CN108557799A - A kind of high-purity high conductivity class graphene grading-hole porous charcoal and preparation method thereof - Google Patents
A kind of high-purity high conductivity class graphene grading-hole porous charcoal and preparation method thereof Download PDFInfo
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- CN108557799A CN108557799A CN201810564634.8A CN201810564634A CN108557799A CN 108557799 A CN108557799 A CN 108557799A CN 201810564634 A CN201810564634 A CN 201810564634A CN 108557799 A CN108557799 A CN 108557799A
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- grading
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
Abstract
The invention discloses a kind of high-purity high conductivity class graphene grading-hole porous charcoals and preparation method thereof, using the high substance of phosphorus content as precursor, under atmosphere, are obtained through direct pore-creating, catalyzed graphitization and/or post-processing.The preparation method of the present invention is laser heating, and step linking is close, avoids in conventional method the thermal loss caused by step linking difference, is easy to serialization, large-scale production.Gained Carbon Materials not only possess the characteristics such as high-specific surface area, aperture controllable, and the class graphene-structured of charcoal skeleton for the benefit of electronics conduction, can take into account the double grading of high mass transfer and high conduction, possess good hot vibration resistance, the advantages such as stronger mechanical strength.It can be applied to the fields such as high efficiency and heat radiation, electrode material and conductive agent, catalyst carrier.
Description
Technical field
The present invention relates to a kind of high-purity high conductivity class graphene grading-hole porous charcoals and preparation method thereof, belong to new material
Field.
Background technology
Porous charcoal large specific surface area, the characteristics such as pore structure and interfacial property are controllable, chemical stability is good, and its electric conductivity
Transformation of the semiconductor to superconductor may be implemented, be applied to new energy, environmental protection, gas separation with storage, pharmaceutical carrier,
The fields such as catalyst carrier.But the high voidage of porous charcoal and high electronic conductivity are difficult to be unified on porous carbon material of the same race.
Such as porosity, high commercial absorbent charcoal material conductivity is about 4us/m, the conductivity of all kinds of porous carbon materials reported in the literature
Substantially all<100us/m;And Carbon Materials graphene (1u Ω m), carbon nanotube and the graphite electrode (5.5-9u of high conductivity
Ω m), Carbon fibe (16-900u Ω m), prebaked anode (55-60u Ω m), soberberg anode (70-80u Ω m), and it is few
The after-smithing petroleum coke (500u Ω m or so) in hole, contains only a small amount of defective hole substantially.In special dimension, easily grain is such as needed
Sub-transmission path, and facilitate the field of electronics quickly transmitted, such Carbon Materials will be unable to be competent at.
Carbon Materials will realize high porosity, and more charcoals is needed to be etched pore-forming, and charcoal skeleton is weakened at this time.And Carbon Materials
With the raising of porosity, electron conduction will reduce, and porous class Carbon Materials structure is essentially unformed, this structure is also unfavorable
In transmission of the electronics on charcoal skeleton.The general porosity of Carbon Materials of high conductivity is extremely low, and the electronics caused by vacancy passes at this time
Path elongation is passed to be weakened.And the Carbon Materials of more high conductivity are essentially graphite-structure or graphite-like structure, regular structure is just
In the transmission of electronics, and two-dimensional laminated structure can build delocalized pi-bond, improve the delivery rate of electronics.But the shape of this structure
At needs graphitization or graphite alkylene.
Porous charcoal is graphitized, the degree of graphitization of skeleton is increased, is a kind of method effectively improving conductivity.But it is conventional
Way be:Porous charcoal is first prepared, carries out graphitization processing afterwards, two processes are artificially partitioned, technological process is increased, is caused
The complexity of energy consumption great increase and operation.《It is a kind of using activated carbon as the preparation side of Material synthesis graphitized stephanoporate material with carbon element
Method》In (CN 103318871A), using activated carbon as raw material, the dispersion of porous charcoal, the network of catalyst are realized under liquid environment
It closes, though realize the graphitization under lower temperature, it is complicated for operation in solution system, it is difficult to which that large-scale production, there is also catalyst
It is difficult to remove the problems such as clean.《A method of electrical conductance is improved based on purifying petroleum coke based super capacitor activated carbon》
(106744945 A of CN), using petroleum coke as raw material, chemical activation method prepares porous charcoal, after further increase temperature, will be high
The metal impurities gasification heel row of boiling point is removed, and by " carbide generation-decomposition or dissolving-are precipitated again " mechanism, obtains high-purity height
The porous charcoal of conductance.But the method needs 2000 DEG C or more of high temperature, and high energy consumption, equipment requirement is high, the discontinuum of reaction process,
Cause the waste of energy consumption.
Invention content
The high porosity and high electronic conduction shown in crossing domain application the purpose of the present invention is reply Carbon Materials
Property difficulty compatibility problem, a kind of double grading for being produced on a large scale, taking into account high mass transfer and high conduction is provided, possesses good heat
Shock resistance, high-purity high conductivity class graphene grading-hole porous charcoal of the advantages such as stronger mechanical strength and preparation method thereof.It borrows
To expand the application field of novel charcoal material and meet requirement of the special dimension to Carbon Materials.
The technical scheme is that:
A kind of high-purity high conductivity class graphene grading-hole porous charcoal, using the substance of high carbon content as precursor, through direct
After pore-creating, catalyzed graphitization and/or post-processing, porous charcoal is obtained.
A kind of preparation method of high-purity high conductivity class graphene grading-hole porous charcoal, with the substance of high carbon content for preceding body
Pore creating material and catalyst is added in body, and after direct pore-creating, catalyzed graphitization and/or post-processing, cleaning to neutrality is dry, obtains
Porous charcoal.
The substance of high carbon content is in petroleum coke, pitch coke, coal tar, polyvinyl chloride-based charcoal, mesocarbon microspheres, Carbon fibe
One or more.
The molar ratio of pore creating material and presoma is (0.01-15):1;Pore creating material be sodium hydroxide, potassium hydroxide, potassium oxide,
Sodium oxide molybdena, zinc oxide, sylvite, sodium salt, zinc salt, H2O、CO2One or more of.
The condition of direct pore-creating is:Under A atmosphere, it is warming up to 300-950 DEG C, keeps the temperature 0.01-10h, heating rate is
0.1-50℃/min;A atmosphere is one or more of argon gas, nitrogen, helium, vacuum.
The molar ratio of catalyst and precursor is (0.01-10):1;Catalyst is iron chloride, iron oxide, ferric nitrate, chlorination
One or more of nickel, nickel oxide, nickel nitrate, nickelous carbonate, cobalt chloride, cobalt oxide, cobalt nitrate, cobalt carbonate.
The condition of catalyzed graphitization is:Under B atmosphere, it is warming up to 950-1800 DEG C, keeps the temperature 0-12h, heating rate is
0.1-50℃/min;B atmosphere is one or more of argon gas, nitrogen, helium, chlorine, gaseous silicon.
Post-processing is one or both of atmosphere heating, solution reaction.
Atmosphere heating method be:Under C atmosphere, 950-1800 DEG C of heat preservation 1-3h;C atmosphere be argon gas, nitrogen, helium,
One or more of chlorine, gaseous silicon.
The method of solution reaction is:Pickling or alkali cleaning or soda acid replace one kind in embathing.
Beneficial effects of the present invention:
The method of the present invention is realized pore-creating and graphitization, is shortened using high carbon content material as precursor in same reactor
Technological process, while the use of catalyst can reduce graphitization temperature, construct and remove mechanism conducive to impurity.The preparation of the present invention
Method is laser heating, and step linking is close, avoids in conventional method the thermal loss caused by step linking difference, is easy to continuous
Change, large-scale production.The method of the present invention can effectively improve the porosity, electric conductivity and purity of Carbon Materials, be it is a kind of it is simple,
The efficient porous charcoal preparation method for taking into account high porosity and high conductivity.
Specific implementation mode
The specific implementation mode of the present invention is described in further detail with reference to embodiments.It should be understood that this
The described specific implementation mode in place is merely to illustrate and explain the present invention, and is not intended to restrict the invention.Additionally need explanation
, specific technical features described in the above specific embodiments in the case of no contradiction can be by appointing
What suitable mode is combined, in order to avoid unnecessary repetition, the present invention to various combinations of possible ways no longer separately
Explanation.Following embodiment is intended to illustrate invention, rather than limitation of the invention further, the present invention can be by inventions
Hold the either type to implement.
Embodiment 1
By petroleum coke, potassium hydroxide, ferric nitrate in molar ratio 1:3:0.05 mixing, is put into nickel crucible, is subsequently placed in height
In warm atmosphere furnace, it is passed through the nitrogen of 200ccm, and 850 DEG C of heat preservation 1h are warming up to 2 DEG C/min, increases the chlorine of 30ccm afterwards, with
5 DEG C/min is warming up to 1350 DEG C, and keeps the temperature 4h, and stopping is passed through chlorine (continuing to be passed through nitrogen), and is down to room temperature naturally, by gained
1h in the HCl solution of product immersion 0.05M, rear take out simultaneously are cleaned to neutrality with deionized water, dry 8h in 80 DEG C of baking ovens, obtain ash
Point content is 0.06%, conductivity 10S/cm, specific surface area 1370m2The class graphene grading-hole porous charcoal of/g.
Embodiment 2
By pitch coke, sodium oxide molybdena, nickel chloride in molar ratio 1:3:0.02 mixing, is put into nickel crucible, is subsequently placed in high temperature
In atmosphere furnace, it is passed through the nitrogen of 600ccm, and 750 DEG C of heat preservation 2h, the rear chlorine for increasing 60ccm, with 5 are warming up to 2 DEG C/min
DEG C/min is warming up to 1550 DEG C, and keeps the temperature 2h, stopping is passed through chlorine (continuing to be passed through nitrogen), and is down to room temperature naturally, by gained
0.5h in the HCl solution of product immersion 0.1M, rear take out simultaneously are cleaned with deionized water to neutrality, 4h in 100 DEG C of vacuum drying chambers,
Obtain that content of ashes is 0.09%, Franklin's P values are 0.404, specific surface area 1150m2The class graphene grading-hole of/g is more
Hole charcoal.
Embodiment 3
By coal tar, nickel chloride in molar ratio 1:0.02 mixing, is put into nickel crucible, is subsequently placed in high-temperature atmosphere furnace, leads to
Enter the nitrogen of 600ccm and the CO of 45ccm2, and 700 DEG C of heat preservation 5h are warming up to 10 DEG C/min, rear stopping is passed through CO2, increase
The chlorine of 20ccm is warming up to 1650 DEG C with 10 DEG C/min, and keeps the temperature 2h, and stopping is passed through chlorine (continuing to be passed through nitrogen), and natural
It is down to room temperature, products therefrom is immersed to the HNO of 0.5M30.5h in solution, it is rear to take out and cleaned to neutrality with deionized water, 100
2h in DEG C vacuum drying chamber, obtains that content of ashes is 0.045%, Franklin's P values are 0.37, specific surface area 850m2/ g's
Class graphene grading-hole porous charcoal.
Embodiment 4
By petroleum coke, zinc chloride, ferric nitrate in molar ratio 1:5:0.01 mixing, is put into nickel crucible, is subsequently placed in high temperature
In atmosphere furnace, it is passed through the nitrogen of 60ccm, and 950 DEG C of heat preservation 0.5h, the rear chlorine for increasing 30ccm, with 5 are warming up to 2 DEG C/min
DEG C/min is warming up to 1800 DEG C, and keeps the temperature 4h, stopping is passed through chlorine (continuing to be passed through nitrogen), and is down to room temperature naturally, by gained
Product immerses the HNO of 1..5M31h in solution, rear to take out and cleaned to neutrality with deionized water, 8h in 80 DEG C of baking ovens obtains ash
Point content is 0.06%, conductivity 15S/cm, specific surface area 850m2The class graphene grading-hole porous charcoal of/g.
Embodiment 5
By mesocarbon microspheres, potassium carbonate, ferric nitrate in molar ratio 1:3:0.07 mixing, is put into nickel crucible, then sets
In high-temperature atmosphere furnace, it is passed through the nitrogen of 100ccm, and 750 DEG C of heat preservation 2h are warming up to 10 DEG C/min, is warming up to 5 DEG C/min
It is 1800 DEG C, rear to increase the gaseous silicon for being passed through 50ccm, and 2h is kept the temperature, the rear chlorine for increasing 30ccm continues to keep the temperature 1h, after
Stopping is passed through chlorine and gaseous silicon (continuing to be passed through nitrogen), and is down to room temperature naturally, and products therefrom is immersed 0.5M's
4h in HCl solution, it is rear to take out and cleaned to neutrality with deionized water, 8h in 80 DEG C of baking ovens, content of ashes is obtained as 0.07%, electricity
Conductance is 20S/cm, specific surface area 950m2The class graphene grading-hole porous charcoal of/g.
Embodiment 6
By polyvinyl chloride-based charcoal, potassium hydroxide, cobalt nitrate in molar ratio 1:7:0.03 mixing, is put into nickel crucible, then
It is placed in high-temperature atmosphere furnace, is passed through the nitrogen of 150ccm, and 850 DEG C of heat preservation 1.5h are warming up to 20 DEG C/min, increases 30ccm afterwards
Chlorine, be warming up to 1550 DEG C with 5 DEG C/min, and keep the temperature 6h, stopping is passed through chlorine (continuing to be passed through nitrogen), and is down to room naturally
Products therefrom is immersed 1h in the HCl solution of 0.05M by temperature, rear to take out and cleaned to neutrality with deionized water, in 110 DEG C of baking ovens
8h, obtain content of ashes be 0.045%, conductivity 7.6S/cm, specific surface area 1870m2The class graphene grading-hole of/g is more
Hole charcoal.
Claims (10)
1. a kind of high-purity high conductivity class graphene grading-hole porous charcoal, which is characterized in that with the substance of high carbon content for preceding body
Body obtains porous charcoal after direct pore-creating, catalyzed graphitization and/or post-processing.
2. a kind of preparation method of high-purity high conductivity class graphene grading-hole porous charcoal as described in claim 1, feature
Be, using the substance of high carbon content as precursor, pore creating material and catalyst be added, through direct pore-creating, catalyzed graphitization and/or after
After processing, cleaning to neutrality is dry, obtains porous charcoal.
3. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 2, feature exist
In the substance of high carbon content is one in petroleum coke, pitch coke, coal tar, polyvinyl chloride-based charcoal, mesocarbon microspheres, Carbon fibe
Kind is several.
4. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 2, feature exist
In the molar ratio of pore creating material and presoma is (0.01-15):1;Pore creating material is sodium hydroxide, potassium hydroxide, potassium oxide, oxidation
Sodium, zinc oxide, sylvite, sodium salt, zinc salt, H2O、CO2One or more of.
5. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 2, feature exist
In the condition of direct pore-creating is:Under A atmosphere, it is warming up to 300-950 DEG C, keeps the temperature 0.01-10h, heating rate 0.1-50
℃/min;A atmosphere is one or more of argon gas, nitrogen, helium, vacuum.
6. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 2, feature exist
In the molar ratio of catalyst and precursor is (0.01-10):1;Catalyst is iron chloride, iron oxide, ferric nitrate, nickel chloride, oxygen
Change one or more of nickel, nickel nitrate, nickelous carbonate, cobalt chloride, cobalt oxide, cobalt nitrate, cobalt carbonate.
7. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 2, feature exist
In the condition of catalyzed graphitization is:Under B atmosphere, it is warming up to 950-1800 DEG C, keeps the temperature 0-12h, heating rate 0.1-50
℃/min;B atmosphere is one or more of argon gas, nitrogen, helium, chlorine, gaseous silicon.
8. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 2, feature exist
In post-processing as atmosphere heating, one or both of solution reaction.
9. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 8, feature exist
In the method for atmosphere heating is:Under C atmosphere, 950-1800 DEG C of heat preservation 1-3h;C atmosphere be argon gas, nitrogen, helium, chlorine,
One or more of gaseous silicon.
10. the preparation method of high-purity high conductivity class graphene grading-hole porous charcoal according to claim 8, feature exist
In the method for solution reaction is:Pickling or alkali cleaning or soda acid replace one kind in embathing.
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CN109321211A (en) * | 2018-10-19 | 2019-02-12 | 福州大学 | A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof |
CN109850888A (en) * | 2019-01-31 | 2019-06-07 | 西安科技大学 | A kind of method of semicoke sub-prime coproduction porous activated carbon and class graphene aerogel |
CN110436459A (en) * | 2019-09-19 | 2019-11-12 | 盐城工学院 | A kind of preparation method being graphitized graded porous carbon |
CN112551514A (en) * | 2020-12-10 | 2021-03-26 | 珠海复旦创新研究院 | Preparation method of graphene |
CN113871590A (en) * | 2021-09-16 | 2021-12-31 | 广东凯金新能源科技股份有限公司 | Layered porous graphite negative electrode material and preparation method thereof |
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