CN106044953A - Preparation method of nitrogen-doped porous carbon rod capacitance desalting electrode - Google Patents
Preparation method of nitrogen-doped porous carbon rod capacitance desalting electrode Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/4604—Treatment of water, waste water, or sewage by electrochemical methods for desalination of seawater or brackish water
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a preparation method of a nitrogen-doped porous carbon rod capacitance desalting electrode and belongs to the field of capacitance desalting electrode preparation. According to the preparation method, firstly, a metal organic frame MIL-88-NH2 is synthesized through a hydrothermal reaction, and washing, drying, high temperature annealing and etching with acid liquor are conducted to obtain highly-graphitized nitrogen-doped porous carbon which is in a fusiform rod shape and has a wide pore diameter; the prepared nitrogen-doped porous carbon rod, acetylene black and polyvinyl alcohol are mixed to be uniform, graphite paper is coated with the mixture, drying is conducted, and the capacitance desalting electrode is obtained. The preparation method has the advantages that the metal organic frame is used for preparing the highly-graphitized nitrogen-doped porous carbon material which is of a fusiform rod structure and has the wide pore diameter for a precursor; the specific surface area, the degree of graphitization and the nitrogen doping content of the prepared fusiform porous carbon rod can be controlled by controlling temperature; the preparation process is simple and easy to conduct, conditions are mild, and the preparation method can be used for large-scale production.
Description
Technical field
The present invention relates to capacitive desalination electrode fabrication techniques field, be specifically related to a kind of wide aperture footpath, the nitrogen of high graphitization is mixed
The preparation method of miscellaneous porous carbon-point capacitive desalination electrode.Prepared desalination electrode have high efficiency, two-forty, low energy consumption de-
Salt performance, it is adaptable to high salt concentration water desalination processes, and sea water and brackish water desalination, for high efficiency, low energy consumption, low cost desalination skill
Art provides new approach.
Background technology
Capacitive desalination technology, i.e. capacitive deionization technology, also known as electro-adsorption, it has the high and low energy consumption of desalting efficiency, environment
The advantage such as friendly, be recent decades along with material with carbon element the reach of science the widest valued novel sea water desalinization technology.Enter
Entering 21st century, along with world population and the quick growth of global industry process, shortage of fresh water problem is the most prominent
Go out, want water the most very urgent to sea.Traditional desalination technology, as reverse osmosis, electrodialysis and ion exchange, due to it
The problem such as high energy consumption that body is very important and poor efficiency, can not meet the requirement of mankind's intensive style social development.Electric capacity takes off
The appearance of salt technology compensate for the defect of tradition desalination technology, makes low energy consumption, high efficiency desalting technology have reality
Probability.Therefore, the rationale of capacitive desalination technology based on Novel carbon electrode and actual application are carried out energetically in a deep going way
Research, the most important scientific value, it is often more important that have foreseeable broad prospect of application in human social development
And realistic meaning.
In general, capacitive desalination technology mainly utilizes surface electric double layer to carry out capacitive adsorption and removes charged ion in water,
The porous carbon materials therefore with higher specific surface area and good electric conductivity becomes a kind of preferably capacitive desalination electrode
Material.But the capacitive desalination carbon electrode material reported at present such as activated carbon, carbon aerogels, mesoporous carbon, CNT and stone
The desalination amount of ink alkene etc. is relatively low, greatly limit the application of capacitive desalination technology.Development has the New Type of Carbon of high desalination amount
Material is the key solving the problems referred to above.
In recent years, the research being templated synthesis porous carbon materials with metal organic frame is worldwide subject to application
Extensive concern.But derive the porous carbon materials applied research in capacitive desalination field based on metal organic frame
(Chem.Commun., 2015,51,12020-12023) is still in the starting stage.And synthesized by metal organic frame derivatization method
Porous carbon materials pore-size distribution narrow (mostly being micropore), degree of graphitization ratio is relatively low, is unfavorable for the electronics during electro-adsorption
And the transfer of ion.Utilize that metal organic frame synthesis a kind of has wide aperture footpath, the porous carbon materials of high graphitization has become as
An important study hotspot and development trend in capacitive desalination field.ChemElectroChem,2016,DOI:
10.1002/celc.201600051 report a kind of wide aperture footpath, the porous carbon of high graphitization, and it is applied to capacitive desalination
Field.Although achieving reasonable effect, but still cannot meet the demand of actual application.In order to improve synthesized wide aperture
Footpath, the desalination amount of porous carbon of high graphitization, a kind of method of improvement is that synthesized porous carbon materials is carried out N doping.So
And later stage N doping processes and adds synthesis cost, extend synthesis cycle, be unfavorable for large-scale production.Therefore, utilize nitrogenous
Metal organic frame synthesis wide aperture footpath, the N doping porous carbon of high graphitization be the effective way solving this problem.
Summary of the invention
It is an object of the invention to for the problems referred to above, propose a kind of there is the wide aperture footpath of fusiformis club shaped structure, high graphitization
The preparation method of nitrogen-doped porous carbon material, and be applied to capacitive desalination field.
The object of the present invention is achieved like this:
A kind of wide aperture footpath, the preparation method of N doping fusiformis porous carbon-point capacitive desalination electrode of high graphitization, the method
Including step in detail below；
Step 1: the preparation of electrode material
2-amino p-phthalic acid and ferric chloride hexahydrate are dissolved in deionized water, vigorous mechanical agitation mix homogeneously,
Obtain iron chloride and 2-amino p-phthalic acid mixed solution；Gained iron chloride is turned with 2-amino p-phthalic acid mixed solution
Move on to water heating kettle reacts；The sample obtained is centrifuged, and is dried, obtains metal organic frame MIL-88-MH2；By gained
MIL-88-NH2It is placed in tube furnace, under an inert atmosphere carbonization；Gained carbonized product is placed in hydrochloric acid solution reaction removing contain
Ferrum component, fully washing are dried, i.e. obtain the N doping fusiformis i.e. electrode material of porous carbon bar material；Wherein:
The mol ratio of 2-amino p-phthalic acid, ferric chloride hexahydrate and deionized water is 1:0.5-2:50-100；Acutely
Mechanical agitation speed is 400-8000rpm/min, and mixing time is 5-10min；Hydrothermal temperature, at 60～150 DEG C, reacts
Time is 6-12h；Carbonisation under an inert atmosphere: heating rate is 2-5 DEG C/min, holding temperature is 700-900 DEG C, insulation
Time is 2-4h；The concentration of hydrochloric acid solution is 1-5M；
Step 2: the preparation of capacitive desalination electrode
N doping fusiformis porous carbon bar material step (1) prepared, acetylene black and polyvinyl alcohol water solution are according to quality
It is uniformly coated on graphite paper than after stirring for 80:10:10, dries 6-12h at 80-100 DEG C subsequently, obtain described N doping many
Hole carbon-point capacitive desalination electrode.
Wide aperture footpath, the porous carbon materials of high graphitization that the present invention prepares have unique fusiformis club shaped structure, bigger
Specific surface area, good conductivity, high N doping content and the pore structure of level.
It is an advantage of the current invention that:
(1) metal organic frame is utilized to be prepared for a kind of having the wide aperture footpath of fusiformis club shaped structure, high graphite for presoma
The nitrogen-doped porous carbon material changed；
(2) method provided by the present invention, specific surface area, degree of graphitization and the nitrogen of the fusiformis porous carbon-point of preparation
Doping content can be controlled by regulating and controlling temperature；
(3) preparation method provided by the present invention is simple for process, and mild condition can be used for large-scale production.
Accompanying drawing explanation
Fig. 1 is the scanning of the N doping fusiformis porous carbon-point that carburizing temperature is obtained when being 700 DEG C in the embodiment of the present invention 1
Electromicroscopic photograph figure；
Fig. 2 is the scanning of the N doping fusiformis porous carbon-point that carburizing temperature is obtained when being 800 DEG C in the embodiment of the present invention 2
Electromicroscopic photograph figure；
Fig. 3 is the scanning of the N doping fusiformis porous carbon-point that carburizing temperature is obtained when being 900 DEG C in the embodiment of the present invention 3
Electromicroscopic photograph figure；
Fig. 4 is the nitrogen adsorption desorption figure of the embodiment of the present invention 1,2 and 3 gained sample；
Fig. 5 is the graph of pore diameter distribution of the embodiment of the present invention 1,2 and 3 gained sample；
Fig. 6 is the X-ray powder diffraction figure of the embodiment of the present invention 1,2 and 3 gained sample；
Fig. 7 is the photoelectron spectroscopy figure of the embodiment of the present invention 1,2 and 3 gained sample；
Fig. 8 is the electro-adsorption desalination figure of the embodiment of the present invention 1,2 and 3 gained sample.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further elaborated.Should be understood that these embodiments are only used for
The bright present invention rather than be used for limiting the scope of the present invention.Additionally, after having read present disclosure, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application institute appended claims equally and limit
Scope.
Embodiment 1
1) prepared by capacitive desalination electrode
At normal temperatures the ferric chloride hexahydrate of the 2-amino p-phthalic acid of 0.5mol Yu 0.5mol is dissolved in 50ml go from
Stirring 10 minutes after sub-water, be transferred in the water heating kettle of 100mL, in thermostatic drying chamber, 100 DEG C are heated 6 hours.The sample obtained
Product eccentric cleaning is dried, and i.e. obtains MIL-88-NH2；By obtained MIL-88-NH2It is placed in tube furnace, under nitrogen atmosphere, heats up
Speed is that 2 DEG C/min is warming up at 700 DEG C insulation 2 hours.Obtained carbonized product 5M hydrochloric acid is performed etching process, washes
Wash dry, i.e. obtain N doping fusiformis porous carbon-point (named NCRs-700), see Fig. 1.Utilizing nitrogen adsorption to be desorbed, X penetrates
Synthesized porous carbon-point is analyzed by line diffraction and photoelectron spectroscopy, it was demonstrated that it has wide aperture footpath, high graphitization, high nitrogen doped
The feature of content, sees table 1, Fig. 4, Fig. 5, Fig. 6 and Fig. 7.
By obtained N doping fusiformis porous carbon bar material, acetylene black and polyvinyl alcohol water solution according to mass ratio are
80:10:10 is uniformly coated on graphite paper after stirring, and dries 6-12h at 80-100 DEG C subsequently, i.e. obtains capacitive desalination electricity
Pole.
2) desalting performance test
The electrode prepared is carried out device assembling, carries out desalination test.Test brine strength is 500mg/ml, applies electricity
Pressure is DC voltage 1.2V, and adsorption time is 40min.Desalination processes concentration change is detected in real time by conductivity meter, logical
The change crossing solution concentration can calculate salt rejection rate under this concentration.Experimental result is shown in Fig. 8.
Embodiment 2
1) prepared by capacitive desalination electrode
At normal temperatures the ferric chloride hexahydrate of the 2-amino p-phthalic acid of 0.5mol Yu 0.5mol is dissolved in 50ml go from
Stirring 10 minutes after sub-water, be transferred in the water heating kettle of 100mL, in thermostatic drying chamber, 100 DEG C are heated 6 hours.The sample obtained
Product eccentric cleaning is dried, and i.e. obtains MIL-88-NH2；By obtained MIL-88-NH2It is placed in tube furnace, under nitrogen atmosphere, heats up
Speed is that 2 DEG C/min is warming up at 800 DEG C insulation 2 hours.Obtained carbonized product 5M hydrochloric acid is performed etching process, washes
Wash dry, i.e. obtain N doping fusiformis porous carbon-point (named NCRs-800), see Fig. 2.Utilizing nitrogen adsorption to be desorbed, X penetrates
Synthesized porous carbon-point is analyzed by line diffraction and photoelectron spectroscopy, it was demonstrated that it has wide aperture footpath, high graphitization, high nitrogen doped
The feature of content, sees table 1, Fig. 4, Fig. 5, Fig. 6 and Fig. 7.
By obtained N doping fusiformis porous carbon bar material, acetylene black and polyvinyl alcohol water solution according to mass ratio are
80:10:10 is uniformly coated on graphite paper after stirring, and dries 6-12h at 80-100 DEG C subsequently, i.e. obtains capacitive desalination electricity
Pole.
2) desalting performance test
The electrode prepared is carried out device assembling, carries out desalination test.Test brine strength is 500mg/mL, applies electricity
Pressure is DC voltage 1.2V, and adsorption time is 40min.Desalination processes concentration change is detected in real time by conductivity meter, logical
The change crossing solution concentration can calculate salt rejection rate under this concentration.Experimental result is shown in Fig. 8.
Embodiment 3
1) prepared by capacitive desalination electrode
At normal temperatures the ferric chloride hexahydrate of the 2-amino p-phthalic acid of 0.5mol Yu 0.5mol is dissolved in 50ml go from
Stirring 10 minutes after sub-water, be transferred in the water heating kettle of 100mL, in thermostatic drying chamber, 100 DEG C are heated 6 hours.The sample obtained
Product eccentric cleaning is dried, and i.e. obtains MIL-88-NH2；By obtained MIL-88-NH2It is placed in tube furnace, under nitrogen atmosphere, heats up
Speed is that 2 DEG C/min is warming up at 900 DEG C insulation 2 hours.Obtained carbonized product 5M hydrochloric acid is performed etching process, washes
Wash dry, i.e. obtain N doping fusiformis porous carbon-point (named NCRs-900), see Fig. 3.Utilizing nitrogen adsorption to be desorbed, X penetrates
Synthesized porous carbon-point is analyzed by line diffraction and photoelectron spectroscopy, it was demonstrated that it has wide aperture footpath, high graphitization, high nitrogen doped
The feature of content, sees table 1, Fig. 4, Fig. 5, Fig. 6 and Fig. 7.
By obtained N doping fusiformis porous carbon bar material, acetylene black and polyvinyl alcohol water solution according to mass ratio are
80:10:10 is uniformly coated on graphite paper after stirring, and dries 6-12h at 80-100 DEG C subsequently, i.e. obtains capacitive desalination electricity
Pole.
2) desalting performance test
The electrode prepared is carried out device assembling, carries out desalination test.Test brine strength is 500mg/ml, applies electricity
Pressure is DC voltage 1.2V, and adsorption time is 40min.Desalination processes concentration change is detected in real time by conductivity meter, logical
The change crossing solution concentration can calculate salt rejection rate under this concentration.Experimental result is shown in Fig. 8.
The preparation of table 1 embodiment of the present invention different total specific surface area of N doping fusiformis porous carbon-point, total pore volume, micropore ratio
Surface area and N doping content.
Note: total specific surface area, total pore volume and micropore specific area are by using BELSORP-MAX nitrogen adsorption device
Measure (Japan Instrumentation System Co., Ltd) to measure.N doping content passes through X-ray photoelectron
Power spectrum test obtains.
Claims (1)
1. the preparation method of a N doping porous carbon-point capacitive desalination electrode, it is characterised in that comprise the steps of
Step 1: the preparation of electrode material
2-amino p-phthalic acid and ferric chloride hexahydrate are dissolved in deionized water, vigorous mechanical agitation mix homogeneously, obtain
Iron chloride and 2-amino p-phthalic acid mixed solution；Gained iron chloride is transferred to 2-amino p-phthalic acid mixed solution
Water heating kettle reacts；The sample obtained is centrifuged, and is dried, obtains metal organic frame MIL-88-MH2；By the MIL-of gained
88-NH2It is placed in tube furnace, under an inert atmosphere carbonization；Gained carbonized product is placed in hydrochloric acid solution reaction and removes iron content group
Point, fully washing is dried, i.e. obtains the N doping fusiformis i.e. electrode material of porous carbon bar material；Wherein:
The mol ratio of 2-amino p-phthalic acid, ferric chloride hexahydrate and deionized water is 1:0.5-2:50-100；Vigorous
Stir speed (S.S.) is 400-8000rpm/min, and mixing time is 5-10min；Hydrothermal temperature at 60 ~ 150 DEG C, the response time
For 6-12h；Carbonisation under an inert atmosphere: heating rate is 2-5 DEG C/min, holding temperature is 700-900 DEG C, temperature retention time
For 2-4h；The concentration of hydrochloric acid solution is 1-5M；
Step 2: the preparation of capacitive desalination electrode
N doping fusiformis porous carbon bar material step (1) prepared, acetylene black and polyvinyl alcohol water solution according to mass ratio are
It is uniformly coated on graphite paper after 80:10:10 stirring, dries 6-12h at 80-100 DEG C subsequently, obtain described N doping porous carbon
Rod capacitive desalination electrode.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957441A (en) * | 2017-05-26 | 2017-07-18 | 中南大学 | A kind of solvent structure carbonization MOFs method |
| CN107555553A (en) * | 2017-08-04 | 2018-01-09 | 天津大学 | A kind of preparation method of nitrogen-doped carbon nanometer pipe film for capacitive deionization |
| CN108928816A (en) * | 2018-07-23 | 2018-12-04 | 燕山大学 | A kind of N doping graphitized carbon microballoon and its preparation method and application with ultra-microporous |
| CN110451615A (en) * | 2019-07-31 | 2019-11-15 | 河海大学 | A kind of preparation method of metal-organic framework carbon nano-tube hybridization desalination electrode |
| CN110614041A (en) * | 2019-08-29 | 2019-12-27 | 浙江工业大学 | Hollow MOF-loaded graphene oxide composite membrane and preparation method and application thereof |
| CN111392712A (en) * | 2020-04-13 | 2020-07-10 | 湘潭大学 | Nitrogen modified mesoporous carbon material, preparation method thereof and application of nitrogen modified mesoporous carbon material as electro-adsorption desalination electrode material |
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| CN112811537A (en) * | 2021-02-07 | 2021-05-18 | 河海大学 | Preparation method and application of iron-nitrogen doped carbon nanotube electrode |
| CN113113618A (en) * | 2021-03-26 | 2021-07-13 | 西北工业大学 | Preparation method of cobalt-based nitrogen-doped MOF (metal organic framework) derived porous carbon material |
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| CN106957441A (en) * | 2017-05-26 | 2017-07-18 | 中南大学 | A kind of solvent structure carbonization MOFs method |
| CN106957441B (en) * | 2017-05-26 | 2020-02-14 | 中南大学 | Method for synthesizing carbonized MOFs (metal-organic frameworks) by solvothermal method |
| CN107555553A (en) * | 2017-08-04 | 2018-01-09 | 天津大学 | A kind of preparation method of nitrogen-doped carbon nanometer pipe film for capacitive deionization |
| CN108928816A (en) * | 2018-07-23 | 2018-12-04 | 燕山大学 | A kind of N doping graphitized carbon microballoon and its preparation method and application with ultra-microporous |
| CN108928816B (en) * | 2018-07-23 | 2020-04-17 | 燕山大学 | Nitrogen-doped graphitized carbon microsphere with ultramicropore structure and preparation method and application thereof |
| CN110451615A (en) * | 2019-07-31 | 2019-11-15 | 河海大学 | A kind of preparation method of metal-organic framework carbon nano-tube hybridization desalination electrode |
| CN110614041A (en) * | 2019-08-29 | 2019-12-27 | 浙江工业大学 | Hollow MOF-loaded graphene oxide composite membrane and preparation method and application thereof |
| CN111392712A (en) * | 2020-04-13 | 2020-07-10 | 湘潭大学 | Nitrogen modified mesoporous carbon material, preparation method thereof and application of nitrogen modified mesoporous carbon material as electro-adsorption desalination electrode material |
| CN111689624A (en) * | 2020-05-11 | 2020-09-22 | 中南大学 | Application method of carbon-based metal vanadium monoatomic material in ammonia nitrogen wastewater treatment |
| CN112811537A (en) * | 2021-02-07 | 2021-05-18 | 河海大学 | Preparation method and application of iron-nitrogen doped carbon nanotube electrode |
| CN112811537B (en) * | 2021-02-07 | 2022-02-01 | 河海大学 | Preparation method and application of iron-nitrogen doped carbon nanotube electrode |
| CN113113618A (en) * | 2021-03-26 | 2021-07-13 | 西北工业大学 | Preparation method of cobalt-based nitrogen-doped MOF (metal organic framework) derived porous carbon material |
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