• 专利标题:   Preparing highly dispersed nickel cobalt manganate composition graphene comprises e.g. adding graphite powder into concentrated sulfuric acid, potassium sulfate, phosphorus oxide, and placing in a water bath, washing in deionized water.
  • 专利号:   CN111106327-A
  • 发明人:   CHEN G, SHI R, XIE X
  • 专利权人:   SHENZHEN YUPENG NEW ENERGY VEHICLE TEST
  • 国际专利分类:   H01M010/0525, H01M004/36, H01M004/505, H01M004/525, H01M004/62
  • 专利详细信息:   CN111106327-A 05 May 2020 H01M-004/36 202041 Pages: 9 Chinese
  • 申请详细信息:   CN111106327-A CN11272247 26 Oct 2018
  • 优先权号:   CN11272247

▎ 摘  要

NOVELTY - Preparing highly dispersed nickel cobalt manganate composition graphene comprises e.g. adding graphite powder into concentrated sulfuric acid, potassium sulfate, phosphorus oxide, and placing in a water bath, washing in deionized water to neutrality and drying, measuring concentrated sulfuric acid in an ice-water bath and cooling, adding pre-oxidized graphite powder and sodium nitrate to concentrated sulfuric acid under stirring, then slowly adding potassium nitrate, maintaining the temperature, and stirring, this stage is a low temperature reaction, placing the beaker in constant-temperature water bath, after the temperature of the reaction liquid increases, continuing stirring to complete the medium-temperature reaction, carrying out high temperature reaction, adding deionized water to the stirring to control the reaction, and continuing stirring, diluting the reaction solution to with deionized water, and treating the reaction solution. USE - The method is useful for preparing highly dispersed nickel cobalt manganate composition graphene. ADVANTAGE - The method: produces highly dispersed nickel cobalt manganate composition graphene, which produces has high purity, lithium nickel cobalt manganate particles, which are highly dispersed on graphene, is rich in mesoporous, can electrochemical tests, which has high gram capacity and good cycle performance. DETAILED DESCRIPTION - Preparing highly dispersed nickel cobalt manganate composition grapheme comprises (i) adding 5 g graphite powder into 12 ml concentrated sulfuric acid, 2.5 g potassium sulfate, 2.5 g phosphorus oxide, and placing in a water bath at 80 degrees C for 6 hours, washing with 250 ml deionized water to neutrality and drying, measuring 46 ml concentrated sulfuric acid in an ice-water bath and cooling to 0 degrees C, adding 2 g pre-oxidized graphite powder and 1 g sodium nitrate to concentrated sulfuric acid under stirring, then slowly adding potassium nitrate, maintaining the temperature to 20 degrees C, and stirring for 15 minutes, this stage is a low temperature reaction, placing the beaker in constant-temperature water bath at 35 degrees C, after the temperature of the reaction liquid increases to 35 degrees C, continuing stirring for 30 minutes to complete the medium-temperature reaction, carrying out high temperature reaction, adding deionized water to the stirring to control the reaction to be less than 98 degrees C, and continuing stirring for 30 minutes, diluting the reaction solution to 280 ml with deionized water, treating the reaction solution with 3% hydrogen peroxide to reduce potassium permanganate and manganese dioxide to colorless manganese sulfate and filtering while hot, gradually washing with 5% hydrochloric acid and deionized water until the filtrate is free of sulfate (SO42-) (detected with barium chlroide), and graphene oxide (GO) sol (density of 0.01 g/ml); (ii) dissolving nickel nitrate hexahydrate, cobalt nitrate hexahydrate and 50% manganese nitrate solution in 50 ml deionized water, carrying out ultrasonic for 5 minutes, and preparing into nickel: cobalt for the mixed metal salt solution with manganese(ii) at a molar ratio of 8:1:1, the total cation concentration is 1 mol/l, then adding 100 ml graphene oxide (GO) sol, and stirring magnetically at room temperature for 0.5 hours to obtain mixed solution, then adding 15 g urea to it, and continuously to magnetically stirring for 0.5 hour at room temperature; (ii) transferring the mixed solution to a 200 ml reaction kettle, reacting at 8-24 hours at 100-160 degrees C, cooling at room temperature, centrifuging, washing for three times with deionized water and absolute ethanol, and vacuum-drying at 80 degrees C for 24 hours to obtain a nickel-cobalt-manganese oxide composition graphene precursor; (iv) placing the precursor prepared in step (iii) in a tube furnace, adding lithium fluoride, calcining at 1 degrees C/ minute to 400-600 degrees C under argon atmosphere for 4 hours to obtain nickel-cobalt-manganese oxide graphene composition.