CN107973286A - A kind of preparation method and application of baobab scytoblastema multiporous biological matter Carbon Materials - Google Patents

A kind of preparation method and application of baobab scytoblastema multiporous biological matter Carbon Materials Download PDF

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Publication number
CN107973286A
CN107973286A CN201711156913.2A CN201711156913A CN107973286A CN 107973286 A CN107973286 A CN 107973286A CN 201711156913 A CN201711156913 A CN 201711156913A CN 107973286 A CN107973286 A CN 107973286A
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scytoblastema
baobab
multiporous biological
carbon materials
biological matter
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吕秋丰
梁恕侠
王钧锐
马正威
王书豪
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Fuzhou University
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Fuzhou University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/34Carbon-based characterised by carbonisation or activation of carbon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/44Raw materials therefor, e.g. resins or coal
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention belongs to the preparing technical field of porous carbon material, and in particular to a kind of preparation method and applications of baobab scytoblastema multiporous biological matter Carbon Materials.First by the pretreatment of raw material of kapok pericarp, clean, drying, crush, pre- carbonizing production is obtained after normal pressure pyrolysis.Then by pre- carbonizing production acid treatment, finally by dried pre- carbonizing production, normal heating carbonizes under nitrogen protection, treats that it is down to room temperature, and with washing after salt acid soak to neutrality, drying to constant weight obtains baobab scytoblastema multiporous biological Carbon Materials.Prepared baobab scytoblastema multiporous biological matter Carbon Materials can be used for electrode material for super capacitor.The preparation method is easy to operate easily-controllable, of low cost, can in advance be carbonized, carbonized on the basis of material original structure is kept, and the multiporous biological matter charcoal prepared has different pore structures, can be as the electrode material for super capacitor of excellent performance.

Description

A kind of preparation method and application of baobab scytoblastema multiporous biological matter Carbon Materials
Technical field
The invention belongs to the preparing technical field of porous carbon material, it is related to the system of baobab scytoblastema multiporous biological matter Carbon Materials Preparation Method and application.
Background technology
Ultracapacitor generally includes four electrode, electrolyte, collector, spacer components.Wherein, electrode material is to close Key, it decides the Specifeca tion speeification of capacitor.Common electrode material have carbon-based material electrode, conductive polymer electrodes and Metal oxide electrode.The main problem that conducting polymer presently, there are is that its cycle performance is unstable, in long-term discharge and recharge Cheng Zhong, it may occur that the phenomenon of volumetric expansion or contraction, causes conducting polymer materials hydraulic performance decline.Metal oxide base capacitance In device, research at present is mainly the most successfully ruthenic oxide and aqueous sulfuric acid system.Its specific capacitance is up to 760 F g-1.But It is that Ru prices are too high, is unsuitable for being commercialized.Carbon material chemical property is stablized, and has good corrosion resistance and electrical and thermal conductivity, is The electrode material being most widely used, and the electrode material for super capacitor of only commerciallyization at present.
Biomass carbon refers to biological material such as industry, agricultural wastes, aquatic, careless and its residue, the organic work in cities and towns A kind of Carbon Materials by certain processing, chemical reaction generation such as industry waste, animals and humans excrement.This Carbon Materials have good Good chemical property, higher electric conductivity, there is universal application in terms of the energy, aerospace, electronics, mechanical industry.At present Common carbon material mainly has carbon aerosol, carbon nanotubes, porous charcoal, in carbon aerosol preparation process formaldehyde etc. can be used organic molten Agent, pollutes environment, and preparation process is cumbersome;Carbon nanotubes manufacturing cost is high, and technical requirements are high, and commercialization is difficult;Porous carbon material Prepare simply, source is wide, and cost is low, and performance is good, is adapted to large-scale production.
SOUTHERN CHINA kapok resource very abundant, every kapok fruit mature period, has a large amount of kapok fruits and falls naturally Fall.It is conceivable that can all there are a large amount of kapok pericarps to produce every year.Multiporous biological charcoal is prepared into, can not only be turned waste into wealth, And avoid the influence of waste biomass confrontation ambient air generation.Up to the present, for baobab scytoblastema multiporous biological matter The research of Carbon Materials is considerably less and is limited to study its absorption property, is not found and is made with baobab scytoblastema multiporous biological matter charcoal For the research of electrode material.By the pre- carbonization and activation to kapok pericarp, the charcoal prepared contain substantial amounts of macropore and Micropore, has higher specific surface area, has higher specific capacitance, power density using it as the electrode slice that active material is prepared And energy density.In addition, baobab scytoblastema multiporous biological charcoal contain more nitrogen element sulphur and oxygen-containing functional group, oxygen-containing functional group can To improve hydrophily of the electrode in aqueous electrolyte, be conducive to the transmission of electrolyte ion, nitrogen sulphur can improve electrode slice Specific capacitance.
The content of the invention
It is an object of the invention to provide a kind of preparation method and application of multiporous biological matter Carbon Materials, it is easy that this method possesses raw material Obtain, is easy to operate easily-controllable, and can carbonize and activate on the basis of material original structure is kept.
The present invention adopts the following technical scheme that to achieve these goals:
A kind of preparation method of baobab scytoblastema multiporous biological matter charcoal, comprises the following steps:
(1)Soaked in deionized water under room temperature first by kapok pericarp 24 it is small when after clean, drying, crush;
(2)The kapok pericarp of crushing is put into crucible in resistance furnace to be carbonized in advance(Anaerobic heats), 4 ~ 10 DEG C of heating rate min-1, when normal pressure pyrolysis 0.5 ~ 3 is small, room temperature is down to, by product with 1 mol L-1When salt acid soak 0.5 is small, then wash into Property, drying, grinding obtain pre- carbonizing production;
(3)By step 2)In pre- carbonizing production be put into graphite crucible, under nitrogen protection in 600 ~ 1000 DEG C heating charing, rise Warm 0.5 ~ 10 DEG C of min of speed-1, when soaking time 0.5 ~ 3 is small, it is down to room temperature and obtains carbonizing production, by the product with 1 mol L-1After when salt acid soak 0.5 is small, washs to neutrality, drying and obtain baobab scytoblastema multiporous biological charcoal.
Step(2)Described in pre- carbonization temperature be 300 ~ 500 DEG C.
Multiporous biological matter charcoal prepared by the above method can be used for electrode material for super capacitor.
The beneficial effects of the present invention are:
(1)The present invention raw material kapok pericarp belong to renewable biological source, derive from a wealth of sources, it is cheap be easy to get it is environmentally protective. The present invention can be carbonized on the basis of kapok pericarp structure is kept, without activation process, it is possible to prepare multiporous biological Matter Carbon Materials, realize turning waste into wealth for kapok pericarp, and the inventive method is simple for process, are adapted to large-scale production.
(2)Baobab scytoblastema multiporous biological matter charcoal prepared by the present invention can be as the super electricity of electrochemical performance Container electrode material.
Brief description of the drawings
Fig. 1 is the SEM pictures of the multiporous biological matter Carbon Materials prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM pictures of the multiporous biological matter Carbon Materials prepared by the embodiment of the present invention 2.
Fig. 3 be multiporous biological matter Carbon Materials prepared by the embodiment of the present invention 2 as electrode material in 1 A g-1Electric current Charging and discharging curve under density.
Fig. 4 is discharge and recharge of the multiporous biological matter Carbon Materials under different current densities prepared by the embodiment of the present invention 3 Curve.
Fig. 5 is that the multiporous biological matter Carbon Materials prepared by the embodiment of the present invention 4 are steady after 5000 charge and discharge cycles Qualitative curve.
Embodiment
The preparation method of baobab scytoblastema multiporous biological matter Carbon Materials of the present invention is as follows:
(1)Kapok pericarp is soaked under room temperature in deionized water 24 it is small when after clean, drying, crush, load crucible and be placed in In resistance furnace, anaerobic heats under the conditions of 300 ~ 500 DEG C, and heating rate is 4 ~ 8 DEG C of min-1;Soaking time is small for 0.5 ~ 3 When after be down to room temperature, with 1 mol L-1To neutrality, dry, grinding, obtains pre- carbonizing production for washing after when salt acid soak 0.5 is small;
(2)The pre- carbonizing production of acquisition is fitted into graphite crucible, is placed in tube furnace, under nitrogen protection in normal pressure 600 ~ 900 DEG C of heating charings, heating rate is 4 ~ 8 DEG C of min-1, when soaking time is 0.5 ~ 3 small;Treat that it is cooled to room temperature product With 1 mol L-1After when salt acid soak 0.5 is small, washs to neutrality, kapok pericarp multiporous biological matter Carbon Materials are obtained after dry;
(3)It is prepared by electrode:Using pressed disc method, selecting stainless (steel) wire, for acetylene black as conductive agent, 5 wt.%'s is poly- as collector Tetrafluoroethene is binding agent, by baobab scytoblastema multiporous biological matter Carbon Materials, acetylene black, polytetrafluoroethylene (PTFE) mass ratio 85:10: 5, mixed grinding is uniform, is pressed into thin slice, is cut into 1 cm*, 1 cm sizes;The thin slice of cutting is placed on steel mesh, is placed in Under tablet press machine, under the pressure of 10 MPa, pressurize 90s, obtains working electrode;
(4)Electrochemical property test:Tested using three-electrode system, using the electrode of sheet as working electrode, then with to electricity Pole and reference electrode are together placed in electrolyte, and test baobab scytoblastema multiporous biological matter raw material of wood-charcoal is carried out by electrochemical workstation The chemical property of material.
The purposes of the present invention is that baobab scytoblastema multiporous biological matter Carbon Materials are used as to the electrode material of ultracapacitor.
It is several specific embodiments of invention below, further illustrates the present invention, it is all according to scope of the present invention patent institute The equivalent changes and modifications done, should all belong to the covering scope of the present invention.
Embodiment 1
(1)It will be fitted into by 2 g kapok pericarp powder of pretreatment in 20 mL crucibles, be placed in resistance furnace, with 5 DEG C of min-1 Speed heating, to 300 DEG C, carry out Non-oxygen pyrolytic at this temperature, when soaking time 2 is small postcooling to room temperature, by product with 1 mol L-1Washing after drying, grinding, obtains pre- carbonizing production to neutrality after when salt acid soak 0.5 is small.
(2)The pre- carbonizing productions of 2 g are put into 20 mL graphite crucibles, are placed in resistance furnace, with 5 DEG C of min-1Speed 700 DEG C are warming up to, heating charing at this temperature under nitrogen protection, when soaking time is 2 small, fully carbonizes it under normal pressure After cool to room temperature with the furnace, with 1 mol L-1Washing obtains baobab to neutrality after drying to constant weight after when salt acid soak 0.5 is small Scytoblastema multiporous biological matter Carbon Materials.Its SEM picture by picture as shown in Figure 1, can see gained baobab scytoblastema multiporous biological Matter Carbon Materials have abundant cellular structures, its specific surface area is 1300 cm2/g。
Embodiment 2
(1)It will be fitted into by 2 g kapok pericarp powder of pretreatment in 20 mL crucibles, be placed in resistance furnace, with 4 DEG C of min-1 Speed heating, to 500 DEG C, carry out Non-oxygen pyrolytic at this temperature, when soaking time 1 is small postcooling to room temperature, by product with 1 mol L-1Washing after drying, grinding, obtains pre- carbonizing production to neutrality after when salt acid soak 0.5 is small.
(2)The pre- carbonizing productions of 3 g are put into 20 mL graphite crucibles, are placed in resistance furnace, with 4 DEG C of min-1Speed 900 DEG C are warming up to, heating charing at this temperature under nitrogen protection, when soaking time is 1 small, fully carbonizes it under normal pressure After cool to room temperature with the furnace, with 1 mol L-1Washing obtains baobab to neutrality after drying to constant weight after when salt acid soak 0.5 is small Scytoblastema multiporous biological matter Carbon Materials.Its SEM picture by picture as shown in Fig. 2, can see gained baobab scytoblastema multiporous biological Matter Carbon Materials have abundant lamella loose structure.Using the multiporous biological matter Carbon Materials as electrode material for super capacitor, 1 A g-1Charging and discharging curve under current density is as shown in Figure 3.Its electrochemical property test the result shows that, the electrode material is in 1 A g-1Specific capacitance under current density can reach 380 F g-1.In general, the electric conductivity of carbon material is poorer than metal, carbon material Specific capacitance is 100 ~ 260 F g-1, and the specific capacitance of the electrode material of the present invention can reach 380 F g-1, illustrate this material conduct Electrode material for super capacitor has excellent chemical property.
Embodiment 3
(1)It will be fitted into by 2 g kapok pericarp powder of pretreatment in 20 mL crucibles, be placed in resistance furnace, with 8 DEG C of min-1 Speed be warming up to 400 DEG C, carry out Non-oxygen pyrolytic at this temperature, postcooling is to room temperature when soaking time 0.5 is small, by product With 1 mol L-1Washing after drying, grinding, obtains pre- carbonizing production to neutrality after when salt acid soak 0.5 is small.
(2)The pre- carbonizing productions of 3 g are put into 20 mL graphite crucibles, are placed in resistance furnace, with 4 DEG C of min-1Speed 1000 DEG C are warming up to, heating charing at this temperature under nitrogen protection, when soaking time is 2 small, fully charing under normal pressure Room temperature is cooled to the furnace afterwards, with 1 mol L-1Washing obtains kapok to neutrality after drying to constant weight after when salt acid soak 0.5 is small Pericarp Quito hole biomass carbon material.Using the multiporous biological matter Carbon Materials as electrode material for super capacitor, the electrode material Charging and discharging curve under different current densities is as shown in Figure 4.Its electrochemical property test the result shows that, the electrode material is 1 A g-1Specific capacitance under current density can reach 400 F g-1, it is excellent to illustrate that this material has as electrode material for super capacitor Different chemical property.
Embodiment 4
(1)It will be fitted into by 2 g kapok pericarp powder of pretreatment in 20 mL crucibles, be placed in resistance furnace, with 10 DEG C of min-1Speed be warming up to 500 DEG C, carry out Non-oxygen pyrolytic at this temperature, postcooling is to room temperature when soaking time 0.5 is small, by product With 1 mol L-1Washing after drying, grinding, obtains pre- carbonizing production to neutrality after when salt acid soak 0.5 is small.
(2)The pre- carbonizing productions of 3 g are put into 20 mL graphite crucibles, are placed in resistance furnace, with 10 DEG C of min-1Speed 1000 DEG C are warming up to, heating charing at this temperature under nitrogen protection, when soaking time is 2 small, fully charing under normal pressure Room temperature is cooled to the furnace afterwards, with 1 mol L-1Washing obtains kapok to neutrality after drying to constant weight after when salt acid soak 0.5 is small Pericarp Quito hole biomass carbon material.Using the multiporous biological matter Carbon Materials as electrode material for super capacitor, its electrochemistry Energy test result is as shown in Figure 5.Should the result shows that, gained multiporous biological matter carbon material electrode material is through 5000 charge and discharge cycles Stability curve retention rate afterwards is 95.17%, and specific capacitance is declined by less than 5% after 5000 circulations.Therefore, the multiporous biological matter Carbon Materials have prominent cyclical stability as electrode material for super capacitor.
Embodiment 5
(1)It will be fitted into by 2 g kapok pericarp powder of pretreatment in 20 mL crucibles, be placed in resistance furnace, with 5 DEG C of min-1 Speed be warming up to 500 DEG C, carry out Non-oxygen pyrolytic at this temperature, postcooling is to room temperature when soaking time 2 is small, by product with 1 mol L-1Washing after drying, grinding, obtains pre- carbonizing production to neutrality after when salt acid soak 0.5 is small.
(2)The pre- carbonizing productions of 3 g are put into 20 mL graphite crucibles, are placed in resistance furnace, with 5 DEG C of min-1Speed 1000 DEG C are warming up to, heating charing at this temperature under nitrogen protection, when soaking time is 2 small, fully charing under normal pressure Room temperature is cooled to the furnace afterwards, with 1 mol L-1Washing obtains kapok to neutrality after drying to constant weight after when salt acid soak 0.5 is small Pericarp Quito hole biomass carbon material.Using the multiporous biological matter Carbon Materials as electrode material for super capacitor, its electrochemistry Energy test result shows that the electrode material is in 1 A g-1Specific capacitance under current density can reach 375 F g-1

Claims (5)

1. a kind of preparation method of baobab scytoblastema multiporous biological matter Carbon Materials, it is characterised in that comprise the following steps:
(1) kapok pericarp is pre-processed first:Kapok pericarp is soaked under room temperature in deionized water 24 it is small when to remove fruit The impurity in epidermis face, then cleaned repeatedly with deionized water to, drying, crush;
(2) pericarp of crushing is placed in crucible in resistance furnace and is carbonized in advance, room temperature is down to after normal pressure pyrolysis, by product With 1 mol L-1When salt acid soak 0.5 is small, then wash to neutrality, drying, grinding, obtain pre- carbonizing production;
(3) the pre- carbonizing production in step (2) is put into graphite crucible, under nitrogen protection heating charing postcooling to room temperature, By the product with 1 mol L-1After when salt acid soak 0.5 is small, washs to neutrality, baobab scytoblastema multiporous biological is obtained after dry Matter charcoal.
2. the preparation method of baobab scytoblastema multiporous biological matter Carbon Materials according to claim 1, it is characterised in that:Step (2) pre- 300 ~ 500 DEG C of carbonization temperature described in, 4 ~ 10 DEG C of min of heating rate-1, when normal pressure pyrolysis time 0.5 ~ 3 is small.
3. the preparation method of baobab scytoblastema multiporous biological matter Carbon Materials according to claim 1, it is characterised in that:Step (3) 600 ~ 1000 DEG C of the heating carbonization temperature described in, 0.5 ~ 10 DEG C of min of heating rate-1, when soaking time 0.5 ~ 3 is small.
A kind of 4. baobab scytoblastema multiporous biological matter Carbon Materials being prepared such as claim 1 ~ 3 either method.
5. a kind of application of baobab scytoblastema multiporous biological matter Carbon Materials prepared by method according to claim 1, its feature It is:Applied to electrode material for super capacitor.
CN201711156913.2A 2017-11-20 2017-11-20 A kind of preparation method and application of baobab scytoblastema multiporous biological matter Carbon Materials Pending CN107973286A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109763576A (en) * 2018-12-30 2019-05-17 张全康 Kapok aerogel thermal insulation plate
CN110753673A (en) * 2018-11-23 2020-02-04 辽宁星空钠电电池有限公司 Biomass-based functional group modified sodium ion battery negative electrode material and preparation method and application thereof
CN111244477A (en) * 2020-01-14 2020-06-05 北京理工大学 Preparation and application of biomass carbon nanosphere cluster material
CN111389382A (en) * 2020-04-03 2020-07-10 江苏省农业科学院 Preparation method and application of lanthanum-iron oxide modified nano inorganic material straw porous carbon
CN114950359A (en) * 2022-04-25 2022-08-30 山东农业工程学院 Biomass charcoal-based nano composite material and preparation method and application thereof
CN115028158A (en) * 2022-06-24 2022-09-09 张家港博威新能源材料研究所有限公司 Preparation method of kapok-based conductive carbon tube
CN115312326A (en) * 2022-04-20 2022-11-08 湖南和广生物科技有限公司 Method for preparing supercapacitor electrode material based on camellia peel

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Publication number Priority date Publication date Assignee Title
CN103787303A (en) * 2014-01-24 2014-05-14 同济大学 Natural biomass in-situ transformation preparation method of porous carbon in graded mesh structure
CN107098327A (en) * 2017-04-24 2017-08-29 福州大学 The preparation method and application of biomass porous carbon plate based on bombax cotton

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103787303A (en) * 2014-01-24 2014-05-14 同济大学 Natural biomass in-situ transformation preparation method of porous carbon in graded mesh structure
CN107098327A (en) * 2017-04-24 2017-08-29 福州大学 The preparation method and application of biomass porous carbon plate based on bombax cotton

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110753673A (en) * 2018-11-23 2020-02-04 辽宁星空钠电电池有限公司 Biomass-based functional group modified sodium ion battery negative electrode material and preparation method and application thereof
WO2020103138A1 (en) * 2018-11-23 2020-05-28 辽宁星空钠电电池有限公司 Biomass-based functional-group-modified sodium-ion battery anode material, preparing method therefor and use thereof
CN109763576A (en) * 2018-12-30 2019-05-17 张全康 Kapok aerogel thermal insulation plate
CN111244477A (en) * 2020-01-14 2020-06-05 北京理工大学 Preparation and application of biomass carbon nanosphere cluster material
CN111389382A (en) * 2020-04-03 2020-07-10 江苏省农业科学院 Preparation method and application of lanthanum-iron oxide modified nano inorganic material straw porous carbon
CN111389382B (en) * 2020-04-03 2023-02-14 江苏省农业科学院 Preparation method and application of lanthanum-iron oxide modified nano inorganic material straw porous carbon
CN115312326A (en) * 2022-04-20 2022-11-08 湖南和广生物科技有限公司 Method for preparing supercapacitor electrode material based on camellia peel
CN114950359A (en) * 2022-04-25 2022-08-30 山东农业工程学院 Biomass charcoal-based nano composite material and preparation method and application thereof
CN115028158A (en) * 2022-06-24 2022-09-09 张家港博威新能源材料研究所有限公司 Preparation method of kapok-based conductive carbon tube

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