CN105197925B - A kind of preparation method and applications of nitrogen-dopped activated carbon - Google Patents
A kind of preparation method and applications of nitrogen-dopped activated carbon Download PDFInfo
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Abstract
A kind of preparation method and applications of nitrogen-dopped activated carbon, the present invention relates to a kind of preparation method and applications of nitrogen-dopped activated carbon, the invention aims to solve the waste degradation complex process of nitrogenous based thermoset polymer, the problem of cost is higher, method is：Prepare aminal dynamic covalent networks structural polymer spawn；Aminal dynamic covalent networks structural polymer product is prepared, high temperature pyrolysis is then carried out, produces nitrogen-dopped activated carbon；Nitrogen-dopped activated carbon of the present invention is applied to ultracapacitor.The Preparation equipment of the present invention is simple, environmental protection and energy saving, and insoluble insoluble thermosetting polymer carries out proper treatment by made from, can reuse, and simple to operate, is easy to mass produce；The activated carbon obtained can be used as electrode material for super capacitor.The invention belongs to technical field of nano material.
Description
Technical field
The present invention relates to a kind of preparation method and applications of nitrogen-dopped activated carbon.
Background technology
Nitrogenous based thermoset polymer, such as polyamide, polybenzimidazoles, polyimides etc., it has good heat engine
Tool performance, resist chemical performance, electrical property etc., which may be advantageously employed in, prepares foam, adhesive, automobile, aviation, and electronics is set
It is standby etc..It is well known that thermosetting polymer has the performance of " insoluble not melt ".So be difficult transformation once preparing shaping,
It is difficult processing with product later, general degradation technique requires higher, and cost is higher, and its degraded will be for a long time.
Traditional energy sources is increasingly depleted, stimulates people to look for the alternative energy and effective energy storage
Device, power density is high, the charging interval is short, service life is long, good temp characteristic, the saving energy because it has for ultracapacitor
And the features such as green, there is good application prospect in fields such as hybrid electric vehicle, electric car and back-up sources, by people
Concern.
Activated carbon is because having the advantages that the ratio surface of super large, stable chemical performance, preferable electric conductivity, becoming super
One of important materials of level electrode for capacitors.
It is contemplated that whether can be utilized obtained nitrogenous based thermoset polymer again, nitrogenous activity is prepared
Charcoal material, is applied in capacitor.Rationally reuse, environmental protection and energy saving, technique is simple, and cost is low, has important reality
Border application value.
The content of the invention
The invention aims to solve the waste degradation complex process of nitrogenous based thermoset polymer, cost is higher
A kind of and the problem of cannot be used in ultracapacitor, there is provided preparation method and applications of nitrogen-dopped activated carbon.
A kind of preparation method of nitrogen-dopped activated carbon of the present invention, is carried out as follows：
First, p-phenylenediamine, paraformaldehyde and N-methyl pyrrolidones are put into three-necked bottle, nitrogen environment protection, magnetic force
Stirring, reaction terminate rear temperature and are down to room temperature, obtain aminal dynamic covalent networks structural polymer spawn；
2nd, aminal dynamic covalent networks structural polymer spawn is settled with acetone, suction filtration is dried in vacuo
To aminal dynamic covalent networks structural polymer product；
3rd, aminal dynamic covalent networks structural polymer product is placed in tube furnace and carries out high temperature pyrolysis, produce nitrogen
Dopped activated carbon；Wherein the mol ratio of p-phenylenediamine and paraformaldehyde is 1:(1~6), p-phenylenediamine and N-methyl pyrrolidones
Molal volume compare 1mmol:(2ml~5ml).
The application of nitrogen-dopped activated carbon of the present invention refers to nitrogen-dopped activated carbon being applied in ultracapacitor, application process
For：Using nickel foam as collector, with nitrogen-dopped activated carbon, acetylene black and PVDF in mass ratio 8:1:1 preparation work electrode,
Commercially to use activated carbon, acetylene black, PVDF in mass ratio 8:1:1 prepares to electrode, assembles electrochemical capacitor.
The Preparation equipment of the present invention is simple, environmental protection and energy saving, and insoluble insoluble thermosetting polymer is carried out appropriate by made from
Processing, can be reused, and simple to operate, be easy to mass produce；The nitrogen-dopped activated carbon obtained can be used as super electricity
Container electrode material, the electrode material of preparation can keep stablizing reversible electrochemical properties, and with the increase of sweep speed, ring
Induced current increases successively, illustrates there is preferable high rate performance.
Brief description of the drawings
The photo of ultracapacitor working electrode prepared by the nitrogen-dopped activated carbon that Fig. 1 is obtained by embodiment 1；
Fig. 2 is the ultracapacitor photo that the nitrogen-dopped activated carbon that embodiment 1 obtains is working electrode assembling；
Fig. 3 by embodiment 1 obtain with nitrogen-dopped activated carbon prepare working electrode in 6M potassium hydroxide electrolytes
Different scanning speed under cyclic voltammetry curve；Wherein a is 1mV/s, b 3mV/s, c 5mV/s；
Fig. 4 is obtained electric in 6M potassium hydroxide with working electrode prepared by nitrogen-dopped activated carbon by the embodiment of the present invention 1
Solve the constant current charge-discharge curve in liquid；Wherein a is 1A/g, b 2A/g, c 3A/g, d 4A/g, e 5A/g；
Fig. 5 is obtained electric in 6M potassium hydroxide with working electrode prepared by nitrogen-dopped activated carbon by the embodiment of the present invention 1
Solve the specific capacitance curve for calculating gained in liquid according to constant current charge-discharge curve；
Fig. 6 is the working electrode prepared with nitrogen-dopped activated carbon of the acquisition of the embodiment of the present invention 2 in 1M sodium sulphate electrolyte
In different scanning speed under cyclic voltammetry curve；Wherein a is 1mV/s, b 8mV/s, c 10mV/s；
Fig. 7 is the working electrode prepared with nitrogen-dopped activated carbon of the acquisition of the embodiment of the present invention 3 in 1M sodium sulphate electrolyte
In constant current charge-discharge curve；Wherein a is 0.5A/g, b 1A/g, c 2A/g, d 3A/g；
Fig. 8 is the working electrode prepared with nitrogen-dopped activated carbon of the acquisition of the embodiment of the present invention 3 in 1M sodium sulphate electrolyte
The middle specific capacitance curve that gained is calculated according to constant current charge-discharge curve.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.
Embodiment one：A kind of preparation method of nitrogen-dopped activated carbon of present embodiment, is carried out as follows：
First, p-phenylenediamine, paraformaldehyde and N-methyl pyrrolidones are put into three-necked bottle, nitrogen environment protection, magnetic force
Stirring, reaction terminate rear temperature and are down to room temperature, obtain aminal dynamic covalent networks structural polymer spawn；
2nd, aminal dynamic covalent networks structural polymer spawn is settled with acetone, suction filtration is dried in vacuo
To aminal dynamic covalent networks structural polymer product；
3rd, aminal dynamic covalent networks structural polymer product (PHDN) is placed in tube furnace and carries out high temperature pyrolysis,
Produce nitrogen-dopped activated carbon；Wherein the mol ratio of p-phenylenediamine and paraformaldehyde is 1:(1~6), p-phenylenediamine and N-methyl pyrrole
The molal volume of pyrrolidone compares 1mmol:(2ml~5ml).
The application of the nitrogen-dopped activated carbon of present embodiment refers to nitrogen-dopped activated carbon being applied in ultracapacitor, should
It is with method：Using nickel foam as collector, with nitrogen-dopped activated carbon, acetylene black and PVDF in mass ratio 8:1:1 prepares work
Make electrode, commercially to use activated carbon, acetylene black, PVDF in mass ratio 8:1:1 prepares to electrode, assembles electrochemical capacitor.
The Preparation equipment of present embodiment is simple, environmental protection and energy saving, and insoluble insoluble thermosetting polymer is carried out by made from
Proper treatment, it can reuse, and it is simple to operate, it is easy to mass produce；The activated carbon obtained can be used as super capacitor
Device electrode material, the electrode material of preparation can keep stablizing reversible electrochemical properties, and with the increase of sweep speed, response
Electric current increases successively, illustrates there is preferable high rate performance.
Embodiment two：Present embodiment is unlike embodiment one：In step 1 p-phenylenediamine and
The mol ratio of paraformaldehyde is 1:5.It is other identical with embodiment one.
Embodiment three：Present embodiment is unlike embodiment one or two：To benzene two in step 1
The molal volume of amine and N-methyl pyrrolidones compares 1mmol:3ml.It is other identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Magnetic in step 1
Power stirring refers to the magnetic agitation 24h under conditions of 50 DEG C.It is other identical with one of embodiment one to three.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Institute in step 3
The method for the high temperature pyrolysis stated is：The PHDN is placed in porcelain boat, is then placed in tube furnace；Be passed through into tube furnace nitrogen or
Argon gas removes 3~8h of oxygen, and nitrogen or argon gas are warming up to as protection gas, then by tube furnace with 3~5 DEG C/min speed
200 DEG C, be then warming up to 450 DEG C with 0.5~2 DEG C/min speed, then with 2~6 DEG C/min speed be warming up to 600 DEG C~
1100 DEG C, keep 2~4h；Then 400 DEG C are cooled to 3~5 DEG C/min speed, then are down to room temperature, that is, completed.Other and tool
One of body embodiment one to four is identical.
Embodiment six：Unlike one of present embodiment and embodiment one to five：Institute in step 3
The method for the high temperature pyrolysis stated is：The PHDN is placed in porcelain boat, is then placed in tube furnace；Be passed through into tube furnace nitrogen or
Argon gas removes oxygen 6h, and nitrogen or argon gas are warming up into 200 DEG C with 5 DEG C/min speed as protection gas, then by tube furnace, so
450 DEG C are warming up to 1 DEG C/min speed afterwards, then 700 DEG C are warming up to 4 DEG C/min speed, keeps 2h；Then with 5 DEG C/
Min speed is cooled to 400 DEG C, then is down to room temperature, that is, completes.It is other identical with one of embodiment one to five.
Embodiment seven：The application of present embodiment nitrogen-dopped activated carbon refers to be applied to surpass by nitrogen-dopped activated carbon
In level capacitor, application process is：Using nickel foam as collector, quality is pressed with nitrogen-dopped activated carbon, acetylene black and PVDF
Than 8:1:1 preparation work electrode, commercially to use activated carbon, acetylene black, PVDF in mass ratio 8:1:1 prepares to electrode, assembling electricity
Chemical capacitor.
Embodiment eight：Present embodiment is unlike embodiment seven：The specific method of application is：
First, porous nickel mesh is cut into 1 × 1cm2Square, nickel bar and the nickel foam that cuts out then are welded together into structure with mash welder
Into collector；2nd, Kynoar is dissolved in 1-METHYLPYRROLIDONE, is made into the PVDF/NMP solution that mass fraction is 4%, makees
For binding agent；3rd, by nitrogen-dopped activated carbon, acetylene black, PVDF solid contents in mass ratio 8:1:1 mixing, is placed in container, magnetic force
5~24h is stirred, then on a current collector, then 100 DEG C of vacuum drying 12h are subsequently placed in hydraulic press uniform blade coating, then with 1
~10MPa pressure will be compacted, as ultracapacitor working electrode.It is other identical with embodiment seven.
Embodiment nine：Present embodiment is unlike embodiment seven or eight：Described super capacitor
The reference electrode of device is mercury/mercury oxide, and electrolyte is 6M potassium hydroxide.It is other identical with embodiment seven or eight.
Embodiment ten：Unlike one of present embodiment and embodiment seven to nine：Described is super
The reference electrode of capacitor is silver/silver chlorate, and electrolyte is 1M sodium sulphate.Other phases one of with embodiment seven to nine
Together.
Beneficial effects of the present invention are verified by following examples：
Embodiment 1, a kind of preparation method of nitrogen-dopped activated carbon, it is to carry out as follows：
First, 10mmol p-phenylenediamine, 50mmol paraformaldehydes and 30mL N-methyl pyrrolidones are put into three-necked bottle, nitrogen
Gas environmental protection, 50 DEG C of magnetic agitation 24h, reaction terminate rear temperature and are down to room temperature, obtain the covalent net of 1.3000g aminals dynamic
Network structural polymer spawn；
2nd, aminal dynamic covalent networks structural polymer spawn is settled with acetone, suction filtration is dried in vacuo
To aminal dynamic covalent networks structural polymer product；
3rd, 0.8g aminal dynamic covalent networks structural polymer products are weighed to be put into tube furnace, are led into tube furnace
Enter argon gas or nitrogen removes oxygen 6h, and as protection gas, tube furnace is then warming up to 200 DEG C with 4 DEG C/min speed, afterwards
1 DEG C/min speed is warming up to 450 DEG C, is then warming up to 600 DEG C with 5 DEG C/min speed, keeps 3h；Again with 5 DEG C/min's
Speed is cooled to 400 DEG C, is finally down to room temperature naturally again, obtains nitrogen-dopped activated carbon, and weigh 0.384g, yield 48.6%.
The nitrogen-dopped activated carbon of preparation is applied in ultracapacitor, application process is：Porous nickel mesh is cut into 1 first
×1cm2Square, nickel bar and the nickel foam that cuts out then are welded together into composition collector with mash welder；Inclined fluorine will be gathered
Ethene (PVDF) is dissolved in 1-METHYLPYRROLIDONE (NMP), the PVDF/NMP solution that mass fraction is 4% is made into, as binding agent；
By nitrogen-dopped activated carbon, acetylene black, PVDF (solid content) in mass ratio 8:1:1 mixing, is placed in container, magnetic agitation 24h, will
Uniformly blade coating on a current collector, makes it be uniformly distributed in the hole of nickel foam, 100 DEG C of vacuum are done afterwards to the paste become reconciled
Dry 12h, finally the complete electrode slice of drying is placed in hydraulic press, is compacted electrode slice with 3MPa pressure, as super capacitor
Device working electrode.Commercially to use activated carbon, acetylene black, PVDF in mass ratio 8:1:1 prepares to electrode, is assembled into super capacitor
Device；Reference electrode is mercury/mercury oxide；Electrolyte is 6M potassium hydroxide.Test sample is labeled as PHDN-AC-1.
Ultracapacitor working electrode prepared by the activated carbon obtained to the present embodiment is in 6M potassium hydroxide electrolytes
The middle cyclic voltammetric performance test carried out without sweep speed, as a result referring to Fig. 3, there is preferably circulation bent under different scanning speed
Line.As Fig. 4 constant current charge-discharges figure understands that curve shows good triangle, and under 1A/g current density, specific capacitance can
To reach 153.8F/g, when current density increase, in 5A/g, specific capacitance stills remain in 108F/g, shows preferably again
Rate performance.
Ultracapacitor working electrode prepared by the activated carbon obtained to the present embodiment is in potassium hydroxide electrolyte
The specific capacitance calculating obtained by constant current charge-discharge performance test is carried out, as a result electric capacity difference 153.8,128.6,120.6,
109.8,108.4F/g, referring to Fig. 5.
Embodiment 2, a kind of preparation method of nitrogen-dopped activated carbon, it is to carry out as follows：
First, 10mmol p-phenylenediamine, 50mmol paraformaldehydes and 30mL N-methyl pyrrolidones are put into three-necked bottle, nitrogen
Gas environmental protection, 50 DEG C of magnetic agitation 24h, reaction terminate rear temperature and are down to room temperature, obtain the covalent net of 1.3000g aminals dynamic
Network structural polymer spawn；
2nd, aminal dynamic covalent networks structural polymer spawn is settled with acetone, suction filtration is dried in vacuo
To aminal dynamic covalent networks structural polymer product；
3rd, 0.8g aminal dynamic covalent networks structural polymer products are weighed to be put into tube furnace, are led into tube furnace
Enter argon gas or nitrogen removes oxygen 6h, and as protection gas, tube furnace is then warming up to 200 DEG C with 4 DEG C/min speed, afterwards
1 DEG C/min speed is warming up to 450 DEG C, is then warming up to 600 DEG C with 5 DEG C/min speed, keeps 3h；Again with 5 DEG C/min's
Speed is cooled to 400 DEG C, is finally down to room temperature naturally again, obtains nitrogen-dopped activated carbon, and weigh 0.384g, yield 48.6%.
The nitrogen-dopped activated carbon of preparation is applied in ultracapacitor, application process is：Porous nickel mesh is cut into 1 first
×1cm2Square, nickel bar and the nickel foam that cuts out then are welded together into composition collector with mash welder；Inclined fluorine will be gathered
Ethene (PVDF) is dissolved in 1-METHYLPYRROLIDONE (NMP), the PVDF/NMP solution that mass fraction is 4% is made into, as binding agent；
By nitrogen-dopped activated carbon, acetylene black, PVDF (solid content) in mass ratio 8:1:1 mixing, is placed in container, magnetic agitation 18h, will
Uniformly blade coating on a current collector, makes it be uniformly distributed in the hole of nickel foam, 100 DEG C of vacuum are done afterwards to the paste become reconciled
Dry 12h, finally the complete electrode slice of drying is placed in hydraulic press, is compacted electrode slice with 3MPa pressure, as super capacitor
Device working electrode.Commercially to use activated carbon, acetylene black, PVDF in mass ratio 8:1:1 prepares to electrode, is assembled into super capacitor
Device；Reference electrode is silver/silver chlorate；Electrolyte is 1M sodium sulphate.Test sample is labeled as PHDN-AC-2.
Ultracapacitor working electrode prepared by the activated carbon obtained to the present embodiment enters in sodium sulphate electrolyte
Row does not have to the cyclic voltammetric performance test of sweep speed, as a result referring to Fig. 6.There is preferable cyclic curve under different scanning speed,
In aqueous systems, electrochemical window can reach 1.5V.As Fig. 7 constant current charge-discharges figure understands that curve shows good three
Angular, under 1A/g current density, specific capacitance 88F/g, when current density increase, in 5A/g, specific capacitance is about 66F/
G, show preferable high rate performance.
Ultracapacitor working electrode prepared by the activated carbon obtained to the present embodiment is in potassium hydroxide electrolyte
The specific capacitance calculating obtained by constant current charge-discharge performance test is carried out, as a result specific capacitance difference 153.8F/g, 128.6F/g,
120.6F/g, 109.8F/g, 108.4F/g, referring to Fig. 8.
The Preparation equipment of embodiment 1~2 is simple, environmental protection and energy saving, and insoluble insoluble thermosetting polymer is carried out by made from
Proper treatment, it can reuse, and it is simple to operate, it is easy to mass produce；The nitrogen-dopped activated carbon obtained can be used as super
Level capacitor electrode material, the electrode material of preparation can keep stablizing reversible electrochemical properties, and with the increasing of sweep speed
Add, response current increases successively, illustrates there is preferable high rate performance.
Claims (6)
1. a kind of preparation method of nitrogen-dopped activated carbon, it is characterised in that this method is carried out as follows：
First, p-phenylenediamine, paraformaldehyde and N-methyl pyrrolidones are put into three-necked bottle, nitrogen environment protection, magnetic agitation,
Reaction terminates rear temperature and is down to room temperature, obtains aminal dynamic covalent networks structural polymer spawn；
2nd, aminal dynamic covalent networks structural polymer spawn is settled with acetone, filters vacuum drying and contracted
Aldehyde amine dynamic covalent networks structural polymer product；
3rd, aminal dynamic covalent networks structural polymer product is placed in tube furnace and carries out high temperature pyrolysis, produce N doping
Activated carbon；Wherein the mol ratio of p-phenylenediamine and paraformaldehyde is 1:5, the molal volume of p-phenylenediamine and N-methyl pyrrolidones
Compare 1mmol:3ml；Prepared nitrogen-dopped activated carbon is used in ultracapacitor；The method of high temperature pyrolysis described in step 3
For：Aminal dynamic covalent networks structural polymer product is placed in porcelain boat, is then placed in tube furnace；It is passed through into tube furnace
Nitrogen or argon gas remove 3~8h of oxygen, and using nitrogen or argon gas as protection gas, then by tube furnace with 3~5 DEG C/min speed liter
Then temperature is warming up to 450 DEG C, then be warming up to 600 DEG C with 2~6 DEG C/min speed to 200 DEG C with 0.5~2 DEG C/min speed
~1100 DEG C, keep 2~4h；Then 400 DEG C are cooled to 3~5 DEG C/min speed, then are down to room temperature, that is, completed；
The nitrogen-dopped activated carbon is applied in ultracapacitor, and application process is：Using nickel foam as collector, with N doping
Activated carbon, acetylene black and PVDF in mass ratio 8:1:1 preparation work electrode, commercially to use activated carbon, acetylene black, PVDF to press quality
Than 8:1:1 prepares to electrode, assembles electrochemical capacitor.
2. the preparation method of a kind of nitrogen-dopped activated carbon according to claim 1, it is characterised in that magnetic force stirs in step 1
Mix and refer to the magnetic agitation 24h under conditions of 50 DEG C.
3. the preparation method of a kind of nitrogen-dopped activated carbon according to claim 1, it is characterised in that described in step 3
The method of high temperature pyrolysis is：Aminal dynamic covalent networks structural polymer product is placed in porcelain boat, is then placed in tube furnace；
Nitrogen is passed through into tube furnace or argon gas removes oxygen 6h, and using nitrogen or argon gas as protection gas, then by tube furnace with 5 DEG C/min
Speed be warming up to 200 DEG C, be then warming up to 450 DEG C with 1 DEG C/min speed, then 700 are warming up to 4 DEG C/min speed
DEG C, keep 2~4h；Then 400 DEG C are cooled to 5 DEG C/min speed, then are down to room temperature, that is, completed.
A kind of 4. preparation method of nitrogen-dopped activated carbon according to claim 1, it is characterised in that the specific method of application
For：First, porous nickel mesh is cut into 1 × 1cm2Square, nickel bar and the nickel foam that cuts out then are welded on one with mash welder
Rise and form collector；2nd, Kynoar is dissolved in 1-METHYLPYRROLIDONE, it is molten is made into the PVDF/NMP that mass fraction is 4%
Liquid, as binding agent；3rd, by nitrogen-dopped activated carbon, acetylene black, PVDF solid contents in mass ratio 8:1:1 mixing, is placed in container
In, 5~24h of magnetic agitation is then uniform to scratch on a current collector, is dried in vacuo 12h at 100 DEG C, is subsequently placed in hydraulic press
In, then will compacting, as ultracapacitor working electrode with 1~10MPa pressure；Matter is pressed with activated carbon, acetylene black, PVDF
Measure ratio 8:1:1 prepares to electrode, is assembled into ultracapacitor.
5. according to a kind of preparation method of nitrogen-dopped activated carbon of claim 1 or 4, it is characterised in that described ultracapacitor
Reference electrode is mercury/mercury oxide, and electrolyte is 6M potassium hydroxide.
6. according to a kind of preparation method of nitrogen-dopped activated carbon of claim 1 or 4, it is characterised in that described ultracapacitor
Reference electrode is silver/silver chlorate, and electrolyte is 1M sodium sulphate.
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