A preparation method of fluorosilane-modified graphene-filled fluoroether rubber
A fluoroether rubber and fluorosilane technology, which is applied in the field of preparation of fluorosilane-modified graphene-filled fluoroether rubber, can solve the problems of slow hydrolysis reaction rate of fluorosilane at room temperature, low degree of graphene reaction, and unsuitability for mass preparation, etc. The effect of application prospect, excellent product performance and simple and easy preparation method
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[0049] The preparation method of the fluoroether rubber filled with fluorosilane modified graphene of the present invention comprises the following steps:
[0050] (1), fluorosilane grafted graphite oxide, the specific method is as follows:
[0051] Weigh graphite oxide and fluorosilane, mix the two with an organic solvent and adjust the pH value to 4-5 with acid, and ultrasonically treat the mixture in a water bath for 1-6 hours until the graphite oxide is uniformly dispersed, then reflux the mixture at a high temperature, and the reaction temperature The temperature is 50℃~90℃, and the reaction time is 1~12h. The reaction product is purified to remove fluorosilane that does not participate in the reaction, and the purified sample is dried to obtain a reaction product of fluorosilane grafted graphite oxide. Wherein the purification treatment method is one or more of centrifugal washing, vacuum filtration washing, and vacuum distillation.
[0052] The fluorosilanes are trifl...
Embodiment 1
[0074] 1. Fluorosilane grafted graphite oxide
[0075] Weigh 1 g of graphite oxide, 1 g of heptadecafluorodecyltriethoxysilane, and 200 mL of organic solvent into a reaction vessel, and adjust the pH value of the solution to 4-5 with glacial acetic acid. After sonicating in a water bath for 5 h, react at 75° C. for 6 h. The reaction product is purified by a centrifugal washing method to remove unreacted fluorosilane, and the product is vacuum-dried to obtain a reaction product of fluorosilane grafted graphite oxide.
[0076] 2. Reduction of fluorosilane-grafted graphite oxide
[0077] Weigh 1 g of fluorosilane-grafted graphite oxide, 15 g of hydroiodic acid, and 200 mL of glacial acetic acid, place them in a reaction vessel, and conduct ultrasonic treatment in a water bath for 3 h. The mixture was reacted at 40°C for 24h. The reaction product was filtered and washed with 100 mL of saturated sodium bicarbonate solution, 100 mL of distilled water and 100 mL of acetone, respec...
Embodiment 2
[0084] 1. Fluorosilane grafted graphite oxide
[0085] Weigh 1 g of graphite oxide, 2 g of tridecafluorooctyltriethoxysilane, and 200 mL of organic solvent into a reaction vessel, and adjust the pH value of the solution to 4-5 with glacial acetic acid. After sonicating in a water bath for 6 hours, react at 90°C for 3 hours. The reaction product is purified by centrifugal washing method to remove unreacted fluorosilane, and the product is dried in vacuum.
[0086] 2. Reduction of fluorosilane-grafted graphite oxide
[0087] Weigh 1 g of fluorosilane-grafted graphite oxide, 10 g of hydroiodic acid, and 200 mL of glacial acetic acid, place them in a reaction vessel, and conduct ultrasonic treatment in a water bath for 1 h. The mixture was reacted at 30°C for 48h. The reaction product was filtered and washed with 100 mL of saturated sodium bicarbonate solution, 100 mL of distilled water and 100 mL of acetone, respectively, to remove unreacted hydroiodic acid, and the product wa...
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