Triblock copolymers
A technology of block copolymers and copolymers, applied in the field of triblock copolymers, which can solve the problems of brittle nature limiting bending and handling tolerance, scaling, etc.
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[0067] general considerations :
[0068] Polymer synthesis and reagent purification were performed in an MBraun Labmaster SP glove box or in custom glassware designed for anionic polymerization (see, for example, Ndoni, S.; Papadakis, C.M.; Bates, F.S.; Almdal, K., " A laboratory-scale apparatus for anionic polymerization under an inert atmosphere". Review of Scientific Instruments, 1995, Vol. 66 (No. 2), pp. 1090-1095 (Ndoni, S.; Papadakis, C.M.; Bates, F.S.; Almdal, K. Laboratory-scale Setup for Anionic Polymerization under InertAtmosphere. Review of Scientific Instruments 1995, 66(2), 1090–1095) DOI: 10.1063 / 1.1146052). Anionic polymerizations and reagent manipulations were performed using standard air-free techniques. The hydrogenation was performed in a Parr series 4530 / 40 / 50 (rated at 1900 pounds per square inch (psi) (13.1 MPa)) 2 liter (L) stirred reactor under temperature control. Reagents and corresponding suppliers are listed in Table 1 below.
[0069] Table ...
preparation Embodiment 1
[0094] PREPARATIVE EXAMPLE 1: TDBMS-TERMINATED POLY(ISOPRENE-BLOCK-STYRENE) BLOCK COPOLYMER (IS-OR)
[0095]
[0096]In the glove box, benzene (approximately 600 mL) and styrene (43.60 grams (g), 419 millimoles (mmol)) were added to a 1 L Schlenk flask equipped with a stir bar. With vigorous stirring, the protected initiator TBDMSPL (0.63 mL, 0.63 mmol) was quickly injected by syringe. The reaction color slowly changed from colorless to orange over the course of 15 minutes. The polymerization system was allowed to stir in the glove box at room temperature for 48 hours. Then isoprene (21.10 g, 309 mmol) was added, causing the color of the reaction system to turn pale yellow rapidly. The polymerization system was stirred for an additional 24 hours, during which time the composition became more viscous.
[0097] Twenty-four hours after the introduction of the isoprene, the polymerization was quenched with degassed isopropanol. The polymer was then dried under reduced pre...
preparation Embodiment 2
[0101] Preparation Example 2: Hydrogenation of IS-OH Block Copolymers: Synthesis of PEP-PCHE-OH
[0102]
[0103] In the glove box, the polymer (58.0 g, PI-PS-OR, PE-1B) was added to a 1 L jar with a stir bar. Cyclohexane (approximately 750 mL) was then added and the polymer solution was stirred overnight to dissolve. The next day, the Pd / CaCO 3 The catalyst (7.5 g) was introduced into the polymer solution and suspended under vigorous stirring. The polymer solution is sealed and removed from the glove box. A clean 2L Parr reactor was fitted with a glass insert and placed under Ar gas sparge. The polymer solution was then quickly added to the reactor under Ar sparge before sealing.
[0104] Once sealed, the reactor was placed under a hydrogen atmosphere through four cycles of pressurization (200 psi, 1.38 MPa) and venting while stirring and monitoring with a hydrogen sensor. After the hydrogen atmosphere was established, the reactor was pressurized to 500 psi (3.45 MP...
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