CN108163833A - A kind of method for preparing the mesoporous carbon nanomaterial of sulfur doping class graphene - Google Patents
A kind of method for preparing the mesoporous carbon nanomaterial of sulfur doping class graphene Download PDFInfo
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- CN108163833A CN108163833A CN201810053530.0A CN201810053530A CN108163833A CN 108163833 A CN108163833 A CN 108163833A CN 201810053530 A CN201810053530 A CN 201810053530A CN 108163833 A CN108163833 A CN 108163833A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 24
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 17
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 12
- 239000011593 sulfur Substances 0.000 title claims abstract description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 11
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 230000005587 bubbling Effects 0.000 claims abstract description 5
- 238000006722 reduction reaction Methods 0.000 claims abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000003575 carbonaceous material Substances 0.000 abstract description 7
- 239000007789 gas Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- QENHCSSJTJWZAL-UHFFFAOYSA-N magnesium sulfide Chemical compound [Mg+2].[S-2] QENHCSSJTJWZAL-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005554 pickling Methods 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 abstract 1
- 238000012983 electrochemical energy storage Methods 0.000 abstract 1
- 238000004108 freeze drying Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000007704 wet chemistry method Methods 0.000 description 2
- PNHZSBZGAMNFLT-UHFFFAOYSA-N C(=S)=S.[Ar] Chemical compound C(=S)=S.[Ar] PNHZSBZGAMNFLT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003738 black carbon Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- Y02E60/10—Energy storage using batteries
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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
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- Inorganic Chemistry (AREA)
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Abstract
This technology invents the preparation for being related to the mesoporous carbon nanomaterial of sulfur doping.Porous carbon nanomaterial has very high application value in fields such as ultracapacitor, negative electrode of lithium ion battery, catalysis, absorption.The present invention obtains mesoporous class graphene-structured carbon nanomaterial using the thermal reduction reaction of magnesium powder and carbon disulfide gas, can realize prepared by the big yield of high quality class graphene carbon material.By liquid carbon disulphide bubbling argon, volatilization steam is brought into reaction cavity, is reacted in 550 650 DEG C of temperature ranges with magnesium powder, obtain the mixture of carbon nanomaterial and magnesium sulfide.Product is washed successively and pickling, the class graphene carbon nano material of loose lightweight, the element percentage about 6% of sulfur doping are obtained after freeze-drying.Carbon nanomaterial is prepared by consuming the method for magnesium powder reduction carbon disulfide, the advantage with cost low yield height, and also the sulfur doping introduced is conducive to application of the material in terms of electrochemical energy storage electrode.
Description
Technical field
The invention belongs to functional carbon field of nanometer material technology, to the effect that a kind of skill for preparing class graphene carbon nano material
Art.By using magnesium powder and the pyroreaction of carbon disulfide steam, carbon and magnesium sulfide mix products are generated.By pickling processes
Afterwards, the mesoporous carbon nanomaterial of sulfur doping is obtained.This method is simple for process, at low cost.Product applications include ion battery
Cathode, ultracapacitor, solar energy optical-thermal water evaporation etc..
Background technology
Carbon be present in nature with the mankind are most closely related, one of most important element, it have SP, SP2,
The multiple electronic orbital characteristics of SP3 hydridization, the anisotropy of SP2 in addition cause each guide property of crystal and each of other arrangements to
The property led.Therefore the carbon materials using carbon as unique constitution element have miscellaneous property, and new carbon is harmonious newly
Carbon materials are also constantly found and are manually made.Mesoporous carbon is a kind of novel non-silicon-based mesoporous material, 2nm<Aperture<
50nm has huge specific surface area and pore volume, is expected to very much in catalyst carrier, hydrogen storage material, electrode material etc.
Important application is obtained, therefore is paid much attention to by people.
Compared with pure mesoporous silicon material, meso-porous carbon material shows special property, there is high specific surface area, high hole
Rate；Aperture size is adjustable in a certain range；Mesoporous various shapes, hole wall composition, structure and property are adjustable；Pass through optimum synthesis
Condition can obtain high thermal stability and hydrothermal stability；Synthesize simple, easy to operate, physiological-toxicity-free.Its tempting part is also
It is its potential using value in fields such as fuel cell, molecular sieve, absorption, catalysis reaction, electrochemistry.In recent years, it is mesoporous
Material science has become in the world across one of hot research field of the subject crossings such as chemistry, physics, material, biology, more into
An important milestone for material science development.
Graphene is a kind of cellular two-dimensional nano material of the individual layer atom formed in a manner of sp2 hydridization by carbon atom
Material has excellent physical and chemical properties.It was found in 2004, was initially to remove high quality graphite by using adhesive tape
Method obtains single-layer graphene.Since graphene has big specific surface area 2630m2/ g, high electron mobility 15 at room temperature,
000m2/V/s.The preparation method of graphene is broadly divided into two classes：Wet chemistry method and gas-phase reaction method.Chemical vapour deposition technique system
Standby graphene low yield and severe reaction conditions, need vacuum environment.And Hummer ' the s methods in wet chemistry method, i.e., by stone
Ink powder carries out oxidation stripping, and then the graphene oxide of monoatomic layer is restored, and has the advantage for being easy to preparation of industrialization.
But preparation process is cumbersome, and needs a large amount of chemical reagent, has no cost advantage.Graphene oxide price currently on the market
About 550 yuan/gram, expensive price are the major obstacles towards industrial applications.
Invention content
This technology invention is for the first time by magnesium powder (Mg) and carbon disulfide (CS2) steam reacts under the conditions of low-voltage high-temperature, finally
It is prepared for the mesoporous class graphene carbon nano material of three-dimensional structure of sulfur doping.The advantage that this technology protrudes is yield to give birth to greatly
Production, and preliminary test finds the carbon material product in the application aspects such as solar seawater desalination, negative electrode of lithium ion battery all tables
Reveal excellent properties.
Chemical raw material used in the present invention is cheap and common, and preparation process can further upgrade to meet large-scale production need
It asks.
This technology invention is mixed using magnesium powder with sodium chloride powder, and the carbon disulfide brought into vacuum tube furnace with argon gas steams
Vapour reacts, and generates magnesium sulfide and carbon, 2Mg+CS2→2MgS+C.The effect of sodium chloride is to make magnesium powder reaction thorough, improve carbon
The yield of nano material.The front and rear picture of mixture reaction is as shown in Figure 1.Mixture is purified by washing and acid pickling step
To loose carbon nanomaterial, electron microscope picture is as shown in Figure 2.Carbon disulfide is volatile liquid at normal temperatures and pressures
Body.We are brought carbon disulfide steam in vacuum tube furnace into bubbling argon method.Magnesium occurs in 550-650 DEG C of temperature range
Thermal reduction reaction.
Preparation process specifically includes following steps：
(1) by magnesium powder and NaCl powder according to 1：4 mass ratio mixing, is loaded in ceramic boat, is put into the tubular type of single temperature zone
Among stove.Tube furnace with mechanical pump is evacuated, then passes to argon gas.
(2) container for filling liquid carbon disulphide is placed in water-bath, keeps the temperature 35 DEG C.It, will with bubbling argon carbon disulfide
Reaction gas is brought into stove, while is warming up to 600 DEG C, is kept for 90 minutes.Aspiration pump is evacuated in reaction process, maintains air pressure in stove
About 1/50 standard atmospheric pressure.
(3) after reaction, black product is completely dissolved in deionized water, filters removal foreign ion twice.Filter
Black carbon product on film is dispersed in water again, is added in hydrochloric acid and is fully reacted, then filters, in redisperse to deionized water.
The carbon material being dispersed in water is freeze-dried after cleaning repeatedly.
The present invention prepares mesoporous carbon nanomaterial using magnesiothermic reduction carbon disulfide method, this technical solution major advantage exists
In：
(1) high temperature solid-gas reaction method will not introduce any oxygen-containing group, moreover it is possible to realize the sulfur doping of carbon nanomaterial.
(2) yield is high, is easily enlarged metaplasia production.With small size vacuum stove, the functional carbon material of the available gram rank of single reaction
Material.If improving size of burner hearth, the ceramic boat of packing of multiple-level stack is designed so as to can also while powder weight is increased
Holding comes into full contact with gas, then can further improve the yield of single experiment.
(3) reaction time is short.
(4) it is easy to purify, the removal of by-product magnesium chloride usable acid.
(5) easy to operate, controllability is strong.
Description of the drawings
Attached drawing 1 (a) produces the schematic device of carbon nanomaterial；(b) photo of carbon nanomaterial.
2 product photo of attached drawing.(a) before reacting, the magnesium powder and the mixture of sodium chloride that are loaded in corundum boat.(b) after reacting,
The photo of mixture.
The scanning electron microscope analysis figure of 3 sample of attached drawing.
Specific embodiment
The present invention is further elaborated, but the invention is not limited in specific embodiments below in conjunction with example.
1) 8 grams of magnesium powders and 42 grams of NaCl powder are weighed, are mixed in plastic test tube with oscillator, are subsequently poured into two large scales
Corundum boat in.
2) two ceramic boats equipped with reactant are put into boiler tube, are evacuated with oil-sealed rotary pump, then pour into argon gas, instead
It answers twice to eliminate oxygen.
3) argon gas is passed through in liquid carbon disulphide container, with the flow velocity of 200mL/min, by liquid bubbling, Ar and CS2's
Gaseous mixture is passed through in tube furnace.Stove is warming up to 600 DEG C with 15 DEG C of rates simultaneously, keeps the temperature 90 minutes.Tubular type in reaction process
Stove is evacuated with vacuum pump.
4) after reacting, after stove Temperature fall to room temperature, ceramic boat is taken out, is immersed in aqueous solution to dissolve sodium chloride.
5) the aqueous filter membrane of 0.2 μm of micropore of solution is filtered.In the black object re-ultrasonic dispersion to deionized water of collection,
Then excessive hydrochloric acid is added in.Fully dark solution is filtered again after reaction, the black object on filter membrane is distributed in deionized water.
It filters again, then being distributed to product in a small amount of deionized water, is freeze-dried, obtains the fluffy carbon nanomaterial of black.
Claims (4)
- A kind of 1. method for preparing the mesoporous carbon nanomaterial of sulfur doping class graphene, it is characterised in that the design and system of consersion unit Preparation Method and step.1) raw material are magnesium powder and liquid carbon disulphide, reaction equation 2Mg+CS2→2MgS2+C.We use two sulphur of bubbling argon Change carbon liquid body, be passed through progress high temperature reaction in vacuum drying oven.2) in order to which magnesium powder is enable to react thorough, magnesium powder and sodium chloride powder are uniformly mixed according to certain mass ratio.3) reduction reaction of magnesium and carbon disulfide can all occur for 550-650 DEG C of range.4) product obtained by the reaction is submerged into the aqueous solution of dilute hydrochloric acid, removes sulphide removal and remaining a small amount of magnesium granules.5) aqueous solution containing carbon nanomaterial is filtered, be scattered in deionized water, then filter, remove foreign ion.Filter membrane On black product can be freeze-dried.
- 2. a kind of method for preparing the mesoporous carbon nanomaterial of sulfur doping class graphene according to claim 1, feature exist In raw material described in step (1) and the experimental facilities for chemically reacting design thus.
- 3. a kind of method for preparing the mesoporous carbon nanomaterial of sulfur doping class graphene according to claim 1, feature exist In mixing magnesium powder with sodium chloride powder described in step (2) and the temperature range described in step (3).
- 4. a kind of method for preparing the mesoporous carbon nanomaterial of sulfur doping class graphene according to claim 1, feature exist In the method for the purification graphene described in step (4) and (5).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110098068A (en) * | 2019-04-03 | 2019-08-06 | 中南大学 | A kind of preparation method of ternary nickel cobalt manganese sulfide fake capacitance super capacitor material |
| CN110289383A (en) * | 2019-06-18 | 2019-09-27 | 深圳昌茂粘胶新材料有限公司 | A kind of lithium battery power battery high-temperature resistant micropore thin film material and preparation method thereof |
| CN113430533A (en) * | 2021-06-23 | 2021-09-24 | 景德镇陶瓷大学 | Nickel-cobalt-iron trimetal catalyst for in-situ growth of graphene through phosphorization and sulfuration and preparation method thereof |
| CN113502502A (en) * | 2021-06-23 | 2021-10-15 | 景德镇陶瓷大学 | Sulfur-doped graphene-coated nickel-cobalt bimetallic catalyst and preparation method thereof |
| CN113529127A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Tungsten metal catalyst for in-situ growth of sulfur and graphene and preparation method thereof |
| CN113522318A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution and preparation method thereof |
| CN113529100A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Graphene-coated vulcanized nickel-cobalt-iron trimetal catalyst and preparation method thereof |
| CN113529128A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Sulfur-phosphorus co-doped in-situ growth graphene coated nickel-cobalt-iron hydrogen evolution catalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293468A (en) * | 2015-11-04 | 2016-02-03 | 上海应用技术学院 | Method for efficiently preparing sulphur-doped hollow carbon spheres |
| CN106241792A (en) * | 2016-08-30 | 2016-12-21 | 北京航空航天大学 | Magnesiothermic reduction carbon tetrachloride method prepares Graphene |
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| CN110098068B (en) * | 2019-04-03 | 2021-06-15 | 中南大学 | Preparation method of ternary nickel-cobalt-manganese sulfide pseudocapacitance supercapacitor material |
| CN110289383A (en) * | 2019-06-18 | 2019-09-27 | 深圳昌茂粘胶新材料有限公司 | A kind of lithium battery power battery high-temperature resistant micropore thin film material and preparation method thereof |
| CN110289383B (en) * | 2019-06-18 | 2021-12-03 | 深圳昌茂粘胶新材料有限公司 | High-temperature-resistant microporous film material for power battery of lithium battery and preparation method of microporous film material |
| CN113430533A (en) * | 2021-06-23 | 2021-09-24 | 景德镇陶瓷大学 | Nickel-cobalt-iron trimetal catalyst for in-situ growth of graphene through phosphorization and sulfuration and preparation method thereof |
| CN113502502A (en) * | 2021-06-23 | 2021-10-15 | 景德镇陶瓷大学 | Sulfur-doped graphene-coated nickel-cobalt bimetallic catalyst and preparation method thereof |
| CN113529127A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Tungsten metal catalyst for in-situ growth of sulfur and graphene and preparation method thereof |
| CN113522318A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Difunctional tungsten-cobalt bimetallic electrolytic water catalyst for hydrogen evolution and oxygen evolution and preparation method thereof |
| CN113529100A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Graphene-coated vulcanized nickel-cobalt-iron trimetal catalyst and preparation method thereof |
| CN113529128A (en) * | 2021-06-23 | 2021-10-22 | 景德镇陶瓷大学 | Sulfur-phosphorus co-doped in-situ growth graphene coated nickel-cobalt-iron hydrogen evolution catalyst and preparation method thereof |
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