• 专利标题:   Preparing silicon ether alkyl lithium comprises e.g. placing polished lithium sheet in stainless steel boat, heating, immersing graphene paper in molten lithium, injecting molten lithium into graphene paper and mixing with halogenated silicon ether, adding non-polar solvent, reacting, filtering.
  • 专利号:   CN113754690-A, CN113754690-B
  • 发明人:   QIAN D, ZHOU Y, SHEN W, WU X, DAI Y, DONG T, XIE Y, CAO P, ZHU A, JIANG G, CHENG L, SHI X, CHU P, ZHOU W
  • 专利权人:   JIANGSU CHANGJILI NEW ENERGY TECHNOLOGY
  • 国际专利分类:   C07F007/18
  • 专利详细信息:   CN113754690-A 07 Dec 2021 C07F-007/18 202209 Chinese
  • 申请详细信息:   CN113754690-A CN11024032 02 Sep 2021
  • 优先权号:   CN11024032

▎ 摘  要

NOVELTY - Preparing silicon ether alkyl lithium comprises e.g. dispersing nickel-manganese alloy powder in hot ammonium sulfate solution, filtering, dispersing in mixed solution of polyvinylpyrrolidone and glacial acetic acid, filtering out, washing and drying in vacuum, placing the metal powder in an alumina ceramic boat, incubating, carrying out annealing treatment, carrying out the growth deposition of few-layer graphene, cooling, and drying to obtain black-gray powder product, dispersing and dissolving the black-gray powder product and chromium trioxide in hydrochloric acid solution, reacting, separating, dispersing the washed precipitate in deionized water to obtain dispersion liquid, filtering, freeze-drying, immersing the carbon fiber paper in hydroiodic acid solution to obtain graphene paper, immersing the graphene paper in molten lithium, mixing the halogenated silicon ether and the lithium-supported graphene paper, adding non-polar solvent, reacting and filtering. USE - The method is useful preparing silicon ether alkyl lithium. ADVANTAGE - The silicon ether alkyl lithium has good dispersibility, so that the synthesis reaction is sufficient, with high yield, low impurity and easy to separate. DETAILED DESCRIPTION - Preparing silicon ether alkyl lithium comprises (a) dispersing nickel-manganese alloy powder in hot ammonium sulfate solution, keeping warm, allowing to stand for 6-12 hours and filtering out, dispersing in the mixed solution of polyvinylpyrrolidone and glacial acetic acid, filtering out, washing with deionized water and absolute ethanol in turn, and drying in vacuum, placing the metal powder in an alumina ceramic boat and moving into the middle of the tube furnace, closing the tube furnace, evacuating the air in the tube, and filling argon, in an argon atmosphere, raising the temperature to 900-1000degrees Celsius at a rate of 5-8degrees Celsius/minute, incubating for 10-20 minutes, carrying out annealing treatment under the argon-hydrogen mixed atmosphere of volume ratio (20-30):1, annealing time is 3-5 minutes, switching the atmosphere to argon-hydrogen-pyridine mixed atmosphere in volume ratio of (12-18):(8-12):1, carrying out the growth deposition of few-layer graphene for 20-30 minutes, completing the deposition, cooling, washing the deposited product with a hydrochloric acid solution, and drying to obtain a black-gray powder product, where the concentration of polyvinylpyrrolidone in the mixed solution of polyvinylpyrrolidone and glacial acetic acid is 1 g/50 ml, (b) dispersing and dissolving the black-gray powder product and chromium trioxide respectively in the hydrochloric acid solution, stirring and reacting at room temperature for 1-2 hours, separating the precipitate, adding the precipitate into 10% hydrogen peroxide for rinsing and soaking, separating the precipitate, washing with deionized water, dispersing the washed precipitate in deionized water to obtain a dispersion liquid with a dispersion ratio of 4-8 mg/ml, filtering the dispersion on carbon fiber paper, freeze-drying, immersing the carbon fiber paper in a hydroiodic acid solution, rinsing deionized water to neutrality, and drying to obtain graphene paper, where the concentration of the hydrochloric acid solution is 2-10 mol/l, and the mass ratio of the black-gray powder product to the chromium trioxide and the hydrochloric acid solution is 1:8.5:(8.5-10), the soaking concentration of the hydroiodic acid solution is 10 wt.%, the soaking time is 1-5 minutes, and the soaking temperature is 30-60degrees Celsius, (c) placing the polished lithium sheet in a stainless steel boat under the protection of argon atmosphere, heating to 300degrees Celsius to melt the lithium sheet, immersing the graphene paper in molten lithium, injecting the molten lithium into the graphene paper through the pores, and the color changes from black to silver-gray, so that the lithium loading amount is 4-8 mg/cm to obtain the lithium-loaded graphene paper, where the content of water and oxygen in the argon atmosphere is lower than 1 ppm, and (d) mixing the halogenated silicon ether and the lithium-supported graphene paper under the protective atmosphere of argon, adding into a non-polar solvent with 1-3 times the volume of the halogenated silicon ether, reacting at 20-50degrees Celsius for 2-5 hours, and filtering the reaction product, where the molar ratio of the halogenated silicon ether to the lithium in the lithium-supported graphene paper is 1:(1-8).