Preparation method of thermostability enhanced melamine covalent functionalized graphene based nanohybrid material
A graphene-based nanometer and melamine technology, which is applied in the preparation of nanometer hybrid materials and the preparation of melamine covalently functionalized graphene-based nanometer hybrid materials, can solve the problems of high toxicity of coupling reagents, complicated operation and the like, and achieves the Improved thermal stability, simple operation and easy control
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[0029] Such as figure 1 As shown, a melamine covalently functionalized graphene-based nano hybrid material with enhanced thermal stability and a preparation method thereof include the following steps:
[0030] Step 1. Use the improved Hummers method to prepare graphite oxide solid with natural flake graphite powder;
[0031] Step 2. Prepare graphene oxide DMF suspension under ultrasound for 3-10 hours, the ratio of graphite oxide to DMF solvent is 7.5-15 mg / mL;
[0032] Step 3. Add excess thionyl chloride to the graphene oxide DMF suspension and react at 70-90°C for at least one day, then distill under reduced pressure to remove excess SOCl 2 Obtained later, wherein the ratio of graphite oxide to thionyl chloride is not more than 10 mg / mL (GOCl);
[0033] Step 4. Prepare a DMSO solution of melamine (MA); the ratio of melamine to DMSO is (50:1) ~ (5:1) mg / mL;
[0034] Step 5. Mix the GOCl obtained in step 3 with the melamine solution prepared in step 4. In order to speed up the reaction...
Embodiment 1
[0037] The first step is the preparation of graphite oxide solid;
[0038] At 80 ℃, pre-oxidize 20 g of natural graphite (400 mesh) with 30 mL concentrated sulfuric acid, 10 g potassium persulfate and 10 g phosphorus pentoxide, wash with water to pH=7, and dry overnight at room temperature for later use;
[0039] Cool 460 mL of concentrated sulfuric acid to about 0 ℃, then add 20 g of pre-oxidized graphite to it, and slowly add 60 g of potassium permanganate so that the temperature of the system does not exceed 20 ℃. After the addition, the temperature is raised to 35 ℃ and stirred After 2 h, slowly add 920 mL of deionized water in batches so that the temperature of the system does not exceed 98 ℃, and after stirring for 15 minutes, add 2.8 L of deionized water and 50 mL of 30% hydrogen peroxide. The obtained bright yellow suspension was suction filtered and washed under reduced pressure. Until there is no sulfate ion in the filtrate and it is neutral, the product is drie...
Embodiment 2
[0047] Steps 1 to 4 are the same as steps 1 to 4 in Example 1.
[0048] In the fifth step, add 7 mL of pyridine to the GOCl obtained in the third step and the solution in the fourth step, adjust the temperature to 110 ℃, and stir for 24 hours at a constant temperature;
[0049] In the sixth step, the crude product obtained in the fifth step is filtered, washed, and dried to obtain the product GO-MA 110 .
[0050] Infrared spectra such as image 3 As shown in d, it is proved that the nano hybrid material has been successfully synthesized.
[0051] Its thermal stability such as Figure 4 As shown in the figure, the thermal stability of the functionalized graphene nano-hybrid material is higher than that of the unmodified graphene oxide.
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