Multibranched polymers and process for production thereof
A polymer and multi-branch technology, applied in electrochemical generators, electrical components, circuits, etc., can solve the problems of polymer solid electrolytes not having ionic conductivity and shape stability
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Embodiment 1
[0611] (Embodiment 1) Synthesis of Multibranched Polymer 1
[0612] (1) Preparation of polymerization initiator-1
[0613] Add 20.0g (50mmol) 1,1,2,2-tetrakis(4-hydroxyphenyl)ethane (TEP), 25.3g (250mmol) triethylamine, 200ml tetrahydrofuran (THF) in the flask, and the whole container Cool to 0 °C. Thereto, 50.58 g (220 mmol) of 2-bromoisobutyryl bromide diluted with 50 ml of THF was slowly added dropwise. After the dropwise addition, it was aged overnight at room temperature. The reaction liquid was filtered to remove triethylamine hydrochloride, and the solvent was distilled off from the filtrate under reduced pressure. Dichloromethane and water were added to the resulting residue for liquid separation, and the organic layer was taken out and washed with anhydrous MgSO 4 dry. After the solvent was distilled off, the obtained crude product was purified by silica gel column chromatography, and the resulting crude product was recrystallized to obtain 23.2 g of white crysta...
Embodiment 2
[0619] (Embodiment 2) Synthesis of Multibranched Polymer 2
[0620] 0.1 g (0.1 mmol) of BiB-TEP obtained in (1) of Example 1, 20.0 g (40 mmol) of the monomer represented by the formula (a11) (R 1000 = R 2000 = R 40b = Hydrogen atom, R 40a = methyl) homopolymer (trade name: Blemmer PME-400, manufactured by NOF Corporation, hereinafter abbreviated as "PME400"), 80.0 g of THF, and the inside was degassed. Next, 0.24 g (0.25 mmol) of dichlorotris(triphenylphosphine)ruthenium was added and mixed uniformly, further, 0.1 g (0.1 mmol) of dichlorotris(triphenylphosphine)ruthenium was added and mixed uniformly. Next, 0.05 g (0.4 mmol) of di-n-butylamine was added and heated to 60° C. to start the polymerization reaction. After 9 hours of polymerization, the reaction solution was cooled to 0° C. to stop the polymerization reaction.
[0621] After distilling off the solvent from the reaction liquid, the resulting residue was purified by silica gel column chromatography to remove trans...
Embodiment 3
[0623] (Embodiment 3) Synthesis of Multibranched Polymer 3
[0624] In the flask, add 0.50g (0.5mmol) BiB-TEP obtained in (1) of Example 1, 0.14g (1.0mmol) CuBr, 0.0067g (0.05mmol) CuBr 2 , 10.0 g (116 mmol) of methyl acrylate (MA), and 10.0 g (78 mmol) of tert-butyl acrylate (tBA) were degassed inside. 0.17 g (1.0 mmol) of degassed N, N, N', N', N"-pentamethyldiethylenetriamine was added thereto, and stirred at room temperature for 30 minutes. The whole vessel was heated to 60° C., The polymerization reaction was started, and after 2 hours of polymerization, the reaction solution was cooled to 0°C to stop the polymerization reaction. After distilling off the solvent from the reaction solution, the residue was dissolved in THF, and the transition metal complex was removed by silica gel column chromatography. , to obtain a crude product, which was reprecipitated using methanol / water to obtain 9.5 g of white crystals of the target multibranched polymer 3 (the yield of separatio...
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