Hyperbranched polysiloxane liquid crystal modified thermosetting resin and preparation method thereof
A technology of polysiloxane and thermosetting, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid nitrile, etc. It can solve the problems of reducing the activity of hyperbranched polysiloxane, achieve outstanding thermal stability, good The effect of manufacturability and long working period
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Embodiment 1
[0044] 1. Preparation of hyperbranched polysiloxane liquid crystals
[0045] (1) Synthesis of methyl bromidedecanoate
[0046] Dissolve 19.34g of bromoundecanoic acid in 100mL of methanol solution, and ultrasonically dissolve to obtain a transparent light yellow solution; add 4mL of concentrated sulfuric acid dropwise to the solution, and then reflux at 65°C for 6h. After the reaction was completed, methanol was removed by rotary evaporation, and a white solid was obtained by standing still. Dissolve the white solid in ether, wash it with saturated sodium bicarbonate solution, deionized water, and saline for 2 to 3 times, and then dry it with anhydrous magnesium sulfate; then distill off the ether, and stand to obtain the white solid, which is Methyl bromoundecanoate, denoted as MBU, has a yield of 86.9%. Its synthetic reaction formula and H NMR spectrum are shown in the attached figure 1 with 2 shown.
[0047] (2) Synthesis of mesogens
[0048] 7.80g of bromoundecan...
Embodiment 2
[0077] Weigh 0.95g epoxy resin (grade E-51) and 8.55g bisphenol A cyanate in a beaker, at 140 o C under mechanical stirring until melting, to obtain a light yellow clear transparent liquid, then add 0.5 g of the hyperbranched polysiloxane liquid crystal (accounting for 5wt% of the total mass of the resin system) prepared in Example 1 to the liquid, and mechanically stir until the liquid crystal melts After 1 hour of prepolymerization, the prepolymer was obtained, and its DSC curve and its curing reaction peak peak temperature are shown in the appendix Figure 19 and Table 1.
[0078] Pour the obtained prepolymer into the preheated mold, vacuumize at 140°C for 1h, and then follow the process of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 240°C / 6h After curing and post-treatment, a hyperbranched polysiloxane liquid crystal modified thermosetting resin is obtained, denoted as HLCP / eCE-2. Its thermogravimetric curve and characteristic parameters are shown in the attached Figure 19...
Embodiment 3
[0080] Weigh 0.9g of epoxy resin (grade E-51) and 8.1g of bisphenol A cyanate in a beaker, stir mechanically at 140°C until it melts to obtain a light yellow clear transparent liquid, then add 1g to the liquid for implementation The hyperbranched polysiloxane liquid crystal (accounting for 10wt% of the total mass of the resin system) prepared in Example 1 was mechanically stirred until the liquid crystal melted, and after prepolymerization for 15 minutes, a prepolymer was obtained. The DSC curve and its curing reaction peak peak temperature are shown in attached Figure 19 and Table 1.
[0081] Pour the prepolymer into the preheated mold, vacuumize at 140°C for 1h, and then cure according to the process of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 240°C / 6h And post-treatment, obtain a kind of hyperbranched polysiloxane liquid crystal modified thermosetting resin, denoted as HLCP / eCE-2. Its thermogravimetric curve and characteristic parameters are shown in the attached Figure...
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