Dissolve emulsifier 0.033g sodium lauryl sulfate and 0.016g OP-10 in 10.195g water to form an aqueous emulsion, then add 1.0g methyl methacrylate and 0.0195g ethyl 2-bromoisobutyrate, stir and mix evenly, Forms a translucent pre-emulsion a. Dissolve emulsifier 0.0021g sodium lauryl sulfate and 0.0011g OP-10 in 0.064g water to form a water emulsion, then add 0.0173g N, N, N ‘ , N ‘ , N ‘ -Pentamethyldiethylenetriamine and 0.0063g copper powder, stir and mix evenly and pre-emulsify for 60 minutes to form dark blue pre-emulsion b. Add pre-emulsion b to pre-emulsion a, repeatedly pass nitrogen into the system for 3-5 times to remove oxygen, initiate the system to start polymerization after about 23 minutes under the protection of nitrogen, end the reaction after 30 minutes, break the emulsion with ice methanol, Precipitate, filter with suction, and dry to obtain polymethyl methacrylate with high molecular weight and narrow molecular weight distribution.

[0017] The num...

Embodiment 2

[0019] Dissolve the emulsifier 0.034g sodium lauryl sulfate and 0.016g OP-10 in 10.195g water to form an aqueous emulsion, then add 0.99g methyl methacrylate and 0.0195g ethyl 2-bromoisobutyrate, stir and mix to form Translucent pre-emulsion a. Dissolve emulsifier 0.0021g sodium lauryl sulfate and 0.0011g OP-10 in 0.064g water to form a water emulsion, then add 0.0173g N, N, N ‘ , N ‘ , N ‘ - Pentamethyldiethylenetriamine and 0.0064g of copper powder, stirred and mixed for pre-emulsification for 60 minutes to form dark blue pre-emulsion b. Add the pre-emulsion b to the pre-emulsion a, repeatedly pass nitrogen into the system 3-5 times to remove oxygen, initiate the system to start polymerization after about 23 minutes under the protection of nitrogen, end the reaction after 120 minutes, break the emulsion with ice methanol, Purification yields polymethyl methacrylate with high molecular weight and narrow molecular weight distribution.

[0020] The number average molecular ...

Embodiment 3

[0022] Dissolve the emulsifier 0.032g sodium lauryl sulfate and 0.015g OP-10 in 10.195g water to form an aqueous emulsion, then add 1.0g methyl methacrylate and 0.0195g ethyl 2-bromoisobutyrate, stir and mix evenly, Forms a translucent pre-emulsion a. Dissolve emulsifier 0.0021g sodium lauryl sulfate and 0.001g OP-10 in 0.064g water to form a water emulsion, then add 0.0178g N, N, N ‘ , N ‘ , N ‘ -Pentamethyldiethylenetriamine and 0.0065g copper powder, stir and mix evenly and pre-emulsify for 60 minutes to form dark blue pre-emulsion b. Add pre-emulsion b to pre-emulsion a, repeatedly pass nitrogen into the system for 3-5 times to remove oxygen, initiate the system to start polymerization after about 23 minutes under the protection of nitrogen, end the reaction after 300 minutes, break the emulsion with ice methanol, Purification yields polymethyl methacrylate with high molecular weight and narrow molecular weight distribution. The number-average molecular weight of the p...

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Abstract

The invention belongs to the field of chemical industry and particularly relates to a method for preparing polymethyl methacrylate. The method includes the following steps that raw materials include water, emulsifying agents, catalyst copper powders, monomer methyl methacrylate, organic halidex initiators and ligand N, N, N', N', N'-pentamethyldiethylenetriamine; the water, the emulsifying agents, the monomer methyl methacrylate and the organic halidex initiators are uniformly mixed and stirred to obtain a pre-emulsion a; the water, the emulsifying agents, the ligand N, N, N', N', N'-pentamethyldiethylenetriamine and the catalyst copper powders are uniformly mixed and subjected to stirring pre-emulsification for 60 minutes to obtain a pre-emulsion b; the pre-emulsion a is added into the pre-emulsion b, and nitrogen is fed to deoxidize; the fully stirring is performed to perform the single electron transfer living radical polymerization at the temperature of 20 DEG C to 30 DEG C under the protection of nitrogen or argon, and demulsification and purification are performed to obtain the polymethyl methacrylate. The method has a good industrialization prospect.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a preparation method of polymethyl methacrylate. Background technique [0002] Polymethyl methacrylate (PMMA) is an industrially important polymer with a wide range of applications due to its well-known unique properties such as low density, high mechanical strength, low melting point, and good light transmission. The PMMA purchased in the market is produced by the traditional free radical polymerization method, and its molecular weight distribution is wide, and the molecular weight is difficult to control. [0003] Living / Controlled Radical Polymerization (L / CRP) is a new polymerization method developed for more than ten years. Compared with traditional free radical polymerization, this method has the advantages of large molecular weight, narrow molecular weight distribution and controllable molecular weight. , controllable molecular structure, etc. Compared with ionic polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F4/50C08F2/26C08F2/30
Inventor 付长清申亮卫晓波
Owner JIANGXI SCI & TECH NORMAL UNIV
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