CN106783204B - The preparation method of electric chemical super capacitor material based on luffa meso-porous carbon material - Google Patents
The preparation method of electric chemical super capacitor material based on luffa meso-porous carbon material Download PDFInfo
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of preparation methods of electric chemical super capacitor material based on luffa meso-porous carbon material, the technique is by carrying out active carbide to biological material luffa, it makes it through a series of chemical reaction and forms hole Carbon Materials structure, wherein utilize ammonia, nitrogen activation, pyroreaction, pickling washing, oil bath is boiled, the process means such as vacuum drying improve the chemical property of luffa active carbon significantly, pressed-disc technique is subsequently used for by compound luffa hole Carbon Materials coated on nickel material electrode, so that the electric chemical super capacitor material based on luffa meso-porous carbon material being prepared, its specific capacity is big, energy density is good, cycle charge discharge electrical stability is high, in addition the preparation process environment-protection low-consumption, process is simple, raw material is cheap and easy to get, with preferable industrial applications prospect.It also discloses and is applied in the fields such as instrument and meter, digital product, wireless phone, LED compact illumination as made from the preparation process based on the electric chemical super capacitor material of luffa meso-porous carbon material simultaneously.
Description
Technical field
The present invention relates to Material Fields, are related specifically to a kind of electric chemical super capacitor based on luffa meso-porous carbon material
The preparation method of equipment material.
Background technique
Traditional fossil resource increasingly consumes environmental pollution and global warming issue brought by exhausted and burning fuel
Have become the problem that countries in the world need to overcome, and as 18 the fifth plenary sessions proposition is promoted a conservation culture, urgently needs
Clean energy resource is produced, therefore develops and utilizes renewable and clean energy resource and traditional fossil resource is replaced to become current economic development
Inevitable choice under mode.Energy battery novel at present, such as lithium ion battery, fuel cell, supercapacitor, solar-electricity
Pond, air cell and sodium lithium battery etc. are gradually applied in national economy every field.In renewable and clean energy resource battery,
Supercapacitor and fuel cell be considered as it is most potential become most widely used, the most energy storage of practicability
One of part or conversion equipment, they can be used as the power supply of portable equipment, can also be used as fixed equipment energy storage device.
Renewable since plant medium is resourceful, cheap feature will prepare the important presoma of carbon material.It plants
Object material often has level pore structure abundant, if by screening varieties, the technique that controls synthesis, it is easy to be retained
The carbon of plant pore structure.In recent years, various living resources are used as the different porous carbon of precursor preparation pattern, and
With good super capacitor performance, and the carbon material of plant resources also has been reported that as redox reaction catalyst.In crowd
In more plants, luffa has the characteristics that distributed more widely, cheap and easy to get as common one of living resources.It is silk
The vascular bundle that the ripening fruits of melon obtains after drying, have very unique structure: every fiber contains micron-sized intensive flat
The duct composition of row arrangement.If remaining the structure of this fiber to form huge hole carbon during carbonization, this will
It is a kind of very novel carbon pattern, but up to the present, occurs still without about the Related product for preparing carbon with luffa, this
Invention is dedicated to developing a kind of preparation method of luffa hole carbon material, using with supercapacitor field, to expect to be
The development of capacitor provides some new approach and break-through point.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of electric chemical super capacitor based on luffa meso-porous carbon material
The preparation method of equipment material makes it through a series of chemical reaction by carrying out active carbide to biological material luffa
Hole Carbon Materials structure is formed, wherein utilizing ammonia, nitrogen activation, pyroreaction, pickling is washed, and oil bath is boiled, vacuum drying etc.
Process means improve the chemical property of luffa active carbon significantly, and being subsequently used for pressed-disc technique will be compound
Luffa hole Carbon Materials are coated on nickel material electrode, so that the electrochemistry based on luffa meso-porous carbon material being prepared is super
Grade capacitor material, specific capacity is big, energy density is good, cycle charge discharge electrical stability is high, in addition the preparation process environment-protection low-consumption,
Process is simple, and raw material is cheap and easy to get, has preferable industrial applications prospect.
The purpose of the present invention can be achieved through the following technical solutions:
The preparation method of electric chemical super capacitor material based on luffa meso-porous carbon material, comprising the following steps:
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and time 30-40min obtains luffa
Active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 10-15min, be then dried in vacuo standby
With;
(5) by 1-3 parts of 10-16 parts of luffa active carbon, the carbon black of step (4), 1-3 parts of acetylene black, polytetrafluoroethylene (PTFE) 2-4
Part, two 1-5 parts of methacrylaldehyde contracting pentaerythrites, 1-5 parts of 2- methylol -2- methyl-1,3-propanediol, pyridine -4- formylhydrazine 1-2
Part, 3-6 part of dehydrated alcohol be uniformly mixed, stirring pulp mixed liquors, then ultrasonic disperse, ultrasonic power 220KW, 10-
20min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min are dried in vacuo 10-12h;
(7) take out step (6) luffa active carbon nickel disk into be put into argon gas incubator stand 2-3h, take out up at
Product.
Preferably, heating rate is 20 DEG C/min in the step (2).
Preferably, vacuum drying temperature is 75 DEG C in the step (4).
Preferably, vacuum drying temperature is 55 DEG C in the step (6).
Preferably, holding temperature is 42 DEG C in the step (7).
The present invention also provides the electric chemical super electricity based on luffa meso-porous carbon material obtained by above-mentioned preparation process
Container material is applied in the fields such as instrument and meter, digital product, wireless phone, LED compact illumination.
Compared with prior art, the present invention has the advantages that:
(1) preparation method of the electric chemical super capacitor material of the invention based on luffa meso-porous carbon material by pair
Biological material luffa carries out active carbide, makes it through a series of chemical reaction and forms hole Carbon Materials structure, wherein benefit
With ammonia, nitrogen activation, pyroreaction, pickling is washed, and oil bath is boiled, and the process means such as vacuum drying make luffa active carbon
Chemical property significantly improved, be subsequently used for pressed-disc technique for compound luffa hole Carbon Materials coated on nickel material
Expect on electrode, so that the electric chemical super capacitor material based on luffa meso-porous carbon material being prepared, specific capacity is big,
Energy density is good, cycle charge discharge electrical stability is high, in addition the preparation process environment-protection low-consumption, and process is simple, and raw material is cheap and easy to get, tool
There is preferable industrial applications prospect.
(2) the electric chemical super capacitor material process of the invention based on luffa meso-porous carbon material is simple, operation side
Just, raw material is easy to get, environment-protection low-consumption, is suitable for big rule industrialization and uses, practical.
Specific embodiment
The technical solution of invention is described in detail combined with specific embodiments below.
Embodiment 1
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, and the time is
30min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 10min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) by 1 part of 10 parts of luffa active carbon, the carbon black of step (4), 1 part of acetylene black, 2 parts of polytetrafluoroethylene (PTFE), two propylene
1 part of aldehyde contracting pentaerythrite, 1 part of 2- methylol -2- methyl-1,3-propanediol, 1 part of pyridine -4- formylhydrazine, 3 parts of dehydrated alcohol it is mixed
It closes uniformly, stirs pulp mixed liquor, then ultrasonic disperse, ultrasonic power 220KW, 10min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min, are dried in vacuo 10h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 2h, holding temperature 42 into argon gas incubator is put into
DEG C, taking-up is got product.
The performance test results of electric chemical super capacitor material obtained based on luffa meso-porous carbon material such as 1 institute of table
Show.
Embodiment 2
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, and the time is
33min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 12min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) by 2 parts of 12 parts of luffa active carbon, the carbon black of step (4), 1 part of acetylene black, 3 parts of polytetrafluoroethylene (PTFE), two propylene
2 parts of aldehyde contracting pentaerythrite, 3 parts of 2- methylol -2- methyl-1,3-propanediol, 1 part of pyridine -4- formylhydrazine, 4 parts of dehydrated alcohol it is mixed
It closes uniformly, stirs pulp mixed liquor, then ultrasonic disperse, ultrasonic power 220KW, 13min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min, are dried in vacuo 10.5h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 2.2h into argon gas incubator is put into, and holding temperature is
42 DEG C, taking-up is got product.
The performance test results of electric chemical super capacitor material obtained based on luffa meso-porous carbon material such as 1 institute of table
Show.
Embodiment 3
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, and the time is
36min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 14min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) by 2 parts of 14 parts of luffa active carbon, the carbon black of step (4), 2 parts of acetylene black, 3 parts of polytetrafluoroethylene (PTFE), two propylene
4 parts of aldehyde contracting pentaerythrite, 3 parts of 2- methylol -2- methyl-1,3-propanediol, 2 parts of pyridine -4- formylhydrazine, 5 parts of dehydrated alcohol it is mixed
It closes uniformly, stirs pulp mixed liquor, then ultrasonic disperse, ultrasonic power 220KW, 17min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min, are dried in vacuo 11h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 2.6h into argon gas incubator is put into, and holding temperature is
42 DEG C, taking-up is got product.
The performance test results of electric chemical super capacitor material obtained based on luffa meso-porous carbon material such as 1 institute of table
Show.
Embodiment 4
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, and the time is
40min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 15min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) by 3 parts of 16 parts of luffa active carbon, the carbon black of step (4), 3 parts of acetylene black, 4 parts of polytetrafluoroethylene (PTFE), two propylene
5 parts of aldehyde contracting pentaerythrite, 5 parts of 2- methylol -2- methyl-1,3-propanediol, 2 parts of pyridine -4- formylhydrazine, 6 parts of dehydrated alcohol it is mixed
It closes uniformly, stirs pulp mixed liquor, then ultrasonic disperse, ultrasonic power 220KW, 20min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min, are dried in vacuo 12h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 3h, holding temperature 42 into argon gas incubator is put into
DEG C, taking-up is got product.
The performance test results of electric chemical super capacitor material obtained based on luffa meso-porous carbon material such as 1 institute of table
Show.
Comparative example 1
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, and the time is
30min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 10min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) by 10 parts of the luffa active carbon of step (4), 1 part of acetylene black, 2 parts of polytetrafluoroethylene (PTFE), two methacrylaldehyde contracting seasons penta
1 part of tetrol, 2- methylol -2- methyl-1,1 part of 3-propanediol, 3 portions of dehydrated alcohol uniformly mixed, stirring pulp mixed liquors, so
Ultrasonic disperse afterwards, ultrasonic power 220KW, 10min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min, are dried in vacuo 10h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 2h, holding temperature 42 into argon gas incubator is put into
DEG C, taking-up is got product.
The performance test results of electric chemical super capacitor material obtained based on luffa meso-porous carbon material such as 1 institute of table
Show.
Comparative example 2
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects case
It is activated in formula atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, and the time is
40min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 15min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) by 4 parts of 3 parts of 16 parts of luffa active carbon, carbon black, the polytetrafluoroethylene (PTFE) of step (4), 2- methylol -2- methyl -
5 parts of 1,3-PD, 2 parts of pyridine -4- formylhydrazine, 6 portions of dehydrated alcohol uniformly mixed, stirring pulp mixed liquors, it is then ultrasonic
Dispersion, ultrasonic power 220KW, 20min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure is
20MPa, duration 1.5min, are dried in vacuo 12h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 3h, holding temperature 42 into argon gas incubator is put into
DEG C, taking-up is got product.
The performance test results of electric chemical super capacitor material obtained based on luffa meso-porous carbon material such as 1 institute of table
Show.
By the electric chemical super capacitor based on luffa meso-porous carbon material made from embodiment 1-4 and comparative example 1-2
Material carries out specific capacity, capacity retention rate, this several energy density, current density coefficient of stabilization performance tests.
Table 1
Specific capacitance (F/g, 1A/g) | Capacity retention rate (%, 5000 cyclic voltammetries) | Energy density (Wh/kg) | Current density coefficient of stabilization (%, 12h, compared with original value) | |
Embodiment 1 | 418 | 95.7 | 10.30 | 88.5 |
Embodiment 2 | 416 | 96.1 | 10.24 | 89.3 |
Embodiment 3 | 414 | 95.3 | 10.29 | 87.3 |
Embodiment 4 | 416 | 96.3 | 10.21 | 87.9 |
Comparative example 1 | 263 | 76.3 | 8.31 | 65.3 |
Comparative example 2 | 301 | 80.2 | 7.29 | 71.6 |
The preparation method of electric chemical super capacitor material based on luffa meso-porous carbon material of the invention passes through to life
Material luffa carries out active carbide, makes it through a series of chemical reaction and forms hole Carbon Materials structure, wherein utilizing
Ammonia, nitrogen activation, pyroreaction, pickling washing, oil bath are boiled, and the process means such as vacuum drying make luffa active carbon
Chemical property is significantly improved, and is subsequently used for pressed-disc technique for compound luffa hole Carbon Materials coated on nickel material
On electrode, so that the electric chemical super capacitor material based on luffa meso-porous carbon material being prepared, specific capacity is big, energy
Metric density is good, cycle charge discharge electrical stability is high, in addition the preparation process environment-protection low-consumption, and process is simple, and raw material is cheap and easy to get, has
Preferable industrial applications prospect.Electric chemical super capacitor material process letter based on luffa meso-porous carbon material of the invention
Single, easy to operate, raw material is easy to get, environment-protection low-consumption, is suitable for big rule industrialization and uses, practical.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (2)
1. the preparation method of the electric chemical super capacitor material based on luffa meso-porous carbon material, which is characterized in that including with
Lower step:
(1) luffa is cleaned, 65 DEG C of drying are placed in high temperature furnace and are carbonized, while ammonia activation is added;
(2) the luffa carbide of step (1) and potassium hydroxide are mixed according to the ratio of 9:2, grinding uniformly, injects box gas
It is activated in atmosphere furnace, while being filled with nitrogen protection, activation temperature is 880 DEG C, and heating rate is 20 DEG C/min, time 30-
40min obtains luffa active carbon;
(3) then the luffa active carbon in step (2) is rinsed 2 times with salt acid elution 2 times of 3% with deionized water;
(4) the luffa active carbon in step (3) is put into oil bath pan and boils 10-15min, be then dried in vacuo it is spare, very
The dry temperature of sky is 75 DEG C;
(5) 2 parts of 12 parts of luffa active carbon, the carbon black of step (4), 1 part of acetylene black, 3 parts of polytetrafluoroethylene (PTFE), two methacrylaldehyde are contracted
2 parts of pentaerythrite, 3 parts of 2- methylol -2- methyl-1,3-propanediol, 1 part of pyridine -4- formylhydrazine, 4 parts of dehydrated alcohol mixing are equal
It is even, pulp mixed liquor is stirred, then ultrasonic disperse, ultrasonic power 220KW, 10-20min;
(6) the pulpous state mixed liquor of step (5) is coated on nickel foam disk, is put on tablet press machine and suppresses, pressure 20MPa,
Duration is 1.5min, is dried in vacuo 10-12h, and vacuum drying temperature is 55 DEG C;
(7) the luffa active carbon nickel disk for taking out step (6) stands 2-3h, holding temperature 42 into argon gas incubator is put into
DEG C, taking-up is got product.
2. the electric chemical super capacitor based on luffa meso-porous carbon material that preparation process according to claim 1 obtains
Material is applied in field in instrument and meter, digital product, wireless phone, LED compact illumination.
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CN102509643A (en) * | 2011-11-29 | 2012-06-20 | 西北师范大学 | Graphene/carbon ball composite material, and preparation and application thereof |
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