Method for microwave-assisted preparation of hyperbranched polycyclophosphazene grafted graphene
A technology of polycyclophosphazene and grafted graphite, which is applied in graphene, chemical instruments and methods, inorganic chemistry, etc., and can solve the problems affecting the application of modified graphene, insufficient heat resistance of hyperbranched polymers, and complicated preparation processes, etc. problems, to achieve excellent chemical stability and thermal stability, high yield and fast reaction rate
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Embodiment 1
[0026] Step (1): Mix 0.3g KH-550 and graphene oxide prepared by the improved Hummer method at a mass ratio of 1:1, add it to 150ml ethanol, and after ultrasonication at 300W for 30min, pour it into a three-necked flask, pass Nitrogen gas was injected, the stirring rate of the microwave reactor was 300 rpm / min, and the reaction was carried out at 80° C. for 2 h. Then, after washing with ethanol and deionized water for 3 times, the dark gray solid product was vacuum-dried at 60°C for 4 hours to obtain KH550-modified graphene oxide (see the attached figure 1 ).
[0027] Step (2): Add sodium citrate and the KH-550-modified graphene oxide into 120ml deionized water at a mass ratio of 1:0.5, ultrasonically disperse for 30min, add to a microwave reactor, and react at 90°C for 10min. Centrifuge to obtain a black solid product, wash with ethanol and deionized water three times respectively, and dry in vacuum at 60°C for 5 hours to obtain KH550-modified graphene.
[0028] Step (3): In t...
Embodiment 2
[0031] Step (1): Mix 0.2g KH-550 and graphene oxide prepared by the improved Hummer method at a mass ratio of 1:2, add it to 150ml ethanol, and after ultrasonication at 300W for 30min, pour it into a three-necked flask, pass Nitrogen gas was injected, the stirring rate of the microwave reactor was 300 rpm / min, and the reaction was carried out at 80° C. for 2 h. After three times of suction filtration and washing, the dark gray solid product was vacuum-dried at 60°C for 4 hours to obtain KH550-modified graphene oxide;
[0032] Step (2): Add sodium citrate and KH-550-modified graphene oxide into 120ml of deionized water at a mass ratio of 1:3, ultrasonically disperse for 30min, add to a microwave reactor, and react at 70°C for 30min. After centrifugation, the black solid product was washed three times with ethanol and deionized water, and dried in vacuum at 60°C for 5 hours to obtain KH550-modified graphene.
[0033] Step (3): In the microwave reactor, add hexachlorocyclotripho...
Embodiment 3
[0036] Step (1): Mix 0.3g KH-550 and graphene oxide prepared by the improved Hummer method at a mass ratio of 1:6, add it to 150ml ethanol, and after ultrasonication at 300W for 30min, pour it into a three-necked flask, pass Nitrogen gas was injected, the stirring rate of the microwave reactor was 300 rpm / min, and the reaction was carried out at 80° C. for 2 h. After three times of suction filtration and washing with ethanol and deionized water, the dark gray solid product was vacuum-dried at 60° C. for 4 hours to obtain KH550-modified graphene oxide.
[0037] Step (2): Add sodium citrate and KH-550-modified graphene oxide into 200ml of deionized water at a mass ratio of 1:1.5, ultrasonically disperse for 30min, add to a microwave reactor, and react at 70°C for 30min. After centrifugation, the black solid product was washed three times with ethanol and deionized water, and dried in vacuum at 60°C for 5 hours to obtain KH550-modified graphene.
[0038] Step (3): In the microwa...
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