Flame retardant thermosetting resin and preparation method thereof
A thermosetting and resin technology, applied in the field of thermosetting resin and its preparation, can solve problems such as low thermal stability, achieve the effects of improving thermal stability, good flame retardant effect, and reducing the amount of addition
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Embodiment 1
[0035] 1. Preparation of intumescent flame retardant
[0036] (1) Under nitrogen protection, 13.6g of pentaerythritol was added to 90mL of phosphorus oxychloride, and then the temperature was gradually raised to 80°C for 8 hours. After the reaction, wash with carbon tetrachloride and ethanol three times in sequence, filter with suction, and dry in vacuum to obtain a white powder product with a yield of 81.5%.
[0037] (2) Under nitrogen protection and normal temperature, add 9g of deionized water, 50mL of ethanol and 0.5mL of tetraethylammonium hydroxide (20% aqueous solution) into a 250mL reactor, and stir to obtain a uniform mixture. 22.1 g of γ-aminopropyltriethoxysilane was added dropwise to the reactor using a constant pressure dropping funnel, and the dropwise addition was completed within 10 minutes. After raising the temperature to 50° C. for 10 hours, hexamethyldisilane was added into the reactor, and the reaction was continued for 6 hours to obtain a clear and trans...
Embodiment 2
[0056] Weigh 45.7g N,N'-4,4'-diphenylmethane bismaleimide and 34.3g O,O'-diallyl bisphenol A in a beaker, mechanically stir at 135°C for prepolymerization After 15 minutes, a brownish-yellow transparent clear liquid was obtained; 8.89 g of the intumescent flame retardant prepared in Example 1 (accounting for 10 wt% of the total mass of the resin system) was added to the liquid, and mechanically stirred for prepolymerization for 15 minutes to obtain a prepolymer. Pour the prepolymer into the preheated mold, vacuumize at 135°C for 1h, and then follow the processes of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 230°C / 4h respectively After curing and post-treatment, a flame-retardant bismaleimide resin is obtained. Its limiting oxygen index, thermogravimetric curve and thermal analysis data refer to the appendix respectively. Figure 10 , 11 and Table 3.
Embodiment 3
[0058] Weigh 45.7g N,N'-4,4'-diphenylmethane bismaleimide and 34.3g O,O'-diallyl bisphenol A in a beaker, mechanically stir at 135°C for prepolymerization After 15 minutes, a brownish-yellow transparent clear liquid was obtained; 14.1 g of the intumescent flame retardant prepared in Example 1 (accounting for 15 wt% of the total mass of the resin system) was added to the liquid, and mechanically stirred for 15 minutes to prepolymerize to obtain a prepolymer. Pour the prepolymer into the preheated mold, vacuumize at 135°C for 1h, and then follow the processes of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 230°C / 4h respectively After curing and post-treatment, a flame-retardant bismaleimide resin is obtained. Its limiting oxygen index, thermogravimetric curve and thermal analysis data refer to the appendix respectively. Figure 10 , 11 and Table 3.
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