▎ 摘 要
NOVELTY - Preparing graphene two-dimensional powder using two-dimensional cellulose obtained by deep hydrolysis of cellulose as a raw material involves preparing a cellulose two-dimensional crystal raw material and a graphene two-dimensional powder. The preparation method of the cellulose two-dimensional crystal raw material involves: (1) preparing raw materials by taking plant fibers having a hollow tubular structure, or taking an initially purified pulp cellulose of a bagasse paper mill as a starting material; (2) carrying out acid solution treatment by immersing the biomass material in a dilute sulfuric acid solution, placing in a high temperature and high pressure resistant container and sealing the container, stewing the sealed container in a high-pressure sterilization pot for 110-130 minutes to complete the acid hydrolysis operation, taking out, drying in a centrifuge and washing with deionized water to obtain an acid-decomposed biomass; and (3) carrying out alkali solution treatment. USE - The method is useful for preparing a graphene two-dimensional powder using two-dimensional cellulose obtained by deep hydrolysis of cellulose. ADVANTAGE - The graphene two-dimensional powder has clear honeycomb hexagonal two-dimensional crystal structure, high carbon atom proportion, less heteroatom content and more than 6 layers, and can be mass-produced. The cellulose used in the graphene two-dimensional powder has wide source of raw materials, low cost and no secondary pollution during the preparation process, and is beneficial to ecological environment protection. DETAILED DESCRIPTION - Preparing graphene two-dimensional powder using two-dimensional cellulose obtained by deep hydrolysis of cellulose as a raw material involves preparing a cellulose two-dimensional crystal raw material and a graphene two-dimensional. The preparation method of the cellulose two-dimensional crystal raw material involves: (1) preparing raw materials by taking plant fibers having a hollow tubular structure, or taking an initially purified pulp cellulose of a bagasse paper mill as a starting material; (2) carrying out acid solution treatment by immersing the biomass material in a 4-6% dilute sulfuric acid solution, placing in a high temperature and high pressure resistant container and sealing the container, stewing the sealed container in a high-pressure sterilization pot for 110-130 minutes to complete the acid hydrolysis operation, taking out, drying in a centrifuge and washing 2-4 times with deionized water to obtain an acid-decomposed biomass; (3) carrying out alkali solution treatment by immersing the acid-decomposed biomass obtained in the step (2) in a 4-6% sodium hydroxide solution, placing in the high temperature and high pressure resistant container and sealing the container, stewing the sealed container in an autoclave for 110-130 minutes to complete the alkaline hydrolysis operation, taking out, drying in the centrifuge, and washing 2-4 times with deionized water to obtain an alkali-decomposed biomass; (4) carrying out formic acid solution treatment by immersing the alkali-decomposed biomass obtained in the step (3) in a 40-50% formic acid solution, then placing in a Teflon (RTM: PTFE) liner of a hydrothermal kettle, sealing the hydrothermal kettle, and heating in a muffle furnace at 115-125 degrees C for 170-190 minutes to obtain formic acid hydrolyzed cellulose; (5) carrying out formic acid reflux treatment by transferring the formic acid hydrolyzed cellulose obtained in the step (4) from the hydrothermal kettle liner to a three-necked flask and refluxing at 110 degrees C for 2 hours; and (6) carrying out liquid nitrogen freeze-drying by taking out the formic acid hydrolyzed cellulose obtained in the step (5) from the three-necked flask, placing in a centrifuge, drying, washing for 2-4 times with deionized water, then drying and separating by liquid nitrogen quick-drying method. The preparation method of petal-state graphene two-dimensional powder involves: (A) carrying out dehydration treatment on cellulose by placing the cellulose two-dimensional crystal powder in an atmosphere tubular electric furnace, heating the tubular furnace at 180 degrees C in an inert gas atmosphere, and heat preserving for more than 60 minutes under an atmospheric pressure to fully desorb water and adsorbed small molecules in the cellulose two-dimensional crystal powder and to complete dehydration treatment; (B) carrying out carbonization treatment on cellulose by heating the dried cellulose two-dimensional crystal powder raw material at 800 degrees C in an inert gas atmosphere, and heat preserving for more than 120 minutes under atmospheric pressure to sufficiently carbonize the cellulose two-dimensional crystal powder raw material; (C) carrying out graphitization on cellulose by heating the carbonized cellulose two-dimensional crystal powder raw material at 1000-1600 degrees C in an inert gas atmosphere for more than 240 minutes to fully graphitize the carbonized cellulose two-dimensional crystal powder raw material; and (D) annealing and cooling by cooling the graphitized two-dimensional crystal powder raw material to 300-400 degrees C in an inert gas atmosphere, and then cooling to room temperature along with a furnace.