Preparation method of triblock acrylic acid ester thermoplastic elastomer
A thermoplastic elastomer and acrylate technology, which is applied in the field of three-block thermoplastic elastomers, can solve the problems of difficult removal and reuse of catalysts, difficulty in industrialization, and increased production costs, so as to improve heat aging resistance and chemical Responsiveness, low catalyst usage, and reduced sensitivity
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[0026] Example 1:
[0027] (1) Preparation of bifunctional macroinitiator polybutyl acrylate: preset molecular weight 60,000 (initiator: monomer=1:600,
[0028] 80% conversion rate to stop the reaction)
[0029] Into a 250mL four-necked flask with a thermometer was added 76.90g (0.6mol) monomer BA, 0.3880g (1×10 -3 mol) bifunctional initiator diα-bromoisobutyric acid 1,4-butanediol ester, 0.02680g (1.2×10 -4 mol) Catalyst CuBr 2 , 0.3122g (1.8×10 - 3mol) ligand PMDETA, 0.9720g (2.4×10 - 3mol) Reducing agent Sn(EH)2, 15.23g toluene, 5g anisole, mix well, then vacuumize and fill with nitrogen, heat up and stir, and react at 75°C. Sampling was taken every 30 minutes, and the monomer conversion rate was measured by gas chromatography and the molecular weight and molecular weight distribution were measured by gel permeation chromatography. After 12 hours of reaction, the conversion rate reached 79.5%, and the reaction ended. The solvent in the system was removed by vacuum distillation t...
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[0035] Example 2:
[0036] (1) Using the same bifunctional macroinitiator as in Example 1.
[0037] (2) Preparation of triblock copolymer poly(methyl methacrylate-b-butyl acrylate-b-methyl methacrylate): preset
[0038] Molecular weight 100,000 (initiator: monomer=1:500, conversion rate 90% to stop the reaction)
[0039] In a 100mL four-necked flask with a thermometer, 10.07g (0.1mol) monomer methyl methacrylate (MMA), 10.65g (2×10 - 4mol) Polybutyl acrylate (PBA) macroinitiator, 0.002690g (2×10 -5 mol) Catalyst CuCl 2 , 0.3469g (3×10 -5 mol) ligand PMDETA, 0.0081g (2×10 -5 mol) Reducing agent Sn(EH)-2, 15.57g toluene, 5.13g anisole, mix uniformly, then vacuum and fill with nitrogen, heat up and stir, and react at 75°C. Sampling was taken every 30 minutes, and the monomer conversion rate was measured by gas chromatography and the molecular weight and molecular weight distribution were measured by gel permeation chromatography. After 8.5 hours of reaction, the conversion rate reached ...
Example Embodiment
[0042] Example 3:
[0043] (1) Preparation of bifunctional macroinitiator polybutyl acrylate: preset molecular weight 2000 (initiator: monomer=1:20, conversion rate 80% to stop the reaction)
[0044] Into a 250mL four-necked flask with a thermometer were added 76.78g (0.6mol) monomer BA, 10.8g (0.03mol) bifunctional initiator α-bromoisobutyric acid 1,4-ethylene glycol ester, 0.04048g (3×10 -4 mol) Catalyst CuCl2, 0.7005g (1.5×10 -3 mol) ligand tris-(N,N-dimethylaminoethyl)amine (Me 6 TREN), 0.2645g (1.5×10 -3 mol) Ascorbic acid (AA), 15.15gs tetrahydrofuran, 3.20g toluene, mix well, then vacuumize and fill with argon, heat up and stir, and react at 60°C. Sampling was taken every 30 minutes, and the monomer conversion rate was measured by gas chromatography and the molecular weight and molecular weight distribution were measured by gel permeation chromatography. After 6.5 hours of reaction, the conversion rate reached 85.2%, and the reaction ended. The solvent in the system was re...
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