Toxic ligand free electrochemistry regulated atom transfer radical polymerization method
A technology of atom transfer and polymerization method, which is applied in the field of electrochemically regulated atom transfer radical polymerization of non-toxic ligands, which can solve the problems of difficult storage and handling of low-valence transition metal catalysts, high price, etc., and simplify the post-processing process , reduce the cost of raw materials, optimize the effect of components
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Embodiment 1
[0042] After purification of methyl methacrylate monomer, acetonitrile solvent, and ethyl 2-bromophenylacetate initiator, the polymerization reaction components are prepared, methyl methacrylate, ethyl 2-bromophenylacetate, iron bromide The molar ratio is 200:1:1, and the volume ratio of methyl methacrylate and acetonitrile is 1:1. The preparation process is: weigh 0.0836 grams of ferric bromide and 0.1303 grams of tetraethylammonium tetrafluoroborate in the glove box and put them into a four-necked bottle, take 6 milliliters of methyl methacrylate monomer and 6 milliliters of acetonitrile with a needle tube and add to In the four-neck flask, after 20 minutes of magnetic stirring, 49.5 microliters of ethyl 2-bromophenylacetate was added, and the stirring was continued for 2 minutes to obtain a pre-reaction mixture.
[0043] Transfer the pre-reaction mixture in the four-shaped bottle to the heating device, control the reaction temperature to 60°C; connect the electrode to set t...
Embodiment 2
[0045] After purifying n-butyl methacrylate monomer, acetonitrile and ethyl 2-bromophenylacetate initiator, the polymerization reaction components were prepared, n-butyl methacrylate, ethyl 2-bromophenylacetate, bromide The molar ratio of iron is 200:1:1, and the volume ratio of n-butyl methacrylate and acetonitrile is 1:1. The preparation process is as follows: weigh 0.0836 grams of ferric bromide and 0.1303 grams of tetraethylammonium tetrafluoroborate in the glove box and put them into a four-neck bottle, take 8 milliliters of n-butyl methacrylate monomer and 8 milliliters of acetonitrile and add into a four-neck flask, and after magnetically stirring for 20 minutes, add 49.5 microliters of ethyl 2-bromophenylacetate, and continue stirring for 2 minutes to obtain a pre-reaction mixture.
[0046] Transfer the pre-reaction mixture in the four-shaped bottle to the heating device, control the reaction temperature to 60°C; connect the electrode, set the voltage (voltage is -0.3V...
Embodiment 3
[0048] After purification of methyl acrylate monomer, N-methylpyrrolidone as solvent and ethyl 2-bromophenylacetate initiator, the polymerization reaction components are prepared, methyl acrylate, ethyl 2-bromophenylacetate, bromide The molar ratio of iron is 200:1:1, and the volume ratio of methyl acrylate and N-methylpyrrolidone is 1:1. The preparation process is as follows: weigh 0.0836 grams of ferric bromide and 0.1303 grams of tetraethylammonium tetrafluoroborate into a four-necked bottle in the glove box, and take 6 milliliters of methyl methacrylate monomer and 6 milliliters of N-methyl methacrylate monomer with a needle tube. The base pyrrolidone was added into the four-neck flask, and after magnetic stirring for 20 minutes, 49.5 microliters of ethyl 2-bromophenylacetate was added, and the stirring was continued for 2 minutes to obtain a pre-reaction mixture.
[0049] Transfer the pre-reaction mixture in the four-shaped bottle to the heating device, control the reacti...
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