• 专利标题:   Preparing graphene composite aerogel comprises selecting chemical substance materials, heating and reacting, filtering, performing ultrasonic dispersion, melting, hydro-thermally heating, freezing and curing, annealing and storing.
  • 专利号:   CN108940141-A
  • 发明人:   LIU X, ZHANG E, LIU W, YANG Y, CHEN L
  • 专利权人:   UNIV TAIYUAN TECHNOLOGY
  • 国际专利分类:   B01J013/00
  • 专利详细信息:   CN108940141-A 07 Dec 2018 B01J-013/00 201917 Pages: 12 Chinese
  • 申请详细信息:   CN108940141-A CN10909975 10 Aug 2018
  • 优先权号:   CN10909975

▎ 摘  要

NOVELTY - Preparing graphene composite aerogel comprises (i) selecting chemical substance materials used for preparation, performing quality purity, concentration and content control of selected chemicals, (ii) (iia) adding carbon micro-spheres, nitric acid and hydrogen peroxide into polytetrafluoroethylene container, (iib) transferring reaction kettle, heating and reacting, cooling, (iic) washing, filtering, discarding, and (iid) drying filter cake, (iii) (iiia) adding graphene and de-ionized water, stirring and mixing, (iiib) performing ultrasonic dispersion, heating, (iiic) freezing, naturally melting, hydro-thermally heating, (iiid) placing composite hydrogel in dialysis bag, sealing, submerging, allowing to stand, repeating dialysis, (iiie) freezing and curing, freezing and drying, and (iiif) annealing, (iv) using weights for mechanical compression performance test, performing shape analysis, analyzing thermal stability, analyzing diffraction intensity, and (v) storing. USE - The method is useful for preparing graphene composite aerogel. ADVANTAGE - The aerogel has good thermal conductivity, mechanical strength and specific surface area. The method is advanced in technology and accurate in data. DETAILED DESCRIPTION - Preparing graphene composite aerogel comprises (i) selecting chemical substance materials used for preparation, performing quality purity, concentration and content control of selected chemicals, where the carbon microsphere has 81% carbon content and 13% oxygen content, the graphene has 43.42% carbon content and 2.02% hydrogen content, ascorbic acid has 54.56% oxygen content, hydrogen peroxide has 99.7% solid purity, absolute ethanol has liquid concentration of 30%, deionized water has liquid purity of 99.7%, nitric acid has liquid purity of 99.99%, nitrogen has liquid concentration of 4.3% and gaseous gas has 99.99% purity, (ii) (iia) adding 0.3672 plus minus 0.0001 g carbon micro-spheres, 20 ml nitric acid and 10 ml hydrogen peroxide into polytetrafluoroethylene container, placing in reaction kettle, (iib) transferring reaction kettle to heating furnace, heating and reacting at 110 plus minus 2 degrees C for 9 hours, cooling to 25 degrees C, (iic) washing using de-ionized water, washing and filtering, leaving filter cake, discarding the washing liquid, and (iid) drying filter cake at 60 degrees C under vacuum degree of 2 Pa for 12 hours in vacuum drying box to obtain functionalized modified carbon micro-sphere, (iii) (iiia) adding 0.025 plus minus 0.0001 g graphene and 5 plus minus 0.0001 ml de-ionized water into beaker, stirring and mixing to obtain graphene dispersion, (iiib) adding 0.05 plus minus 0.0001 g ascorbic acid and 0.005 plus minus 0.0001 g functionalized modified carbon microsphere into beaker and performing ultrasonic dispersion for 20 minutes, transferring into the lining of the reaction kettle, placing in heating furnace to perform hydrothermal synthesis reaction and heating at 100 plus minus 2 degrees C for 30 minutes, (iiic) transferring into refrigerator and freezing at -80 degrees C for 30 minutes, removing and naturally melting at room temperature, placing lining into the reaction kettle, continuously placing in heating furnace for hydro-thermal reaction and heating at 100 plus minus 2 degrees C for 480 minutes to form composite hydrogel, (iiid) removing composite hydrogel and placing in dialysis bag, adding 50 ml de-ionized water and sealing, placing dialysis bag in large beaker having 2000 ml capacity, adding de-ionized water and absolute ethanol into beaker, where the volume ratio of 2000 ml mixed solution is 20:1, submerging mixed solution in the dialysis bag, allowing to stand dialysis, repeating dialysis for 6 hours every time and stopping dialysis when the dialysis bag liquid color changes to colorless and transparent again, (iiie) freezing and curing composite hydrogel placed in the freezer at -78 degrees C for 60 minutes, freezing and drying at -80 degrees C under vacuum degree of 2 Pa for 48 hours into graphene composite aerogel, and (iiif) removing graphene composite aerogel and placing in vacuum heating furnace, annealing at 800 degrees C under nitrogen atmosphere for 2 hours to obtain graphene composite aerogel final product, (iv) using weights for mechanical compression performance test, performing shape analysis using field emission scanning electron microscope, using Fourier infrared spectrometer to surface functional group analysis, analyzing thermal stability of composite aerogel using thermogravimeter, analyzing diffraction intensity of graphene and graphene composite aerogel using X-ray diffractometer, where the graphene composite aerogel has a black cylindrical shape with a porosity of 99.56%, bulk density of 9.6 mg/cm3 and internal carbon microsphere size of less than or equal to 400 nm supported by the graphene sheets to form cross-linked three dimensional porous structure and the pore size in composite aerogel is less than or equal to 50 mu m, and (v) storing prepared graphene composite aerogel in a brown transparent glass container protected from moisture, sunscreen, acid and alkali corrosion at a storage temperature of 20 degrees C and relative humidity of 10%.