CN108101030A - A kind of preparation method of three-dimensional porous grapheme material - Google Patents
A kind of preparation method of three-dimensional porous grapheme material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 239000012943 hotmelt Substances 0.000 claims abstract description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 6
- 238000000197 pyrolysis Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 3
- 230000001960 triggered effect Effects 0.000 claims abstract description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
- -1 polyethylene Polymers 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000004425 Makrolon Substances 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 229920000515 polycarbonate Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 238000009825 accumulation Methods 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 19
- 239000002994 raw material Substances 0.000 description 12
- 239000003575 carbonaceous material Substances 0.000 description 11
- 239000004417 polycarbonate Substances 0.000 description 10
- 229910021389 graphene Inorganic materials 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- BFMKFCLXZSUVPI-UHFFFAOYSA-N ethyl but-3-enoate Chemical compound CCOC(=O)CC=C BFMKFCLXZSUVPI-UHFFFAOYSA-N 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Landscapes
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of three-dimensional porous grapheme material; after hot-melt resin powder and template and deionized water are stirred evenly together; it is transferred in reaction kettle; after certain temperature and time-triggered protocol; room temperature is cooled to furnace temperature; moisture is dried again, is finally transferred in heating furnace and is pyrolyzed in the environment of vacuum either atmosphere protection, the product of pyrolysis is washed through deionized water to neutral, drying and can obtain three-dimensional porous grapheme material；The specific surface area of the three-dimensional porous grapheme material of gained is more than 800m2/ g is demonstrated by excellent electrochemistry accumulation of energy performance in the negative material as lithium ion battery, while the material can be expanded in ultracapacitor.
Description
Technical field
The invention belongs to porous material preparing technical fields, relate in particular to a kind of three-dimensional with porous structure（3D）Class stone
The preparation method of black alkene material.
Background technology
With porous structure carbon material with better steric configuration, while it can be in the energy, environment and catalytic field
It is widely applied, therefore has become current research hotspot for this research with porous structure carbon material.At present, have
Porous structure carbon material is typically to pass through self assembly, water using the presoma of carbon nanotubes, graphene or other types of carbon
Hot method either template constructed its can be directly used for battery either the carrier of the electrode of capacitor or catalyst improve
Catalytic performance can also be assembled into the sorbing material of harmful substance in environment.Zishou Zhang, et al. are by selecting carbon nanometer
Pipe, ethylene vinyl acetate copolymer and poly- propylamine are prepared for a kind of carbon material with three-dimensional structure, and by the material of preparation
For in the electrode of ultracapacitor, the results showed that this carbon material with three-dimensional structure is after charge and discharge reach 45000 times
The specific capacity property retention efficiency of capacitance reaches more than 95%（Zhang, Z. S. et al., Three-dimensional
carbon nanotube/ ethylvinylacetate/polyaniline as a high performance
electrode for supercapacitors. J Mater Chem A 2015, 3 (5), 1884-1889.）；Hui
Mao. et al. polypropylene and acrylic acid and NaHCO3Template is prepared with deionized water collective effect to be prepared for containing carboxylic
The carbon ball of acid group（-COOH-PS）, the carbon ball and platinum chloride, glucose are reacted in hydrochloric acid and aqueous solution, it is dry using washing
Dry and protective atmosphere is sintered to obtain three-dimensional Supported Pt Nanoparticles（Pt）The carbon material of particle, and use it for carbon monoxide（CO）Oxidation
Journey, the results showed that the carbon material of this three-dimensional structure has higher catalytic activity（Mao, H. et al., Highly
active and stable heterogeneous catalysts based on the entrapment of noble
metal nanoparticles in 3D ordered porous carbon. Carbon 2016, 96, 75-82.）；
Kyoungsoo Kim.et al. have synthesized porous three-dimensional graphene carbon materials by using group of the lanthanides catalytic action in zeolite template
Material, the template are removed using the mixed acid of hydrofluoric acid and hydrochloric acid（Kim, K. et al., Lanthanum-catalysed
synthesis of microporous 3D graphene-like carbons in a zeolite template.
Nature 2016, 535 (7610), 131）.
As a result, in the preparation process of 3D porous carbon materials, prepared using self-assembly method and usually require multistep reaction ability
It realizes, and template prepares porous structure carbon material and usually requires to carry out the removal of template, and removing template is gone to usually require to use nothing
Machine strong acid or highly basic, this certainly will need to carry out experimental facilities some special requirements, especially carry out large batch of material
It prepares.Meanwhile strong acid and highly basic necessarily also bring along the problem of environment, do not meet the developing direction of Modern Green chemical industry.Therefore
How to realize that simple for process, scale and green prepare porous structure carbon material and have great importance.
The content of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of environmentally protective and efficient three-dimensional porous graphite
The preparation method of alkene material.
The technical solution adopted by the present invention is：
A kind of preparation method of three-dimensional porous grapheme material, comprises the following steps：By hot-melt resin powder and template with
It and after deionized water stirs evenly together, is transferred in reaction kettle, after certain temperature and time-triggered protocol, is cooled to furnace temperature
Room temperature, then moisture is dried, it is finally transferred in heating furnace and is pyrolyzed in the environment of vacuum either atmosphere protection, by the production of pyrolysis
Object washs to neutral, drying through deionized water and can obtain three-dimensional porous class grapheme material；The hot-melt resin is poly-
It is one or several kinds of in ethylene, makrolon, polyamide, polymethyl methacrylate, polyethylene terephthalate
Mixture；The template is one kind or wherein arbitrary several in sodium carbonate, potassium carbonate, sodium acid carbonate and saleratus
Mixture, total addition level are the 10 ~ 400% of hot-melt resin quality.
As preference, in the preparation method of above-mentioned three-dimensional porous grapheme material, in the reaction heat kettle
Temperature is 100 ~ 200 DEG C, and the time is 1 ~ 20h.
As preference, in the preparation method of above-mentioned three-dimensional porous grapheme material, the drying is in oven heat
Middle progress, controlled at 40 ~ 120 DEG C, the time is 6 ~ 20h.
As preference, in the preparation method of above-mentioned three-dimensional porous grapheme material, the atmosphere is nitrogen, argon
Gas or helium.
As preference, in the preparation method of above-mentioned three-dimensional porous grapheme material, the temperature of the pyrolysis is
500~1000℃。
As preference, in the preparation method of above-mentioned three-dimensional porous grapheme material, described is dry using freezing
Dry or vacuum drying, freeze-drying temperature are -50 ~ -10 DEG C, and vacuum drying temperature is 50 ~ 120 DEG C.
Compared with prior art, the present invention has the advantages that：The present invention has screened distinctive by many experiments
The resin template mating with it, selected template have good water-soluble and catalytic so that it passes through after preparing
Pyrolysis and washing can remove template, without using inorganic acid or highly basic.And prepare the three-dimensional porous class graphite of gained
The specific surface area of alkene material is more than 800m2/ g is demonstrated by excellent electrochemistry in the negative material as lithium ion battery and stores
It can performance.
Description of the drawings
Fig. 1 is the X-ray diffractogram that 3D porous graphene materials are prepared by raw material of PC（XRD）；
Fig. 2 is the scanning electron microscope (SEM) photograph that 3D porous graphene materials are prepared by raw material of PC（SEM）；
Fig. 3 is the transmission electron microscope picture that 3D porous graphene materials are prepared by raw material of PC（TEM）；
Fig. 4 is the specific surface area figure that 3D porous graphene materials are prepared by raw material of PC（BET）；
Fig. 5 is that 3D porous graphenes material is prepared by raw material of PC in 100 mA g-1Capacity Plan during electric current；
Fig. 6 is the SEM figures that 3D porous graphene materials are prepared by raw material of PET and PE；
Fig. 7 is the SEM figures that 3D porous graphene materials are prepared by raw material of PMMA.
Specific embodiment
With reference to embodiment, the invention will be further described, but embodiment does not limit in any form invention.
Embodiment 1
Take 10 grams（g）Makrolon and 10 g sodium acid carbonates and 8 milliliters（ml）Deionized water stirs into uniform mixing together
Object.Then uniformly mixed substance is transferred in PTFE reaction kettles（There is stainless steel sleeve outside）, reaction kettle is put into baking oven, is risen
Temperature is to 160 DEG C, when then constant temperature 5 is small（h）, after being cooled to room temperature with furnace temperature, it is drawn off drying in an oven, is then put
Enter in porcelain crucible in vacuum atmosphere oven with 5 centigrade per minutes（℃/min）Rate be warming up to 700 DEG C, 5 h of constant temperature, with stove
It is taken out after warm natural cooling.It is 7 that reaction product, which carries out deionized water to wash to filtrate pH value, then at 65 degrees Celsius（℃）It is true
Empty drying box dries 12h, obtains specific surface area as 1150 m2The porous class grapheme materials of 3D of/g.The material of the preparation is made
For the negative material of lithium ion battery, it is tested in 100 mA g-1When charge and discharge 60 are enclosed under electric current, specific capacity can reach 705
mAh g-1.It is the X-ray diffractogram of the porous class grapheme materials of 3D prepared by raw material of PC for wherein Fig. 1（XRD）, Fig. 2 is
SEM using PC as the porous class grapheme material of 3D prepared by raw material schemes, and Fig. 3 is using PC as the porous class graphite of 3D prepared by raw material
Alkene material TEM schemes, and Fig. 4 is that the BET using PC as the porous class grapheme material of 3D prepared by raw material schemes, and Fig. 5 is using PC as raw material system
The porous class grapheme materials of standby 3D are in 100 mA g-1Capacity Plan during electric current.
Embodiment 2
Take 15 g polyethylene terephthalates（PET）With 5g polyethylene with 15 g sodium carbonate and 10 ml deionized waters, one
It rises and stirs into uniform mixture.Then uniformly mixed substance is transferred in PTFE reaction kettles（There is stainless steel sleeve outside）, will
Reaction kettle is put into baking oven, is warming up to 180 DEG C, then 4 h of constant temperature, after being cooled to room temperature with furnace temperature, is drawn off in an oven
Drying, then puts it into porcelain crucible in nitrogen（N2）In special atmosphere oven, 800 DEG C are warming up to the rate of 6 DEG C/min,
Constant temperature 3h, with being taken out after furnace temperature natural cooling.It is 7 that reaction product, which carries out deionized water to wash to filtrate pH value, then at -40 DEG C
Freeze drying plant in dry 12 h, obtain specific surface area as 1100 m2The porous class grapheme materials of 3D of/g（See Fig. 6）,
Using the material of the preparation as the negative material of lithium ion battery, it is tested in 500 mA g-1When charge and discharge 100 are enclosed under electric current,
Its specific capacity can reach 605 mAh g-1。
Embodiment 3
Take 15 g polymethyl methacrylates（PMMA）It is gone with 10 g potassium carbonate with 10g saleratus mixed powder and 10 ml
Ionized water stirs into uniform mixture together.Then uniformly mixed substance is transferred in PTFE reaction kettles（Have outside stainless
Steel bushing）, reaction kettle is put into baking oven, is warming up to 200 DEG C, then 3 h of constant temperature, after being cooled to room temperature with furnace temperature, is drawn off
It dries, is then put it into porcelain crucible in argon gas in an oven（Ar）In special atmosphere oven, heated up with the rate of 6 DEG C/min
To 850 DEG C, constant temperature 2h, with being taken out after furnace temperature natural cooling.It is 7 that reaction product, which carries out deionized water to wash to filtrate pH value, so
The vacuum drying chamber at 80 DEG C dries 10h afterwards, obtains specific surface area as 1050 m2The porous class grapheme materials of 3D of/g（See
Fig. 7）, using the material of the preparation as the negative material of lithium ion battery, it is tested in 1000 mA g-1Charge and discharge 100 under electric current
During circle, specific capacity can reach 496 mAh g-1。
Embodiment 4
On the basis of embodiment 1, makrolon is changed into polyamide, sodium acid carbonate changes potassium carbonate into, and other conditions are constant, obtain
It is 1200 m to specific surface area2The porous class grapheme materials of 3D of/g.It is tested in 100 mA g-1Charge and discharge 60 are enclosed under electric current
When, specific capacity can reach 710 mAh g-1, performance and embodiment 1 are substantially quite.
Claims (7)
1. a kind of preparation method of three-dimensional porous grapheme material, feature are comprising the following steps：By hot-melt resin powder
After being stirred evenly together with template and deionized water, it is transferred in reaction kettle, after certain temperature and time-triggered protocol, with
Furnace temperature is cooled to room temperature, then moisture is dried, and is finally transferred in heating furnace and is pyrolyzed in the environment of vacuum either atmosphere protection,
The product of pyrolysis is washed through deionized water to neutral, drying and can obtain three-dimensional porous class grapheme material；
The hot-melt resin is polyethylene, makrolon, polyamide, polymethyl methacrylate, poly terephthalic acid second
One or several kinds of mixtures in diol ester；
The template is arbitrary several for one kind in sodium carbonate, potassium carbonate, sodium acid carbonate and saleratus or wherein to be mixed
Object is closed, total addition level is the 10 ~ 400% of hot-melt resin quality.
2. the preparation method of three-dimensional porous grapheme material according to claim 1, which is characterized in that the reaction heat
Temperature in kettle is 100 ~ 200 DEG C, and the time is 1 ~ 20h.
3. the preparation method of three-dimensional porous grapheme material according to claim 1, which is characterized in that it is described drying be
It is carried out in oven heat, controlled at 40 ~ 120 DEG C, the time is 6 ~ 20h.
4. the preparation method of three-dimensional porous grapheme material according to claim 1, which is characterized in that the atmosphere is
Nitrogen, argon gas or helium.
5. the preparation method of three-dimensional porous grapheme material according to claim 1, which is characterized in that the pyrolysis
Temperature is 500 ~ 1000 DEG C.
6. the preparation method of three-dimensional porous grapheme material according to claim 1, which is characterized in that the drying is adopted
With freeze-drying or vacuum drying, freeze-drying temperature is -50 ~ -10 DEG C, and vacuum drying temperature is 50 ~ 120 DEG C.
7. the three-dimensional porous grapheme material obtained by claim 1 is as the application in lithium ion battery negative material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109250707A (en) * | 2018-11-30 | 2019-01-22 | 浙江农林大学 | A kind of grapheme material and preparation method using waste tire preparation |
| CN114162807A (en) * | 2022-01-18 | 2022-03-11 | 广州巨湾技研有限公司 | Three-dimensional porous graphene material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663448A (en) * | 2012-09-19 | 2014-03-26 | 天津普兰纳米科技有限公司 | Preparation method of carbon material, obtained carbon material and application thereof |
| CN105502359A (en) * | 2015-12-22 | 2016-04-20 | 福州大学 | Preparation method of low-cost porous graphene |
| CN106058173A (en) * | 2016-06-14 | 2016-10-26 | 中南大学 | Graphene-like carbon material/sulphur composite cathode material for lithium-sulphur battery, and preparation method and application thereof |
| CN106744859A (en) * | 2017-01-22 | 2017-05-31 | 广西大学 | Graphene three-dimensional multistage pore structure powder prepared by a kind of low temperature polymer cracking |
| US20170182474A1 (en) * | 2015-12-28 | 2017-06-29 | Aruna Zhamu | Integral 3D graphene-carbon hybrid foam and devices containing same |
| CN107301922A (en) * | 2017-06-07 | 2017-10-27 | 中国人民解放军国防科学技术大学 | Three-dimensional porous graphene nano material and its preparation method and application |
-
2018
- 2018-02-09 CN CN201810131171.6A patent/CN108101030B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663448A (en) * | 2012-09-19 | 2014-03-26 | 天津普兰纳米科技有限公司 | Preparation method of carbon material, obtained carbon material and application thereof |
| CN105502359A (en) * | 2015-12-22 | 2016-04-20 | 福州大学 | Preparation method of low-cost porous graphene |
| US20170182474A1 (en) * | 2015-12-28 | 2017-06-29 | Aruna Zhamu | Integral 3D graphene-carbon hybrid foam and devices containing same |
| CN106058173A (en) * | 2016-06-14 | 2016-10-26 | 中南大学 | Graphene-like carbon material/sulphur composite cathode material for lithium-sulphur battery, and preparation method and application thereof |
| CN106744859A (en) * | 2017-01-22 | 2017-05-31 | 广西大学 | Graphene three-dimensional multistage pore structure powder prepared by a kind of low temperature polymer cracking |
| CN107301922A (en) * | 2017-06-07 | 2017-10-27 | 中国人民解放军国防科学技术大学 | Three-dimensional porous graphene nano material and its preparation method and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109250707A (en) * | 2018-11-30 | 2019-01-22 | 浙江农林大学 | A kind of grapheme material and preparation method using waste tire preparation |
| CN114162807A (en) * | 2022-01-18 | 2022-03-11 | 广州巨湾技研有限公司 | Three-dimensional porous graphene material and preparation method thereof |
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