CN105480970A - Low-cost production method for sheet carbon material powder - Google Patents
Low-cost production method for sheet carbon material powder Download PDFInfo
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- CN105480970A CN105480970A CN201610018123.7A CN201610018123A CN105480970A CN 105480970 A CN105480970 A CN 105480970A CN 201610018123 A CN201610018123 A CN 201610018123A CN 105480970 A CN105480970 A CN 105480970A
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- carbon black
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the field of material chemistry, and particularly relates to a low-cost production method for sheet carbon material powder. The sheet carbon material is one of nanometer graphite sheets, graphene and oxidized graphene. The method is characterized in that a large amount of excessive energy and carbon black tail gas will be generated in the carbon black production process, and sheet carbon material filter cakes or slurry obtained through liquid phase stripping contains a large amount of liquid, so that heat generated in the carbon black production process or carbon black tail gas combustion is used for being supplied to the drying process of the sheet carbon material obtained through liquid phase stripping, the drying energy consumption and the production cost of the production process of the sheet carbon material powder can be greatly lowered, the good industrial potential is achieved, and formation of circular economic benefits between sheet carbon material powder production and carbon black production is facilitated. In the carbon black production process, high-temperature hot air generated by an air preheater or purified carbon black tail gas can be both used as the heat source for the step of drying the sheet carbon material obtained through liquid phase stripping.
Description
Technical field
The invention belongs to technical field of material chemistry, is a kind of Low-cost production method of sheet carbon material powder more specifically.
Background technology
Since 2004 are found by scientists such as the Geim of Univ Manchester UK, the investigation and application of Graphene is operated in extensively is carried out (NovoselovK.S. all over the world, GeimA.K., MorozovS.V., etal.Electricfieldeffectinatomicallythincarbonfilms [J] .Science, 2004,306 (5696): 666-669).Graphene is a kind of by SP
2the planar sheet nano-carbon material that hydbridized carbon atoms is formed, theoretical heat-conduction coefficient 5000W/m.K, theoretical specific surface area 2630m
2/ g, individual layer specific absorbance only has 2.3%.Be the material that known theoretical strength is the highest, there is the good transparency, electroconductibility and thermal conductivity simultaneously, be expected to there is broad prospect of application in matrix material, energy storage material, electronic material, optics etc.Graphene oxide is the derivative of Graphene, remains the outstanding character of a lot of Graphene.Nano graphite flakes, Thickness Ratio Graphene is thick, but production cost is low, compares Graphene and more easily produces.Nano graphite flakes, Graphene or graphene oxide are all the one in sheet carbon material.
At present, the production technology of sheet carbon material powder comprises mechanically peel method, liquid phase stripping method, oxidation reduction process, chemical Vapor deposition process, thermolysis SiC method, electrochemical process etc.Liquid phase stripping method, has the possibility realizing large-tonnage, high quality sheet carbon material power production.Wherein, based on Hummer method, utilize strong acid to carry out oxide treatment to graphite, obtain graphite oxide, then adopt various technique to peel off its degree of depth liquid phase, can graphene oxide be obtained.If on the basis of graphene oxide, finally add that reduction treatment step can also obtain Graphene.Directly in organic solvent to crystalline flake graphite liquid phase stripping method, also high-quality thin graphene can be obtained.(the NatnaelBehabtu such as the JamesM.Tour of the U.S., JayR.Lomeda, MicahJ.Green, etal.Spontaneoushigh-concentrationdispersionsandliquidcr ystalsofgrapnene [J] .NatureNanotechnology5,406-411 (2010)) utilize super acids-chlorsulfonic acid to carry out liquid phase stripping to graphite, based on the strong protonation of super acids, super acids easily enters the laminated structure of graphite, overcome the Van der Waals force between graphite flake layer, peel away Graphene.Obtain Graphene-super acids dispersion liquid in stirring after 2-3 days, directly wherein there is a large amount of single-layer graphenes in observation dispersion liquid.Add water decomposition chlorsulfonic acid, carry out filtration washing drying, just can obtain graphene powder.
Graphite is a kind of typical intercalation compound, when being subject to shearing force, easily sliding and being stripped out between layer and layer.When ball milling, powerful shearing force can be provided to promote the stripping each other of graphite flake layer.The Huanghai Sea waits and adopts the stirring ball-milling equipment (Huanghai Sea, be coated with river equality. the preparation of sheet nano graphite and the friction and wear behavior [J] as lubricating oil additive thereof. friction journal, 25th volume the 4th phase), take natural graphite as raw material take water as medium, liquid phase ball milling separates the nano graphite flakes of more than thickness 10nm.Ball milled equipment and process is simple, is easy to realize large-tonnage and produces.
Due to the characteristic of sheet carbon material, its sheet footpath and thickness larger, specific surface area is from common 40m
2/ g to 2630m
2/ g.After liquid phase has been peeled off, sheet carbon material has adsorbed a large amount of liquid mediums.No matter adopt press filtration to obtain sheet carbon material filtration cakes torrefaction or adopt the dispersion liquid Direct spraying of sheet carbon material dry, wherein all contain a large amount of moisture or organic liquid, wherein 1%-30% is sheet carbon material, wherein 70%-99% is liquid, dry energy consumption is very high, considerably increases its production cost.
Summary of the invention
The object of the present invention is to provide a kind of Low-cost production method of sheet carbon material powder, by significantly reducing the cost of its drying step, thus reducing the comprehensive production cost of sheet carbon material powder.
Technical scheme of the present invention is:
A kind of Low-cost production method of sheet carbon material powder, use liquid phase stripping technology, drying obtains sheet carbon material powder, wherein sheet carbon material is the one in nano graphite flakes, Graphene or graphene oxide, it is characterized in that: the heat that the heat of sheet carbon material powder drying process comes from carbon black process or produces in carbon black tail gas burning.
The production system of carbon black can produce a large amount of excess energies, and these energy can be used for dry sheet carbon material used completely, thus save a large amount of production costs.Particularly, carbon black is the black powder material generated through incomplete combustion or pyrolysis under the strict processing condition controlled by hydro carbons.The industrial production mainly Audit For Process route of carbon black, the output of oil oven carbon black has accounted for 70% ~ 90% of carbon black total amount.The fuel of Audit For Process can be Sweet natural gas, coke(oven)gas or liquid hydrocarbon, and high aromatic oil material then selected by raw material, as ethylene bottom oil and carbolineum etc.Carbon black raw oil sprays in burned flame after atomization, under the high temperature of about 2000 DEG C, form carbon black smoke.Flue gas contains excessive heat energy, and temperature is too high, needs to spray into water coolant, carries out a chilling and temperature is reduced to about 1000 DEG C.After once cooling, send air preheater, oil preheater lowers the temperature further, the dump energy of recovery part, finally sprays into secondary cooling water, and temperature is dropped to less than 250 DEG C, just can enter bag filter, collect.Even if through multi step strategy, in the tail gas of production of carbon black, also has a large amount of dump energy.Carbon black tail gas filters carbon black smoke through main bag filter in production of carbon black to produce, and main component is (volume parts): H
2, 10-12%; CO, 9-13%; CO
2, 2-3%; N
2, 36-38%; H
2o, 36-40%; H
2s (mg/m3), 250-800 (carbon black tail gas composition changes with the kind of carbon black difference of producing).Carbon black tail gas is a kind of calorific value inflammable gas (low heat value Q on the low side
dw=500-700Kcal/Nm
3), it contains the combustible gas such as H2, CO, and its content only accounts for about 20% of carbon black tail gas total amount.But the tail gas output in production of carbon black is very large, and the total energy contained by it is roughly equal to about the 30-40% of production of carbon black total energy, produces carbon black per ton and can produce about 10
4m
3the carbon black tail gas of left and right.At present, the domestic process to carbon black tail gas mainly contains following two kinds of approach.A kind of approach is direct high altitude discharge after incinerator burns, although the basic meet the requirement of environmental protection of this way, effectively do not utilize thermal source, tail gas low heat value is about 510-630Kcal/Nm
3(carbon black tail gas low heat value is different with production kind of carbon black difference), economy is bad.Another is by boiler combustion, produces steam for production, life or the generating of drive turbine LP rotors.Current carbon black tail gas utilizes due to a variety of causes, also there is carbon black tail gas electricity generation grid-connecting difficulty, the phenomenon that carbon black tail gas is not fully used.
The drying of sheet carbon material powder is due to moisture or organic solvent amount large, and dry energy consumption is high, by utilizing the excess energy of carbon black production system, can produce enough heats used for the drying of sheet carbon material, can form efficiency of cycling economy like this.Both be conducive to the energy-saving and emission-reduction of carbon black industry, also greatly can reduce the production cost of sheet carbon material.
Carbon black tail gas through pre-treatment, can also improve combustion gas quality as before fuel heat supply.After removing most of water vapour, sulfide and nitrogen, the calorific value of carbon black tail gas even can bring up to 3000Kcal/Nm
3left and right.
In addition, can also take the advanced row emission power generation of carbon black tail gas, then electrically heated mode is for the electrical heating device of sheet carbon material powder drying.Such mode, can digest the electric energy that carbon black tail gas transforms on the spot, does not need electrical network to be transported to other place, favourable formation recycling economy.
Accompanying drawing explanation
Accompanying drawing illustrates the Graphene stereoscan photograph that the embodiment of the present invention 1 is produced.
Specific embodiment mode
Further illustrate the present invention below in conjunction with drawings and the specific embodiments mode, accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.Some nonessential improvement that those skilled in the art make according to foregoing of the present invention and adjustment all belong to the scope of protection of the invention.Examples below concrete time, charging capacity etc. is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
Fixed carbon content 98% granularity 80 object crystalline flake graphite is used to be raw material, 100 kilograms of crystalline flake graphites are placed in the mixing acid of 400 kilograms of perchloric acid (70% concentration) and 15 kilograms of nitric acid (65% concentration), are heated to 90 DEG C of dip treating 20 minutes.Then, vacuum filtration isolates filtrate, is washed by the crystalline flake graphite of acidleach, dries, just obtain the compound between graphite layers of sour intercalation.Compound between graphite layers, 900 DEG C of thermal expansions, expands 400 times in 15 seconds, obtains expanded graphite.Get 10 kilograms of expanded graphites, add 990 liters of N-Methyl pyrrolidone, stir into liquid form mixt, carry out circulating ultrasonic stripping with the ultrasonic wave liquid towards mixture of 50 every root power 2KW, logical water coolant guarantees that liquid form mixt temperature rises above 50 DEG C simultaneously.Ultrasonic stripping, after 4 hours, is filtered the filter cake obtaining Graphene, is then washed away N-Methyl pyrrolidone with deionized water wash.In wet cake, add water, the Graphene slurry being made into concentration 2% is stand-by.
Oil fuel is sprayed in black reactor and mix at burning zone with the main preheated air supplying blower fan to provide, burn, produce the hot combustion gas stream of about 2000 DEG C; Stock oil is atomized and sprays into black reactor trunnion section after preheating, mixes with hot combustion gas stream, and cracking generates carbon black smoke; Then spray into a quenched water, reduce carbon black smoke temperature and make soot formation react stopping.Pyrocarbon black smoke gas flows through air preheater, produces the high-temperature hot air of 900 DEG C.Draw with blower fan the high-temperature hot air that air at room temperature enters 900 DEG C, the heated drying air being made into 250 DEG C is stand-by.
By the Graphene slurry of 2% concentration, pass in drying machine with centrifugal spray with the speed of 150 kilograms per hour.The disk utilizing horizontal direction to do high speed rotating in spray-drier gives centrifugal force to Graphene slurry, makes it throw away at a high speed, is dispersed into small drop.The heated drying air of 250 DEG C is introduced as dry-heat air in drying machine with centrifugal spray, warm air enters kiln in the shape of a spiral equably simultaneously.The small droplets of graphene-containing, greatly increases because atomization rear surface is long-pending, obtains powder with hot air short period of time inner drying.The specific surface area of the dry graphene powder of gained is 316m
2/ g, accompanying drawing illustrates the stereoscan photograph of the graphene powder that embodiment 1 obtains.Visible by this embodiment, high-temperature hot air is produced by utilizing the excess energy in carbon black production system, directly to the spraying dry heat supply of Graphene slurry, greatly reduce energy consumption and the cost of Graphene production process, be also conducive to the recycling economy of production of carbon black.
Embodiment 2
98% vitriol oil of 230L is added in reactor, and reactor leads to frozen water and is cooled to less than 4 DEG C.The 300 order 99% purity crystalline graphite powders and the 5 kilograms of SODIUMNITRATE that take 10 kilograms add reactor, and stir 1h and slowly add 30 kilograms of potassium permanganate later, control temperature is no more than 10 DEG C, and the reaction times is about 2h altogether; Then reactor heating, temperature controls, at 38 DEG C of reaction 0.5h, to keep stirring; In gained mixed solution, slowly add the deionized water of 800L, then reactor heating, keep mixeding liquid temperature 95 DEG C reaction 30min, period keeps appropriateness to stir; Add about 600L deionized water stopped reaction after pyroreaction, then continue the hydrogen peroxide adding 150L (30% concentration), question response adds the hydrochloric acid soln of 400L (10% concentration) again after being about 15min.Centrifuge washing removes excessive acid and by product.Be scattered in water by after washing in neutral graphite oxide, be made into 1% concentration, carry out circulating ultrasonic stripping with the ultrasonic wave liquid towards mixture of 50 every root power 2KW, logical water coolant guarantees that temperature rises above 50 DEG C simultaneously.Ultrasonic stripping is after 4 hours, and the graphene oxide slurry obtaining 1% concentration is stand-by.
Oil fuel is sprayed in black reactor and mix at burning zone with the main preheated air supplying blower fan to provide, burn, produce the hot combustion gas stream of about 2000 DEG C; Stock oil is atomized and sprays into black reactor trunnion section after preheating, mixes with hot combustion gas stream, and cracking generates carbon black smoke; Then spray into a quenched water, reduce carbon black smoke temperature and make soot formation react stopping, by bag filter, carbon black being collected.Carbon black tail gas, through pre-treatment, improves its calorific value, as fuel gas for graphene oxide Dryly use.The advanced spray column of carbon black tail gas, by water the H in tail gas
2o gas and a part of H
2s washs, and wash water is collected in the waste liquid pool of underground.With Ca (OH)
2to the H in wash water
2s carries out neutralizing treatment, and periodic cleaning neutralized reaction product CaSO
3, CaSO
4.Residue sewage, through precipitation and filtration treatment, is recycled and reused for spray tail gas.Tail gas after washing enters pressure-swing absorption apparatus and carries out drying, the water adsorption of the non-complete drying in tail gas is fallen, siccative activated alumina; Dried tail gas enters temperature swing absorption unit, by using activated carbon and carbonaceous molecular sieve the H in tail gas
2s, SO
2impurity removal, the H removed
2s and SO
2enter underground waste liquid pool and carry out neutralizing treatment; Tail gas after impurity removal is entered non-cryogenic pressure-swing absorption apparatus, and sorbent material adopts carbonaceous molecular sieve, and fractionation by adsorption goes out the nitrogen in tail gas, and purity can reach 99%, is stored in nitrogen storage tank, for various application.Through such process, the calorific value of carbon black tail gas brings up to 3000Kcal/Nm
3left and right.Passing in burner through pretreated carbon black tail gas, burning produces high-temperature hot flue gas, and in high-temperature hot flue gas, introduce air at room temperature further, the high-temperature hot flue gas obtaining 200 DEG C is stand-by.
By the graphene oxide slurry of 1% concentration, pass in drying machine with centrifugal spray with the speed of 150 kilograms per hour.The disk utilizing horizontal direction to do high speed rotating in spray-drier gives centrifugal force to graphene oxide slurry, makes it throw away at a high speed, is dispersed into small drop.The high-temperature hot flue gas of 200 DEG C is introduced as dry-heat air in drying machine with centrifugal spray, warm air enters kiln in the shape of a spiral equably simultaneously.Containing the small droplets of graphene oxide, greatly increase because atomization rear surface is long-pending, contact short period of time inner drying with heat smoke and obtain powder.The specific surface area of the dry graphene oxide powder of gained is 562m
2/ g.Visible by this embodiment, by utilizing the tail gas of production of carbon black through purifying treatment, then burning produces high-temperature hot flue gas, directly to the spraying dry heat supply of graphene oxide powder, greatly reduce energy consumption and the cost of graphene oxide production process, be also conducive to the recycling economy of production of carbon black.
Embodiment 3
Oil fuel is sprayed in black reactor and mix at burning zone with the main preheated air supplying blower fan to provide, burn, produce the hot combustion gas stream of about 2000 DEG C; Stock oil is atomized and sprays into black reactor trunnion section after preheating, mixes with hot combustion gas stream, and cracking generates carbon black smoke; Then spray into a quenched water, reduce carbon black smoke temperature and reaction is terminated, by being collected by carbon black after bag filter.Carbon black tail gas, through pre-treatment, improves its calorific value, as fuel gas for expanded graphite stove.The advanced spray column of carbon black tail gas, by water the H in tail gas
2o gas and a part of H
2s washs, and wash water is collected in the waste liquid pool of underground.With Ca (OH)
2to the H in wash water
2s carries out neutralizing treatment, and periodic cleaning neutralized reaction product CaSO
3, CaSO
4.Residue sewage, through precipitation and filtration treatment, is recycled and reused for spray tail gas.Tail gas after washing enters pressure-swing absorption apparatus and carries out drying, the water adsorption of the non-complete drying in tail gas is fallen, siccative activated alumina etc.; Dried tail gas enters temperature swing absorption unit, by using activated carbon and carbonaceous molecular sieve the H in tail gas
2s, SO
2impurity removal, the H removed
2s and SO
2enter underground waste liquid pool and carry out neutralizing treatment; Through such process, the calorific value of carbon black tail gas brings up to 1000Kcal/Nm
3left and right.Passing in burner through pretreated carbon black tail gas, the high-temperature hot flue gas of burning generation 1000 DEG C, the high-temperature hot flue gas obtained is stand-by.
Use fixed carbon content 98% granularity 80 object crystalline flake graphite to be raw material, the crystalline flake graphite of 100 kilograms to be placed in the mixing acid of 300 kilograms of vitriol oils (98% concentration) and 100 kilograms of nitric acid (65% concentration) dip treating 1 hour.Then, vacuum filtration isolates filtrate, is washed by the crystalline flake graphite of acidleach, dries, just obtain the compound between graphite layers of sour intercalation.The high-temperature hot flue gas of 1000 DEG C that carbon black tail gas burning produces, introduce graphite expansion stove, graphite expansion stove is heated to about 900 DEG C, and compound between graphite layers enters graphite expansion stove high-temperature heat expansion, and expansion multiplying power is 150 times, obtains expanded graphite.
Get 20 kilograms of expanded graphites, add the deionized water of 980 kilograms, be made into mixture.By the high-shear emulsion machine that power is 50 kilowatts, 4 hours are peeled off to mixture physics.High-shear emulsion machine utilizes high-shear rotor to carry out high-shear stripping to expanded graphite rapidly, and it utilizes the powerful kinetic energy that brings of machinery, makes expanded graphite in the narrow gap of rotor-stator, and per minute bears the aquashear of hundreds of thousands of time.The linear velocity of more than 15m/s is produced in the rotor outer end of high speed rotating, even high to 40m/s, and form strong machinery and aquashear, liquid layer friction, clash into and tear, expanded graphite is disperseed fully, emulsification, homogeneous, fragmentation, to be penetrated by stator slot simultaneously.Centrifugal extruding shock such as to tear at the comprehensive action, and through moving in circles of high frequency, finally obtain the nano graphite flakes slurry fully peeled off, solid content is 2%.Vacuum filtration is carried out to it, obtains the wet cake of solid content about 20%, stand-by.
The high-temperature hot flue gas blower fan of 1000 DEG C that carbon black tail gas burning produces is introduced air at room temperature, obtains the high-temperature hot flue gas of 400 DEG C, stand-by.The wet cake of nano graphite flakes solid content 20%, add internal diameter 360mm with 10-30 kilogram of speed hourly from feed end, the Rotary pipe type drying oven of length 4.8 meters is inner.The high-temperature hot flue gas of 400 DEG C is introduced Rotary pipe type drying oven system, as drying source outside the boiler tube rotated, drying is carried out to nano graphite flakes.Nano graphite flakes is obtained, gained nano graphite flakes thickness 5-20nm from discharge end.Visible by this embodiment, by utilizing the tail gas of production of carbon black through purifying treatment, then burning produces high-temperature hot flue gas, to the drying process heat supply of nano graphite flakes filter cake, greatly reduce energy consumption and the cost of nano graphite flakes production process, be also conducive to the recycling economy of production of carbon black.
Claims (3)
1. the Low-cost production method of a sheet carbon material powder, use liquid phase stripping technology, drying obtains sheet carbon material powder, wherein sheet carbon material is the one in nano graphite flakes, Graphene or graphene oxide, it is characterized in that: the heat that the heat of sheet carbon material powder drying process comes from carbon black process or produces in carbon black tail gas burning.
2. production method according to claim 1, is characterized in that: the heat of sheet carbon material powder drying process comes from the heat produced in the afterfire of carbon black tail gas water vapor removing.
3. production method according to claim 1, is characterized in that: the heat of sheet carbon material powder drying process comes from the high temperature air through air preheater generation in carbon black process.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080279756A1 (en) * | 2007-05-08 | 2008-11-13 | Aruna Zhamu | Method of producing exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| CN102618095A (en) * | 2012-03-07 | 2012-08-01 | 无锡双诚炭黑有限公司 | Production method of environmentally-friendly carbon black |
| CN103466605A (en) * | 2013-08-22 | 2013-12-25 | 广东工业大学 | Preparation method of nano graphite sheet |
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
-
2016
- 2016-01-11 CN CN201610018123.7A patent/CN105480970A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080279756A1 (en) * | 2007-05-08 | 2008-11-13 | Aruna Zhamu | Method of producing exfoliated graphite, flexible graphite, and nano-scaled graphene platelets |
| CN102618095A (en) * | 2012-03-07 | 2012-08-01 | 无锡双诚炭黑有限公司 | Production method of environmentally-friendly carbon black |
| CN103466605A (en) * | 2013-08-22 | 2013-12-25 | 广东工业大学 | Preparation method of nano graphite sheet |
| CN103723708A (en) * | 2013-11-22 | 2014-04-16 | 盐城纳新天地新材料科技有限公司 | Preparation method of organic single-layer graphene solution |
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