CN110422839A - A kind of synthetic method of graphene - Google Patents
A kind of synthetic method of graphene Download PDFInfo
- Publication number
- CN110422839A CN110422839A CN201910723993.8A CN201910723993A CN110422839A CN 110422839 A CN110422839 A CN 110422839A CN 201910723993 A CN201910723993 A CN 201910723993A CN 110422839 A CN110422839 A CN 110422839A
- Authority
- CN
- China
- Prior art keywords
- graphene
- hours
- added
- nanometer sheet
- synthetic method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to technical field of graphene more particularly to a kind of synthetic method of graphene, which is to restore through strong reducing property metal using by halogenated aryl hydrocarbon class, obtain graphene film through coupling reaction.The graphene that preparation method through the invention obtains has the characteristics that high-conductivity.
Description
Technical field
The invention belongs to technical field of graphene preparation more particularly to a kind of synthesis sides of the graphene of high-conductivity
Method.
Background technique
Graphene is the material of two-dimensional nanostructure, has excellent light, electricity, magnetic and mechanical characteristic etc., is considered
Light, electricity, magnetic field all have huge application prospect.The electronic structure of graphene makes which give excellent electrology characteristics.Nothing
, still in application aspect, important meaning is all had by academic research.
Through retrieving, have 13 patent reports about graphene synthesis in the prior art: patent document (1) reports one
The method that kind simply prepares graphite as anode material for lithium-ion battery alkene nanometer sheet, utilizes ferric nitrate (Fe (NO3)3·9H2O), careless
The mixed solution of sour vanadyl and trimesic acid carries out hydro-thermal reaction by being transferred in hydrothermal reaction kettle, setting certain temperature and
Product is obtained after reaction time, after being washed, being dried, obtains persursor material, is then calcined, acidification, washing, is done
Graphene nanometer sheet is obtained after dry.Patent document (2) prepares ultra-thin graphene nanometer sheet using electrochemical method.Preparation process
In using lamellar graphite as anode, metal or graphite electrode are cathode, using liquid-phase system carboxylic-containing acid as electrolyte and intercalation
Source applies a constant current between the anode and cathode, is electrochemically reacted, and forms carboxylic acid intercalated graphite compounds, then
Carry out hot soarfing from and mechanical stripping, be repeated several times according to above step, the final average thickness that obtains is no more than 2nm or the number of plies not
Ultra-thin graphene nanometer sheet more than 5 layers.Patent document (3) discloses a kind of based on the slotting lithium removing preparation of electrolyte solvent heat
The method of single-layer graphene.Preparation process is using graphite as presoma, with the lithium hexafluoro phosphate (LiPF of 1mol/L6) electrolyte is
Solvent, in order to which lithium ion is embedded between graphite linings.Then by LiPF6Electrolyte/graphite precursor solution height
Pressure reaction kettle is transferred in air dry oven, carries out solvent thermal reaction.After reacting cooling, n-hexane, deionization are passed sequentially through
Water cleaning, the preparation of single-layer graphene is realized by techniques such as centrifuge separations.Patent document (4) disclose it is a kind of prepare it is more
The method of hole class graphene nanometer sheet: using linear type anthracene molecule as carbon source, by the hydrogen-oxygen of nano magnesia and grind into powder
Change potassium mixing after be used as template and activator, three according to suitable ratio ground and mixed it is uniform after, in the argon gas gas of flowing
Under atmosphere protection, anneals in tube furnace high temperature, obtain porous class graphene finally by the post-processing approach of pickling, washing
Nanometer sheet.Patent document (5) reports a kind of method for being used to prepare graphene nanometer sheet, by exposing intercalated graphite flakes
At a temperature of 1300~12000 DEG C, the control time expanded the intercalated graphite flakes rapidly less than 2 seconds, then will expansion
Graphite dispersion completes high pressure homogenization process in homogenizer in decentralized medium with the pressure higher than 35MPa.Realize graphite
The dispersion of alkene nanometer sheet, the lateral dimension of wherein at least 90% nanometer sheet are 50~50000nm, thickness between
Between 0.34~50nm.Patent document (6) reports a kind of overcritical sulfur hexafluoride removing of utilization and prepares graphene or graphite
The method of alkene nanometer sheet.Graphite and oxidant that mass ratio is 1:0.1~50 are added to autoclave, temperature reaches
Sulfur hexafluoride is pumped into after preset value, the purpose is to then set certain reaction temperature and time as intercalation stripping agent, super
It is depressurized to normal pressure after circulating under critical pressure and temperature, which moves in circles, finally by Optimizing Process Parameters,
Realize the preparation of the graphene and graphene nanometer sheet of different diameters and thickness.Patent document (7) reports one kind with graphite
Powder is raw material, the flow reactor designed by three, completes the oxidation of graphite powder, dialysis purification, drying and crushing, heat also
The processes such as original expansion removing and post-processing realize the serialization large-scale production of graphene nanometer sheet.Patent document (8) mentions
Gone out a kind of method for preparing graphene nanometer sheet: early period handles graphite expansion, causes followed by gas phase high velocity impact
The removing of graphene nanometer sheet obtains graphene nanometer sheet finally by grinding or removing, can be used for preparing graphene and receive
Rice piece slurry and the conductive coating formed by graphene nanometer sheet slurry.Patent document (9) report it is a kind of it is simple and easy,
Preparation method that is low in cost, being easy to be mass produced graphene nanometer sheet.Using solid high-polymer stable dispersion system, lead to
The untreated graphite material of mechanical lapping is crossed, promotes the removing of graphite during the grinding process and realizes graphite alkylene and obtain greatly
Batch graphene nano sheet material.In this process, solid high-polymer and graphene nanometer sheet are sufficiently mixed on nanoscale
It closes, prevents the graphene nanometer sheet separated from stacking again.Solid high-polymer is removed in last handling process, is finally obtained
Graphene nanometer sheet is obtained, is single-layer or multi-layer with a thickness of 0.35nm~7nm.Hydrophily high polymer assigns graphene simultaneously
Nanometer sheet surface it is hydrophilically modified, this gained graphene nanometer sheet be also used as water system conductive coating application.Patent document
(10) a kind of preparation process of efficient stannic oxide/graphene nano piece is disclosed, using improved Hummers method by common graphite
Powder is prepared into graphene oxide, potassium permanganate is then added and with microwave stove heating, obtains porous oxidation graphene and titanium dioxide
Manganese mixture, it is repeated multiple times to obtain porous oxidation graphene using dilute hydrochloric acid and deionized water centrifuge washing then super with water-bath
Sound is ultrasonically treated, and target product is finally obtained.In the stannic oxide/graphene nano piece aqueous solution sample feature be size it is small,
Narrow distribution range, stable dispersion.It is compound that patent document (11) reports a kind of graphene nanosheet/conductingpolymer polymer nanowire
The preparation method of material, the preparation part about graphene nanometer sheet is to prepare graphite oxide using chemical oxidization method, is passed through
Ultrasound obtains stannic oxide/graphene nano piece suspension, adjusts pH value to 9~10 with sodium hydroxide, sodium borohydride is added to
It states in suspension, is stirred 1~2 hour at 80~90 DEG C, realize and partial reduction is carried out to graphene oxide, finally by true
Empty pump filter and washing obtain graphene nanometer sheet.Patent document (12) disclose prepared using Electron Beam Irradiation it is graphene-based
Nano material: aoxidizing natural graphite obtain graphite oxide first, is then 10~30 according to weight ratio by graphene oxide
It is dissolved in ethyl alcohol, obtains ethanol solution.Deionized water is mixed for 20~5 ratio by volume with the ethanol solution again, is obtained
To mixed solution, the electron beam irradiation of progress 70-560kGy irradiation dose after free radical scavenger is added, is finally centrifugated,
By gained precipitating deionized water and washes of absolute alcohol, graphene-based nanometer powder is ground to obtain in drying.Patent document (13)
It discloses one kind and prepares nitrogen-doped graphene/metal composite method and products thereof and application from bottom to top.About combining unit
Point, using the carbon matrix precursor of different ratio, two dimension pattern plate presoma MA and metal precursor grind 30 in mortar at room temperature
Minute to be uniformly mixed, is subsequently placed in ceramic crucible with cover, and calcining successfully obtains nitrating in tube furnace under nitrogen protection
Graphene/metal composite.
Graphene is as a kind of two-dimensional material in fields such as light, electricity, magnetic with excellent properties, property and size, thickness
Degree and internal structure have much relations.We are reacted by molecule coupling labeled synthesizes large stretch of graphene nano structure, makes it have excellent
Different electric property provides a kind of new material for having excellent properties in research fields such as microelectronics for graphene.
Existing technical literature
Patent document
Patent document 1:CN201810554220.7
Patent document 2:CN201810374798.4
Patent document 3:CN201810063248.0
Patent document 4:CN201810043202.2
Patent document 5:CN201580032693.5
Patent document 6:CN201710138178.6
Patent document 7:CN201410565486.3
Patent document 8:CN201310757079.8
Patent document 9:CN201310628699.1
Patent document 10:CN201510143599.9
Patent document 11:CN201210167617.3
Patent document 12:CN200910052042.9
Patent document 13:CN201410307271.1
Summary of the invention
Technical problems to be solved by the inivention
The object of the present invention is to provide a kind of wet chemical synthesis of graphene.
Method for solving technical problem
In view of the above-mentioned problems, the invention proposes a kind of synthetic methods of graphene comprising following steps:
1) at room temperature, using toluene as solvent, hexabromo benzole soln is configured, active metal is then added in the solution；Activity
Metal selects any in sodium, lithium and magnesium；
2) mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, heating is reacted；
3) sediment obtained after step 2) reaction is washed with dehydrated alcohol, deionized water centrifuge washing, washing is added
Product is dialysed, and graphene nanometer sheet aqueous solution is obtained；Continue to be washed to solution supernatant in after colourless to solid product,
It is dried to obtain solid graphene powder.
A kind of embodiment is, wherein the molar ratio of hexabromobenzene and sodium in step 1) are as follows: 0.0694:1~0.625:1.
A kind of embodiment is, wherein in step 2), heats 24~72 hours in 170~200 DEG C of temperature ranges.
A kind of embodiment is, wherein in step 3), be added deionized water centrifuge washing first pass wash product into
It dialyses within row 72 hours.
A kind of embodiment is, wherein when dry, drying temperature is 60-90 DEG C, >=12 hours dry.
The beneficial effects of the present invention are:
It is raw materials used in synthetic method of the present invention to be easy to get, simple process, synthesized high-quality graphene nanometer chip size
Greatly, thickness is small, while having the characteristics that spinning electron is highly concentrated.
From the description of following exemplary embodiment, further characteristic of the invention will become obvious.
Detailed description of the invention
Fig. 1: (a), (b) be embodiment 1 transmission electron microscope photo.
Fig. 2: (a), (b) be embodiment 2 transmission electron microscope photo.
Fig. 3: (a), (b) be embodiment 3 transmission electron microscope photo.
Fig. 4: (a), (b) be embodiment 4 transmission electron microscope photo.
Fig. 5: (a), (b) be embodiment 5 transmission electron microscope photo.
Fig. 6: (a), (b) be embodiment 6 transmission electron microscope photo.
Fig. 7: (a), (b) be embodiment 7 transmission electron microscope photo.
Fig. 8: (a), (b) be embodiment 8 transmission electron microscope photo.
Fig. 9: (a), (b) be embodiment 9 transmission electron microscope photo.
Figure 10: (a), (b) be embodiment 10 transmission electron microscope photo.
Figure 11: (a), (b) be embodiment 11 transmission electron microscope photo.
Figure 12: (a), (b) be embodiment 12 transmission electron microscope photo.
Figure 13: (a), (b) be embodiment 13 transmission electron microscope photo.
Figure 14: (a), (b) be embodiment 14 transmission electron microscope photo.
Specific embodiment
An embodiment of the disclosure is specifically described below, but the disclosure is not limited to this.
Embodiment
By embodiment, the present invention will be described in more detail, but the present invention is not limited to following embodiments.It should be noted that
As long as not special declaration, " part " expression " mass parts ".
Embodiment 1:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 24 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 1 (a), the graphene nano structure that (b) is embodiment 1.
Embodiment 2:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 2 (a), the graphene nano structure that (b) is embodiment 2.
Embodiment 3:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 72 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 3 (a), the graphene nano structure that (b) is embodiment 3.
Embodiment 4:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.6 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 180 DEG C of temperature ranges
Heating 55 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 4 (a), the graphene nano structure that (b) is embodiment 4.
Embodiment 5:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 190 DEG C of temperature ranges
Heating 24 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 5 (a), the graphene nano structure that (b) is embodiment 5.
Embodiment 6:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 200 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 6 (a), the graphene nano structure that (b) is embodiment 6.
Embodiment 7:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.08 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 7 (a), the graphene nano structure that (b) is embodiment 7.
Embodiment 8:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.12 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 8 (a), the graphene nano structure that (b) is embodiment 8.
Embodiment 9:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.2484 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Fig. 9 (a), the graphene nano structure that (b) is embodiment 9.
Embodiment 10:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.0 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.3312 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Figure 10 (a), the graphene nano structure that (b) is embodiment 10.
Embodiment 11:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 0.5 gram/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Figure 11 (a), the graphene nano structure that (b) is embodiment 11.
Embodiment 12:
With hexabromobenzene (C6Br6), metallic sodium be raw material, at room temperature, using toluene as solvent, configure 1.5 grams/400 milliliters
Hexabromo benzole soln, then in the solution be added 0.1 gram of metallic sodium.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 170 DEG C of temperature ranges
Heating 48 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Figure 12 (a), the graphene nano structure that (b) is embodiment 12.
Embodiment 13:
Using hexabromobenzene (C6Br6), lithium metal as raw material, at room temperature, using toluene as solvent, 0.1 gram/40 milliliters are configured
Hexabromo benzole soln, then in the solution be added 0.0183 gram of lithium metal.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 180 DEG C of temperature ranges
Heating 50 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Figure 13 (a), the graphene nano structure that (b) is embodiment 13.
Embodiment 14:
Using hexabromobenzene (C6Br6), magnesium metal as raw material, at room temperature, using toluene as solvent, 0.1 gram/40 milliliters are configured
Hexabromo benzole soln, then in the solution be added 0.0313 gram of magnesium metal.
The mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, in 180 DEG C of temperature ranges
Heating 50 hours.
After the sediment obtained after reaction is washed repeatedly through dehydrated alcohol, the of deionized water centrifuge washing is added
A time washing product dialyse within 72 hours, and graphene nanometer sheet aqueous solution can be obtained.Solid product is continued to be washed to molten
After liquid supernatant is in colourless, it is put into drying box (60 DEG C) and is dried 12 hours to get solid graphene powder is arrived.
The transmission electron microscope photo of Figure 14 (a), the graphene nano structure that (b) is embodiment 14.
This embodiment is merely preferred embodiments of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with scope of protection of the claims
Subject to.
Claims (5)
1. a kind of synthetic method of graphene, which comprises the following steps:
1) at room temperature, using toluene as solvent, hexabromo benzole soln is configured, active metal is then added in the solution；Active metal
It selects any in sodium, lithium and magnesium；
2) mixed solution is placed in the stainless steel cauldron of a polytetrafluoroethyllining lining, heating is reacted；
3) sediment obtained after step 2) reaction is washed with dehydrated alcohol, deionized water centrifuge washing is added, washes product
It dialyses, obtains graphene nanometer sheet aqueous solution；Continue to be washed to solution supernatant in after colourless to solid product, dry
To solid graphene powder.
2. synthetic method according to claim 1, wherein the molar ratio of hexabromobenzene and active metal in step 1) are as follows:
0.0694:1~0.625:1.
3. synthetic method according to claim 1, wherein in step 2), 170~200 DEG C of temperature ranges heating 24~
72 hours.
4. synthetic method according to claim 1, wherein in step 3), the first pass of deionized water centrifuge washing is added
Washing product is dialysed.
5. synthetic method according to claim 1, wherein when dry, drying temperature is 60-90 DEG C, >=12 hours dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910723993.8A CN110422839B (en) | 2019-08-07 | 2019-08-07 | Synthetic method of graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910723993.8A CN110422839B (en) | 2019-08-07 | 2019-08-07 | Synthetic method of graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110422839A true CN110422839A (en) | 2019-11-08 |
| CN110422839B CN110422839B (en) | 2021-03-16 |
Family
ID=68412967
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910723993.8A Active CN110422839B (en) | 2019-08-07 | 2019-08-07 | Synthetic method of graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110422839B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112645312A (en) * | 2020-12-21 | 2021-04-13 | 北京理工大学 | Crystalline nanopore graphene, preparation method and oxygen-doped crystalline nanopore graphene |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462719A (en) * | 2009-01-16 | 2009-06-24 | 北京大学 | Preparation of graphene |
| CN102408107A (en) * | 2010-09-26 | 2012-04-11 | 中国科学院上海硅酸盐研究所 | Method for preparing high-quality graphene |
| CN104058399A (en) * | 2014-07-17 | 2014-09-24 | 山东理工大学 | Direct preparation method of high-purity high-quality graphene |
| CN104201357A (en) * | 2014-09-18 | 2014-12-10 | 温州大学 | Graphene quantum dot-graphene composite material as well as preparation method and application thereof |
-
2019
- 2019-08-07 CN CN201910723993.8A patent/CN110422839B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462719A (en) * | 2009-01-16 | 2009-06-24 | 北京大学 | Preparation of graphene |
| CN102408107A (en) * | 2010-09-26 | 2012-04-11 | 中国科学院上海硅酸盐研究所 | Method for preparing high-quality graphene |
| CN104058399A (en) * | 2014-07-17 | 2014-09-24 | 山东理工大学 | Direct preparation method of high-purity high-quality graphene |
| CN104201357A (en) * | 2014-09-18 | 2014-12-10 | 温州大学 | Graphene quantum dot-graphene composite material as well as preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112645312A (en) * | 2020-12-21 | 2021-04-13 | 北京理工大学 | Crystalline nanopore graphene, preparation method and oxygen-doped crystalline nanopore graphene |
| CN112645312B (en) * | 2020-12-21 | 2022-05-20 | 北京理工大学 | Crystalline nanopore graphene, preparation method and oxygen-doped crystalline nanopore graphene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110422839B (en) | 2021-03-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | One-step hydrothermal synthesis of a TiO2-Ti3C2Tx nanocomposite with small sized TiO2 nanoparticles | |
| CN106315695B (en) | A kind of strawberry-like cobalt acid nickel nano material and preparation method thereof | |
| Sun et al. | Synthesis and adsorption properties of Li1. 6Mn1. 6O4 by a combination of redox precipitation and solid-phase reaction | |
| Zhu et al. | Scalable synthesis of hierarchical hollow Li4Ti5O12 microspheres assembled by zigzag-like nanosheets for high rate lithium-ion batteries | |
| CN104448305B (en) | A kind of nano combined absorbing material and preparation method thereof | |
| CN108539165A (en) | Antimony oxide/redox graphene nanocomposite and its preparation and application | |
| CN106410199B (en) | A kind of lithium ion battery graphene/ferro-tin alloy composite negative pole material preparation method | |
| CN107651708A (en) | A kind of method that microwave hydrothermal prepares 1T@2H MoS2 | |
| CN104752074B (en) | A kind of preparation method of molybdenum oxide/carbon bead composite | |
| Jokar et al. | Growth control of cobalt oxide nanoparticles on reduced graphene oxide for enhancement of electrochemical capacitance | |
| CN107934965A (en) | A kind of Ti3C2‑Co(OH)(CO3)0.5The preparation method of nanocomposite | |
| Modafferi et al. | Transition metal oxides on reduced graphene oxide nanocomposites: Evaluation of physicochemical properties | |
| CN113000061B (en) | Preparation method of banded graphite carbon nitride nanosheets | |
| CN111099650A (en) | CeO2Molten salt method for synthesizing nano spherical particles | |
| Zhou et al. | Polymerization inspired synthesis of MnO@ carbon nanowires with long cycling stability for lithium ion battery anodes: growth mechanism and electrochemical performance | |
| CN108183204A (en) | A kind of silicon nanometer sheet-graphene nanometer sheet composite material and preparation and application | |
| CN111792669B (en) | TiO 22Nano-rod/multilayer graphene composite material and preparation method thereof | |
| Zhang et al. | The effect of ultrasound on synthesis and energy storage mechanism of Ti3C2Tx MXene | |
| CN107098341A (en) | Graphene oxide new type water thermal stencil agent and its preparation method of nano composite material | |
| Hong et al. | Synthesis of 3D-structured Li4Ti5O12 from titanium (IV) oxysulfate (TiOSO4) solution as a highly sustainable anode material for lithium-ion batteries | |
| Zhang et al. | Facile fabrication of elastic CoO@ graphene aerogel for recycled degradation of chloramphenicol | |
| CN113351230A (en) | Isolated cobalt atom doped single-layer or few-layer MoS2Process for preparing catalyst | |
| CN110422839A (en) | A kind of synthetic method of graphene | |
| Sluban et al. | Role of water in the transformation of protonated titanate nanoribbons to anatase nanoribbons | |
| CN105420794B (en) | A kind of preparation method of graphene/ferriferrous oxide composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |