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
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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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