CN109887760A - A kind of active carbon of high conductivity and its preparation and purposes - Google Patents
A kind of active carbon of high conductivity and its preparation and purposes Download PDFInfo
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
A kind of active carbon of high conductivity and its preparation and purposes, the diameter of the active carbon of the high conductivity is 0.1~30 μm, draw ratio is 1:1~200000:1, average length (corresponding English is in-plane length) is 10-30nm in its carbon-coating crystal face, and specific surface area is 1000~2300m2/g；Preparation method is that template is passed through H after being heated to 500-1200 DEG C in carrier gas and being kept for a period of time including the use of polymer preoxided thread2O or CO2Pore-creating and the shaping of carbon-coating arrangement architecture are carried out, the active carbon of diameter and the constant or reduced high conductivity of draw ratio is made.The preparation method is simple, and products obtained therefrom purity is high, tap density is big, and structural integrity, mechanical strength is strong, is applicable to separate, the electrode material of adsorbent material or electrochemical energy storage.When electrode material for 4V supercapacitor, in the case where 10A/g sweeps speed, specific capacitance is 100-250F/g.
Description
Technical field
The invention belongs to carbon material and its preparation technical field, in particular to the active carbon of a kind of high conductivity and its preparation
With purposes.
Background technique
Double layer capacitor is a kind of based on electrolyte/electrode interface physics energy storage device, has charge and discharge fast, does not put
Heat, power density is big, the long feature of safe life, is widely used in the starting of various heavy equipments, the excitation of high-power system,
And the energy adsorption field of fast energy storage and transfer, and the backup power source etc. of reliability is kept when needing long period standby.
This kind of capacitor often uses the active carbon of large specific surface area, and carbon nanotube and graphene etc. do electrode material, take into account as far as possible electric conductivity,
Chemical stability is suitable for a variety of requirements such as pore structure and processing characteristics.In transmission characteristic, the electronics for both needing to meet long-range is led
Electricity requires, and the ion diffusion for needing to meet short distance requires.The materials such as carbon nanotube and graphene very well satisfy this and want
It asks, but its tap density is too low, liquid absorption amount is excessive, causes the energy density based on device not high.In terms of processing characteristics, activity
For charcoal since particle is big, tap density is big, and absorption liquid measure is small and is widely adopted, but its micropore is too many, and electric conductivity is too poor, restricts
Performance performance.
The fundamental characteristics of above-mentioned material, the performance for resulting in active carbon base double layer capacitor are difficult to improve again.Simultaneously
It results in carbon nanotube and graphene-based double layer capacitor industrialization pace is slow.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of active carbon of high conductivity and
It is prepared and purposes, the electric conductivity of the active carbon are parity with or superiority over carbon nanotube or graphene, is much better than conventional carbon, chemistry
Structural stability is much better than conventional carbon, liquid absorption amount, tap density again therebetween, thus have be currently known it is best
Integrated capacitor part performance.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of active carbon of high conductivity, basic configuration are sheet, graininess, bulk or long Filamentous, wherein it is long it is Filamentous with
Graininess is most important to capacitance applications.Diameter is 0.1~30 μm, and draw ratio is 1:1~200000:1；It is average in its carbon-coating crystal face
Length (corresponding English is in-planelength) is 10-30nm, and the hole of 0.7-5nm accounts for the 65-90% of total pore volume, specific surface area
For 1000~2300m2/g；Conductivity is in 40-350S/cm, tap density 150-750kg/m3。
The present invention also provides a kind of methods of active carbon for preparing the high conductivity, include the following steps:
Step 1: polymer preoxided thread being placed in reactor, 500-1200 DEG C is warming up in carrier gas, keeps 1-24
Hour；
Step 2: and then switching gas, it is passed through H2O and/or CO2Gas carries out pore-creating and the shaping of carbon-coating arrangement architecture, wherein
The air speed of gas is 0.1-300L/kg preoxided thread/h, after handling 0.1-24 hours at 500-1200 DEG C, closes H2O and/or
CO2Gas is down to room temperature under inert gas protection, takes out products therefrom, obtains diameter and the constant or reduced height of draw ratio
The active carbon of electric conductivity.
Preferably, the outer diameter of the polymer preoxided thread is 0.5-30 μm, and draw ratio is 1:1~200000:1.
Polymer preoxided thread is the property according to polymer, using high-temperature control gaseous oxidation or low-temperature oxidation
Acid (such as sulfuric acid) or the method for other solution (such as potassium permanganate, potassium bichromate etc.) liquid phase oxidations obtain.By pre-oxidation, go
Fall most of protium in polymer, retains most of carbon, and form certain hole.
Preferably, the polymer can be polyacrylonitrile, polystyrene, polyurethane, polycarbonate, aramid fiber, polyethers, gather
Vinyl alcohol, polyolefin, phenolic resin, epoxy resin, polythiophene, polyformaldehyde, polyaniline, polypyridine, polypyrrole, polyacetylene gather
One of ethylene oxide is a variety of, and characteristic is in H2O, CO2When activating in medium, any polymerization of carbon skeleton can be left
Object.
Preferably, the carrier gas is one of nitrogen, argon gas, hydrogen, CO or a variety of.
Preferably, the inert gas is nitrogen and/or argon gas.
The active carbon of high conductivity of the present invention can be used as the electrode material of supercapacitor, when the super electricity for 4V
When the electrode material of container, in the case where 10A/g sweeps speed, specific capacitance is 100-250F/g.
Compared with prior art, the beneficial effects of the present invention are:
1) method that the present invention uses is simple, can prepare the biggish conduction active-carbon of draw ratio range and its fiber.Together
When aperture and specific surface area it is adjustable.When as capacitance electrode material, than the high power lower longevity of presently commercially available active carbon based capacitor
Life improves 1-2 times.Or the storage cost of unit time reduces 20-50%.
2) products obtained therefrom can be particle, can also be the one-dimensional linear fibre structure of macroscopic view, facilitate processing.With reported at present
Carbon nano-tube fibre, graphene fiber compares, the capacitor element of composition, and mass energy density improves 50-200%.
3) when being used as the adsorbent material of gas or liquid, under same adsorption efficiency, than current activated carbon product, pressure drop is low
5-10%.Than the product of current carbon nanomaterial, handles intensity and improve 50-300%.
As it can be seen that preparation method of the present invention is simple, products obtained therefrom purity is high, tap density is big, structural integrity, mechanical strength
By force, it is applicable to separate, the electrode material of adsorbent material or electrochemical energy storage.
Specific embodiment
Below with reference to the embodiment embodiment that the present invention will be described in detail.
Embodiment 1
Preoxidized polyacrylonitrile silk (outer diameter is 0.5 μm, draw ratio 200000:1) is placed in reactor, in argon gas
1200 DEG C are warming up to, is kept for 1 hour.Then switch gas, be passed through H2O, the air speed of gas are 0.1L/kg preoxided thread/h,
After handling 4 hours at 1000 DEG C, H is closed2O.It is down to room temperature under protection of argon gas.Product outer diameter is 0.1 μm, and draw ratio is
200000:1, specific surface area 2300m2The hole of/g, 0.7-5nm account for the 90% of total pore volume.Average length is (right in its carbon-coating crystal face
Answering English is in-plane length) it is 30nm.Conductivity is in 350S/cm.Tap density is 350kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 250F/g.
Embodiment 2
By preoxidized polyacrylonitrile silk, polypropylene preoxided thread and polyethylene preoxided thread (mass fraction 50%,
40%, 10%, outer diameter is 10 μm, draw ratio 1:1) it is placed in reactor, 900 DEG C are warming up in hydrogen, holding 6 is small
When.Then switch gas, be passed through CO2, the air speed of gas is 300L/kg preoxided thread/h, after synthermal lower processing 4 hours,
Close CO2, it is down to room temperature under nitrogen protection.Product is that outer diameter is 5 μm, draw ratio 1:1, specific surface area 1600m2/ g,
The hole of 0.7-5nm accounts for the 70% of total pore volume.Average length (corresponding English is in-plane length) is in its carbon-coating crystal face
10nm.Conductivity is in 40S/cm.Tap density is 700kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 150F/g.
Embodiment 3
Polyvinyl alcohol preoxided thread (outer diameter is 0.3 μm, draw ratio 100:1) is placed in reactor, is risen in nitrogen
Temperature is kept for 1 hour to 500 DEG C；Then switch gas, be passed through 10%H2O and 90%CO2, the air speed of gas is the pre- oxygen of 100L/kg
Change silk/h, after synthermal lower processing 24 hours, closes H2O and CO2, it is down to room temperature under nitrogen protection.Product outer diameter is 0.1 μ
M, draw ratio 100:1, specific surface area 1000m2/g.The hole of 0.7-5nm accounts for 65% in total pore volume.It is put down in its carbon-coating crystal face
Equal length (corresponding English is in-plane length) is 15nm.Conductivity is in 140S/cm.Tap density is 750kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 100F/g.
Embodiment 4
By polystyrene preoxided thread, polyethers preoxided thread, polyvinyl alcohol preoxided thread (mass fraction is respectively 20%,
30%, 50%, outer diameter is 5 μm, draw ratio 10000:1) it is placed in reactor, in carrier gas (50% hydrogen, 30% and 20% argon
Gas) in be warming up to 950 DEG C, kept for 24 hours；Then switch gas, be passed through CO2, the air speed of gas be 50L/kg preoxided thread/
H closes H after synthermal lower processing 2 hours2O and CO2Gas drops to room temperature in 40% argon gas and 60% nitrogen protection.It produces
Product outer diameter is 3 μm, draw ratio 10000:1, specific surface area 1800m2/g.The hole of 0.7-5nm accounts for 87% in total pore volume.Its
Average length (corresponding English is in-plane length) is 20nm in carbon-coating crystal face.Conductivity is in 150S/cm.Tap density
For 500kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 195F/g.
Embodiment 5
Aramid fiber preoxided thread (outer diameter is 30 μm, draw ratio 4000:1) is placed in reactor, is warming up in hydrogen
It 1200 DEG C, is kept for 2 hours；Then switch gas, be passed through H2The air speed of O, gas are 2L/kg preoxided thread/h, under synthermal
After processing 0.1 hour, H is closed2O is down to room temperature under nitrogen protection.Product outer diameter is 30 μm, and draw ratio 4000:1 compares table
Area is 1200m2/g.The hole of 0.7-5nm accounts for 90% in total pore volume.(corresponding English is in- to average length in its carbon-coating crystal face
Plane length) it is 14nm.Conductivity is in 80S/cm.Tap density is 720kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 200F/g.
Embodiment 6
By polycarbonate preoxided thread and polyurethane preoxided thread, (mass fraction is respectively 70%, 30%, and outer diameter is 15 μ
M, draw ratio 350:1) it is placed in reactor, 500 DEG C are warming up in carrier gas (5% hydrogen and 95% argon gas), holding 5 is small
When；Then switch gas, be passed through 90%H2O and 10%CO2, the air speed of gas is 220L/kg preoxided thread/h, under synthermal
After processing 24 hours, H is closed2O and CO2, it is down to room temperature under protection of argon gas.Product outer diameter is 10 μm, draw ratio 320:1, than
Surface area is 1400m2/g.The hole of 0.7-5nm accounts for 72% in total pore volume.(correspond to English is average length in its carbon-coating crystal face
In-plane length) it is 25nm.Conductivity is in 150S/cm.Tap density is 600kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 130F/g.
Embodiment 7
By polyethers preoxided thread and polyethylene oxide preoxided thread (mass fraction is respectively 60%, 40%, and outer diameter is 5 μm,
Draw ratio is 50000:1) it is placed in reactor, 700 DEG C are warming up in carrier gas (50%CO and 50% hydrogen), holding 15 is small
When；Then switch gas, be passed through 1%H2O and 99%CO2, the air speed of gas is 10L/kg preoxided thread/h, at synthermal lower place
Reason closed H after 20 hours2O and CO2, it is down to room temperature under nitrogen protection.Product outer diameter is 2.5 μm, draw ratio 50000:1,
Specific surface area is 1800m2/g.The hole of 0.7-5nm accounts for 85% in total pore volume.Average length (corresponding English in its carbon-coating crystal face
It is 18nm for in-plane length).Conductivity is in 90S/cm.Tap density is 480kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 250F/g.
Embodiment 8
By polyurethane preoxided thread and polyformaldehyde preoxided thread, (mass fraction is respectively 20%, 80%, and outer diameter is 3 μm, long
Diameter ratio is 5000:1) it is placed in reactor, it is warming up to 800 DEG C in carrier gas (25% hydrogen and 75% nitrogen), is kept for 8 hours；
Then switch gas, be passed through CO2, the air speed of gas is 30L/kg preoxided thread/h, after synthermal lower processing 24 hours, is closed
CO2, it is down to room temperature under nitrogen protection.Product outer diameter is 1 μm, draw ratio 3000:1, specific surface area 2200m2/g。0.7-
The hole of 5nm accounts for 85% in total pore volume.Average length (corresponding English is in-plane length) is in its carbon-coating crystal face
21nm.Conductivity is in 190S/cm.Tap density is 580kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 250F/g.
Embodiment 9
By polypyridine preoxided thread, polypyrrole preoxided thread, polythiophene preoxided thread (mass fraction is respectively 20%,
20%, 60%, outer diameter is 12 μm, draw ratio 25000:1) it is placed in reactor, in carrier gas (40%H2And 10%CO, 50%
Nitrogen) in be warming up to 1100 DEG C, kept for 0.1 hour；Then switch gas, be passed through CO2, the air speed of gas is the pre- oxygen of 100L/kg
Change silk/h, after synthermal lower processing 6 hours, closes CO2, it is down to room temperature under nitrogen protection.Product outer diameter is 12 μm, major diameter
Than for 1200:1, specific surface area 2200m2/g.The hole of 0.7-5nm accounts for 90% in total pore volume.It is averagely long in its carbon-coating crystal face
Degree (corresponding English is in-plane length) is 28nm.Conductivity is in 240S/cm.Tap density is 150kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 240F/g.
Embodiment 10
Epoxy resin is pre-oxidized into silk, polyethylene oxide preoxided thread, polyacetylene preoxided thread and polyolefin preoxided thread
(mass fraction is respectively 20%, 20%, 50%, 10%, and outer diameter is 2 μm, draw ratio 10:1) is placed in reactor, in hydrogen
In be warming up to 650 DEG C；Then switch gas, be passed through 70%H2O and 30%CO2, the air speed of gas is 140L/kg preoxided thread/h,
After synthermal lower processing 18 hours, H is closed2O and CO2, it is down to room temperature under nitrogen protection.Product outer diameter is 1 μm, draw ratio
For 1:1, specific surface area 1100m2/g.The hole of 0.7-5nm accounts for 70% in total pore volume.Average length is (right in its carbon-coating crystal face
Answering English is in-plane length) it is 15nm.Conductivity is in 100S/cm.Tap density is 500kg/m3。
4V supercapacitor (with EMIBF4For electrolyte) in, 10A/g sweep speed under, the specific capacitance of electrode material
For 120F/g.
Claims (10)
1. a kind of active carbon of high conductivity, average length is 10-30nm in carbon-coating crystal face, and the hole of 0.7-5nm accounts for total pore volume
65-90%, specific surface area be 1000~2300m2/g；Conductivity is in 40-350S/cm, tap density 150-750kg/m3。
2. preparing high conductivity active carbon according to claim 1, which is characterized in that its shape is sheet, graininess, bulk
Or it is long Filamentous.
3. preparation high conductivity active carbon according to claim 1 or claim 2, which is characterized in that a diameter of 0.1~30 μm, long
Diameter ratio is 1:1~200000:1.
4. a kind of method for the active carbon for preparing high conductivity described in claim 1, which comprises the steps of:
Step 1: polymer preoxided thread being placed in reactor, 500-1200 DEG C is warming up in carrier gas, is kept for 1-24 hours；
Step 2: and then switching gas, it is passed through H2O and/or CO2Gas, the air speed of gas are 0.1-300L/kg preoxided thread/h,
After handling 0.1-24 hours at 500-1200 DEG C, H is closed2O and/or CO2Gas is down to room temperature under inert gas protection,
Take out products therefrom.
5. preparing the method for high conductivity active carbon according to claim 4, which is characterized in that the polymer preoxided thread
Outer diameter be 0.5-30 μm, draw ratio be 1:1~200000:1.
6. the method for preparation high conductivity active carbon according to claim 4 or 5, which is characterized in that the pre- oxygen of polymer
Change silk, is the property according to polymer, using high-temperature control gaseous oxidation or the acid or other solution liquid phases of low-temperature oxidation
The method of oxidation obtains, and by pre-oxidation, removes most of protium in polymer, retains most of carbon, and formed
Certain hole.
7. the method for preparation high conductivity active carbon according to claim 4 or 5, which is characterized in that the polymer is poly-
Acrylonitrile, polystyrene, polyurethane, polycarbonate, aramid fiber, polyethers, polyvinyl alcohol, polyolefin, phenolic resin, epoxy resin,
Polythiophene, polyformaldehyde, polyaniline, polypyridine, polypyrrole, polyacetylene, one of polyethylene oxide or a variety of.
8. preparing the method for high conductivity active carbon according to claim 4, which is characterized in that the carrier gas is nitrogen, argon
One of gas, hydrogen, CO or a variety of；The inert gas is nitrogen and/or argon gas.
9. the purposes that the active carbon of high conductivity described in claim 1 is used as the electrode material of supercapacitor.
10. purposes according to claim 9, which is characterized in that the electrode material of the supercapacitor for 4V, in 10A/g
Sweeping specific capacitance under speed is 100-250F/g.
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