CN107555430A - A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method - Google Patents
A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method Download PDFInfo
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Abstract
A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method, choose the soft pin that comes off, clean drying after the removal of impurity repeatedly with pure water；The soft pin that comes off of drying is crushed to powder with pulverizer, is placed in stand-by in drier；Pine needle powder after crushing is placed in ceramic crucible, placed into Muffle furnace, in air atmosphere, from room temperature to final carbonization temperature；To the end of charring process, temperature is down to room temperature, and gained pine needle Quito mesoporous activated carbon is carried out into pickling and washing, removes therein organic and inorganic impurity, 110 DEG C dry again, are placed in dry environment, you can obtain ultracapacitor pine needle matrix activated carbon material.Preparation process cleaning of the present invention, step is simple, and product structure is various controllable, and capacitive property high rate capability is excellent, and manufacturing cost is low.
Description
Technical field
The invention belongs to absorbent charcoal material and charing preparation technology field, and in particular to a kind of with excellent high rate performance
Ultracapacitor pine needle matrix activated carbon material and preparation method thereof.
Background technology
Ultracapacitor has the characteristics that charging rate is fast, power density is high, long lifespan, is to solve power used for electric vehicle
The most effective approach of power supply.The sole power power supply that it can both run as electric vehicle, electric vehicle can also be used as to run
Auxiliary power power supply.Ultracapacitor can be additionally used in photovoltaic cell electric power storage, the stabilization of power grids, radio transmitting constant power device,
And the startup energy of tank, rocket extract；The U.S., Europe, Japan etc. also carry out the research of ultracapacitor.
For pine needle used herein as raw material, wide material sources are cheap, are easy to collect.The eucaryotic cell structure of pine needle in itself,
The metallic element itself having and certain content of heteroatoms.Carbonize, can obtain naturally by a simple step in atmosphere
Porous active Carbon Materials with three-dimensional network shape microstructure.The method need not additionally add any chemical reagents, prepare
Process is very simple, efficient, environmental protection, and reaction vessel will not be caused to corrode.It can only be obtained by the tenor of itself
To certain hole, in temperature-rise period, its sodium contained and potassium atom can produce activation, with carbon-coating occur resolution effect from
And produce substantial amounts of micropore and central hole structure.Meanwhile calcium and magnesium atom can produce occupy-place effect, through overpickling, after washing, also can
Obtain the hole of certain pore size distribution.And air then plays catalytic metal priming reaction in carbonization process, get through between Kong Yukong
Passage and cleaning passage in organic impurities effect.The pine needle Quito mesoporous activated carbon surface finally obtained has substantial amounts of miscellaneous original
Sub- content (N, P, O), can increase the surface wettability of such a material, while improve its chemical property.Simultaneously because its
Body contains substantial amounts of metallic atom, therefore need not additionally add any chemical activation reagent, has broken conventional chemical methods activation
The yoke of activated carbon is prepared, overcomes the shortcomings that conventional chemical methods prepare absorbent charcoal material.Preparation technology is easy, and will not be to life
Production equipment causes to corrode, free from environmental pollution.And such a absorbent charcoal material has excellent times as electrode material for super capacitor
Rate performance, can solve the defects of being commercialized activated carbon for super capacitors material at present, can extend electric car once charging it
Usage time afterwards, there is extraordinary application prospect.
Zhu G et al.（Zhu G, Ma L, Lv H, et al. Pine needle-derived microporous
nitrogen-doped carbon frameworks exhibit high performances in
electrocatalytic hydrogen evolution reaction and supercapacitors[J].
Nanoscale, 2016.）Research is found, pine needle is carried out into low-temperature carbonization, the activated carbon electricity then obtained using KOH activation methods
Pole material, there is higher specific surface area 2433m2/ g, there is condenser of high ratio electric capacity, can reach under 0.1A/g current density
236 F/g, while there is longer and stable cycle life, capacitance fade is not present after 5000 circulations.But in an experiment,
It uses the 4 of big concentration:The alkali of 1 ratio, pollute environment, corrosion reaction equipment, without actual application value.
Biswal M et al. (Biswal M, Banerjee A, Deo M, et al. From dead leaves to
High energy density supercapacitors [J] Energy ＆ Environmental Science, 2013,
6(4):1249-1259.) by being simply carbonized to a kind of distinctive chinaberry leaf of India, porous carbon materials are obtained.And
Its chemical property is analyzed, it is found that it has pole as aqueous super capacitor electrode material under minimum current density
The high F g of quality specific capacitance 400-1 (0.5 A g-1) but this carbon material high rate performance it is poor, it is impossible to be used in it is actual should
With.
An, Hong Joo et al. (An H J, Na R K, Song M Y, et al. Fallen-leaf-
derived microporous pyropolymers for supercapacitors[J]. Journal of
Industrial ＆ Engineering Chemistry, 2016.) leaf that comes off/pyropolymer composite wood is prepared
Material, there is 731 F/g specific capacity, and 1000 cycle performances are good, but long-term cycle stability is poor, and use compound
Material price is expensive, without actual application value, and has used KOH and strong acid, pollutes environment, etching apparatus.
(Alshareef N H, Whitehair D, the Xia C. The Impact of such as Alshareef N H
Surface Chemistry on Bio-derived Carbon Performance as Supercapacitor
Electrodes [J] Journal of Electronic Materials, 2017,46 (3):1628-1636.) use
Eucalyptus leaves is as presoma, and a step is carbonized under an argon atmosphere, but performance is general, the prospect without application.
In summary, although someone is carbonized using the leaf to come off at present, activation is compound with conducting polymer,
It is compound etc. with metallic compound.But all there is certain limitation, and activated using chemical reagent, corrosivity is too strong, if
It is standby invest it is excessive, can not continuous production, and finally produce substantial amounts of toxic gas and liquid and can not reclaim, use is expensive
Conducting polymer and metallic compound carry out compound, step is more, and pollution is big, and performance is general, causes actual application value
It is not high.
The content of the invention
The technical problem of solution：Preparation process is seriously polluted existing for prior art in order to solve, and step is more, and product knot
The problem of structure is single, and capacitive property is low, and cost is high, the present invention propose a kind of ultracapacitor pine with excellent high rate performance
Pin matrix activated carbon material and one step charing preparation method, preparation process cleaning, step is simple, and product structure is various controllable,
Capacitive property high rate capability is excellent, and manufacturing cost is low.
Technical scheme：A kind of ultracapacitor carbonizes preparation method with the step of pine needle matrix activated carbon one, and preparation process is：First
Step, raw material prepare：Selection comes off soft pin, is cleaned after the removal of impurity and dried repeatedly with pure water；Second step, the system of presoma
It is standby：The soft pin that comes off of drying is crushed to powder with pulverizer, is placed in stand-by in drier；3rd step, charing：It will crush
Pine needle powder afterwards is placed in ceramic crucible, places into Muffle furnace, in air atmosphere, from room temperature to final charing temperature
Degree；4th step, washing and drying：To the end of charring process, temperature is down to room temperature, and gained pine needle Quito mesoporous activated carbon is carried out into acid
Wash and wash, remove therein organic and inorganic impurity, 110 DEG C dry again, are placed in dry environment, you can obtain super electricity
Container pine needle matrix activated carbon material.
Preferably, the raw material described in the first step is cedar needles, fall leaves pine needle or needles of pinus massoniana.
Preferably, the mesh number crushed in second step is 60-300 mesh.
Preferably, charing is that in air atmosphere, charing final temperature is 600-1200 DEG C, carbonization time 30-120 in the 3rd step
Min, heating rate are 1-10 DEG C/min.
Preferably, the hydrochloric acid in the 4th step first by " 1+9 " washs through row, reuses deionized water and washs 2-4 times.
The pine needle active charcoal of ultracapacitor made from the above method.
Above-mentioned ultracapacitor pine needle active charcoal, the pore structure to be communicated with one another for three-dimensional network shape, specific surface area 500-
3000 m2/ g, quality specific capacitance 100-400 F/g.
Beneficial effect：Corresponding pine needle Quito mesoporous activated carbon material is prepared using one-step method charing, step is simple, operation letter
Easily, and only by changing the species of pine needle, the temperature of charing, carbonization time, it becomes possible to regulate and control the hole of the activated carbon sample of gained
Footpath distribution, its electrode material as ultracapacitor, there can be excellent high rate performance etc. respectively, it is corresponding so as to be applied to
Demand in.Whole technique need not add any chemical activation reagent, it is only necessary to simple step heating charing, you can
Obtain activated carbon sample to the end.
Brief description of the drawings
Fig. 1 is pine needle matrix activated carbon (1000 DEG C) N prepared by embodiment 52Adsorption-desorption isothermal.
Fig. 2 is 1000 DEG C of pine needle matrix activated carbon prepared by embodiment 5) pore size distribution range.
Fig. 3 is that embodiment 5 prepares pine needle matrix activated carbon (1000 DEG C) SEM figures.
Fig. 4 is pine needle matrix activated carbon (1000 DEG C) constant current charge-discharge curve prepared by embodiment 5.
Fig. 5 is pine needle matrix activated carbon (1000 DEG C) cyclic voltammetric Tequ line prepared by embodiment 5.
Fig. 6 is pine needle matrix activated carbon (1000 DEG C) high rate performance prepared by embodiment 5.
Fig. 7 is pine needle matrix activated carbon (1000 DEG C) impedance behavior prepared by embodiment 5.
Embodiment
The present invention is to a kind of test of the ultracapacitor pine needle matrix activated carbon material property with excellent high rate performance
Method is as follows：
（1）Specific surface area, the measure of pore volume：Measure using activated carbon under the conditions of liquid nitrogen to nitrogen adsorption isotherm, according to
BET formula calculates specific surface area.
（2）Surface topography uses FDAC（Hitachi）The S-4800 type cold field emission electron microscope observations of company.
（3）The measure of specific capacitance：Determined using electrochemical workstation under constant current.
（3）The measure of specific capacitance：Determined using electrochemical workstation under constant current.
A kind of ultracapacitor pine needle matrix activated carbon and one step charing preparation method, comprise the following steps：
Carbonization manufacture method, comprise the following steps：
The first step, raw material prepare：Selection comes off soft pin, after cleaning the removal of impurity repeatedly with pure water, is placed in baking oven 100 DEG C
The lower h of drying 12；
Second step, the preparation of presoma：The obtained soft pin that comes off is crushed to the powder of certain mesh number with pulverizer, is placed in
It is stand-by in drier；
3rd step, charing：Obtained pine needle powder is placed in ceramic crucible, placed into Muffle furnace, in air atmosphere, with one
Fixed heating rate is from room temperature to final carbonization temperature；
4th step, washing and drying：To the end of a step nature charring process, temperature is down to room temperature, by gained pine needle base porous active
Charcoal carries out pickling and repeatedly washing, removes therein organic and inorganic impurity, is finally placed in 110 DEG C of baking ovens fully drying 12
H, the activated carbon sample of drying is fully ground again, is placed in dry environment, you can obtain that there is excellent high rate performance
Ultracapacitor pine needle matrix activated carbon material.
Raw material described in the method for the present invention is cedar needles, pine needle, needles of pinus massoniana etc. of falling leaves.
The mesh number of pine needle after crushed is a certain mesh number in 60-300 mesh.Charing is in air atmosphere, to carbonize final temperature
For 600-1200 DEG C, carbonization time 30-120 min, heating rate is 1-10 DEG C/min.The hydrochloric acid of " 1+9 " is used to be washed through row
Wash, reuse deionized water and wash 2-4 times.Finally it is placed in baking oven and dries, cools down, milling.Obtain ultracapacitor pine needle
Matrix activated carbon material.
A kind of described ultracapacitor with excellent high rate performance pine needle matrix activated carbon material and one step charing
The absorbent charcoal material that preparation method obtains, it is characterised in that specific surface area 500-3000 m2/ g, quality specific capacitance 100-300
F/g, volumetric capacitance can reach 100-300 F/cm3,.
Specific surface area, pore-size distribution, the pore volume of ultracapacitor pine needle matrix activated carbon material of the present invention can be by changing
Become the species of presoma pine needle, the temperature and time of step charing, to be regulated and controled.Obtained activated carbon sample structure is passed through
To control through row.Northern Part of China, green fresh needles and summer are come from using described deodar raw material in the method for the present invention
Pluck in season to obtain, the soft pin that comes off is picked up in autumn.The mesh number of crushing is a certain mesh number in 60-300 mesh.Charing is in air
Under atmosphere, charing final temperature is 600-1200 DEG C, carbonization time 30-120 min, and heating rate is 1-10 DEG C/min.Use " 1+
9 " hydrochloric acid washs through row, reuses deionized water and washs 2-4 times.Finally it is placed in baking oven and dries, cools down, milling.Surpassed
Level capacitor pine needle matrix activated carbon material.
Embodiment 1
（1）It is prepared by presoma：Cedar needles are selected as raw material.Green fresh needles are chosen, is cleaned and cleaned repeatedly with pure water
After matter, it is placed in baking oven at 100 DEG C and dries 12 h.It is 300 that obtained clean green fresh needles pulverizer, which is crushed,
Purpose powder, it is placed in stand-by in drier.
（2）Charing：Obtained pine needle powder is placed in ceramic crucible, is put into Muffle furnace, in air atmosphere, with 1
DEG C/min heating rate keeps 60min from room temperature to final 800 DEG C of carbonization temperature.
（3）Washing and drying：To the end of a step nature charring process, temperature is down to room temperature, by gained pine needle base porous active
Charcoal carries out pickling, and repeatedly washing removes therein organic and inorganic impurity, is finally placed in 110 DEG C of baking ovens fully 12 h of drying,
It is placed in dry environment.Obtained pine needle base super capacitor active carbon material its specific surface area is 1482 m2/ g, total pore volume are
0.31 cm3/ g, the F/g of specific capacitance 223 under 0.5 A/g current density.
Embodiment 2
（1）It is prepared by presoma：Selection fallen leaves pine needle is as raw material.After cleaning the removal of impurity repeatedly with pure water, it is placed in baking oven
12 h are dried at 100 DEG C.Obtained clean green fresh needles pulverizer is crushed into the powder for 150 mesh, is placed in dry
It is stand-by in dry device.
（2）Charing：Obtained pine needle powder is placed in ceramic crucible, is put into Muffle furnace, in air atmosphere, with 5
DEG C/min heating rate keeps 60min from room temperature to final 900 DEG C of carbonization temperature.
（3）Washing and drying：To the end of a step nature charring process, temperature is down to room temperature, by gained pine needle base porous active
Charcoal carries out pickling, and repeatedly washing removes therein organic and inorganic impurity, is finally placed in 110 DEG C of baking ovens fully 12 h of drying,
It is placed in dry environment.Obtained pine needle base super capacitor active carbon material its specific surface area is 1525 m2/ g, total pore volume are
0.50 cm3/ g, the F/g of specific capacitance 160 under 0.5 A/g current density.
Embodiment 3
（1）It is prepared by presoma：Pineneedles of Pinus Massoniana Lamb is selected as raw material.Green fresh needles are chosen, clean removal repeatedly with pure water
After impurity, it is placed in baking oven at 100 DEG C and dries 12 h.It is 60 that obtained clean green fresh needles pulverizer, which is crushed,
Purpose powder, it is placed in stand-by in drier.
（2）Charing：Obtained pine needle powder is placed in ceramic crucible, is put into Muffle furnace, in air atmosphere, with 10
DEG C/min heating rate keeps 60min from room temperature to final 1000 DEG C of carbonization temperature.
（3）Washing and drying：To the end of a step nature charring process, temperature is down to room temperature, by gained pine needle base porous active
Charcoal carries out pickling, and repeatedly washing removes therein organic and inorganic impurity, is finally placed in 110 DEG C of baking ovens fully 12 h of drying,
It is placed in dry environment.Obtained pine needle base super capacitor active carbon material its specific surface area is 1632 m2/ g, total pore volume are
0.66 cm3/ g, the F/g of specific capacitance 214 under 0.5 A/g current density.
Embodiment 4
（1）It is prepared by presoma：Cedar needles are selected as raw material.Green fresh needles are chosen, is cleaned and cleaned repeatedly with pure water
After matter, it is placed in baking oven at 100 DEG C and dries 12 h.It is 60 mesh that obtained clean green fresh needles pulverizer, which is crushed,
Powder, be placed in stand-by in drier.
（2）Charing：Obtained pine needle powder is placed in ceramic crucible, is put into Muffle furnace, in air atmosphere, with 10
DEG C/min heating rate keeps 60 min from room temperature to final 1200 DEG C of carbonization temperature.
（3）Washing and drying：To the end of a step nature charring process, temperature is down to room temperature, by gained pine needle base porous active
Charcoal carries out pickling, and repeatedly washing removes therein organic and inorganic impurity, is finally placed in 110 DEG C of baking ovens fully 12 h of drying,
It is placed in dry environment.Obtained pine needle base super capacitor active carbon material its specific surface area is 1746 m2/ g, total pore volume are
0.61 cm3/ g, the F/g of specific capacitance 128 under 0.5 A/g current density.
Embodiment 5
（1）It is prepared by presoma：Cedar needles are selected as raw material.Selection is come off soft pin, and the removal of impurity is cleaned repeatedly with pure water
Afterwards, it is placed in baking oven at 100 DEG C and dries 12 h.Clean fall soft pin pulverizer by what is obtained and crush powdery for 60 mesh
Thing, it is placed in stand-by in drier.
（2）Charing：Obtained pine needle powder is placed in ceramic crucible, is put into Muffle furnace, in air atmosphere, with 10
DEG C/min heating rate keeps 60min from room temperature to final 1000 DEG C of carbonization temperature.
（3）Washing and drying：To the end of a step nature charring process, temperature is down to room temperature, by gained pine needle base porous active
Charcoal carries out pickling, and repeatedly washing removes therein organic and inorganic impurity, is finally placed in 110 DEG C of baking ovens fully 12 h of drying,
It is placed in dry environment.Obtained pine needle base super capacitor active carbon material its specific surface area is 482 m2/ g, total pore volume are
0.59 cm3/ g, the F/g of specific capacitance 153 under 0.5 A/g current density.
Claims (7)
1. a kind of ultracapacitor carbonizes preparation method with the step of pine needle matrix activated carbon one, it is characterised in that preparation process is：
The first step, raw material prepare：Selection comes off soft pin, is cleaned after the removal of impurity and dried repeatedly with pure water；
Second step, the preparation of presoma：The soft pin that comes off of drying is crushed to powder with pulverizer, is placed in drier and treats
With；
3rd step, charing：Pine needle powder after crushing is placed in ceramic crucible, placed into Muffle furnace, in air atmosphere, from
Room temperature is to final carbonization temperature；
4th step, washing and drying：To the end of charring process, temperature is down to room temperature, and gained pine needle Quito mesoporous activated carbon is carried out into acid
Wash and wash, remove therein organic and inorganic impurity, 110 DEG C dry again, are placed in dry environment, you can obtain super electricity
Container pine needle matrix activated carbon material.
2. a kind of ultracapacitor according to claim 1 carbonizes preparation method with the step of pine needle active charcoal one, its feature exists
In the raw material described in the first step is cedar needles, fall leaves pine needle or needles of pinus massoniana.
3. a kind of ultracapacitor according to claim 1 carbonizes preparation method with the step of pine needle active charcoal one, its feature exists
In the mesh number crushed in second step is 60-300 mesh.
4. a kind of ultracapacitor according to claim 1 carbonizes preparation method with the step of pine needle active charcoal one, its feature exists
In charing is that in air atmosphere, charing final temperature is 600-1200 DEG C, carbonization time 30-120 min in the 3rd step, heating speed
Rate is 1-10 DEG C/min.
5. a kind of ultracapacitor according to claim 1 carbonizes preparation method with the step of pine needle active charcoal one, its feature exists
In the hydrochloric acid in the 4th step first by " 1+9 " washs through row, reuses deionized water and washs 2-4 times.
6. ultracapacitor pine needle active charcoal made from any methods describeds of claim 1-5.
7. ultracapacitor pine needle active charcoal according to claim 6, it is characterised in that communicated with one another for three-dimensional network shape
Pore structure, specific surface area 500-3000 m2/ g, quality specific capacitance 100-400 F/g.
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| CN108622897A (en) * | 2018-05-24 | 2018-10-09 | 东北师范大学 | A kind of pine needle active charcoal and its preparation method and application |
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| CN115124036A (en) * | 2022-06-24 | 2022-09-30 | 闽西职业技术学院 | Preparation method of dragon fruit peel activated carbon for adsorbing phenol in wastewater |
| CN115970650A (en) * | 2023-03-20 | 2023-04-18 | 四川省冶勘设计集团生态环境工程有限公司 | Composite biochar and preparation method and application thereof |
| CN115970650B (en) * | 2023-03-20 | 2023-05-23 | 四川省冶勘设计集团生态环境工程有限公司 | Composite biochar and preparation method and application thereof |
| RU2808985C1 (en) * | 2023-03-28 | 2023-12-05 | Федеральное государственное автономное образовательное учреждение высшего образования "Пермский государственный национальный исследовательский университет" | Method for producing metal-oxide-carbon composite material |
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