A random copolymer and its preparation method, modified PBO fiber and its preparation method, resin-based wave-transparent composite material and its preparation method
A technology of random copolymers and composite materials, applied in fiber processing, fiber types, textiles and papermaking, etc., can solve the problem of poor bonding between modified PBO fiber and resin base, uncontrollable polydopamine molecular weight and dispersion coefficient, and reaction time long wait question
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[0046] The present invention also provides a method for preparing the random copolymer described in the above technical scheme, comprising the following steps:
[0047] Mix styrene, glycidyl methacrylate, 4-vinylbenzocyclobutene, RAFT reagent, initiator and reaction solvent, and carry out RAFT polymerization reaction under protective atmosphere to obtain the random copolymer.
[0048] In the present invention, unless otherwise specified, the raw materials used in the present invention are preferably commercially available products.
[0049] In the present invention, the molar ratio of styrene, glycidyl methacrylate and 4-vinylbenzocyclobutene is (30-50): (10-16): (3-4), preferably (30-40): (12-16): (3.5-4), more preferably (30-35): (15-16): (3.8-4).
[0050] In the present invention, the RAFT reagent is preferably 4-cyano-4-[(dodecylsulfanylthiocarbonyl) sulfanyl] pentanoic acid; the molar ratio of the styrene to the RAFT reagent is preferably ( 30-50): (0.1-0.8) More prefer...
Embodiment 1
[0096] 30.0mmol styrene (S), 16mmol glycidyl methacrylate (GMA), 3.0mmol 4-vinylbenzocyclobutene (BCB), 0.1mmol 4-cyano-4-[(dodeca Alkylsulfanylthiocarbonyl)sulfanyl]pentanoic acid (Raft reagent, CTA), 0.06mmol 1,1-azobis(cyclohexanecarbonitrile) and 10mL dichloromethane were added to the round bottom flask, and the Enter nitrogen and seal; put into 70 ℃ oil bath and stir magnetically for 20h, pass the gained RAFT polymerization reaction system through normal hexane (the volume of normal hexane is 600% of the volume of RAFT polymerization reaction system) 3 times, through drying, obtain Regular copolymer P (S-co-BCB-co-GMA), through the peak area of nuclear magnetic spectrum and the productive rate of product, calculate x is 56 in the random copolymer, y is 2, z is 48; The number average molecular weight of the obtained random copolymer measured by permeation chromatography (GPC) was 32300, and the dispersion coefficient was 1.09.
[0097] figure 1 It is the nuclear magnet...
Embodiment 2
[0101] 40.0mmol styrene (S), 12mmol glycidyl methacrylate (GMA), 4mmol 4-vinylbenzocyclobutene (BCB), 0.5mmol 4-cyano-4-[(dodecane Sulfanylthiocarbonyl)sulfanyl]pentanoic acid (Raft reagent, CTA), 0.08mmol 1,1-azobis(cyclohexanecarbonitrile) and 12mL dichloromethane were added to the round bottom flask, passed through Nitrogen and seal. Put it into an 80°C oil bath and stir it magnetically for 28 hours, pass the obtained RAFT polymerization reaction system through n-hexane (the volume of n-hexane is 700% of the volume of the RAFT polymerization reaction system) 3 times, and dry to obtain the random copolymer P (S-co-BCB-co-GMA), wherein x is 55, y is 1, and z is 44, the molecular weight of the obtained random copolymer is 34200, and the dispersion coefficient is 1.17.
[0102] Soak 110 parts by weight of PBO fiber in 90 parts by weight of 6.0wt% P (S-co-BCB-co-GMA) solution (the first organic solvent is dichloromethane), wait for the first organic solvent to evaporate, put it...
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