CN106987925A - A kind of functionalization graphene preparation method based on ion exchange - Google Patents
A kind of functionalization graphene preparation method based on ion exchange Download PDFInfo
- Publication number
- CN106987925A CN106987925A CN201710311533.5A CN201710311533A CN106987925A CN 106987925 A CN106987925 A CN 106987925A CN 201710311533 A CN201710311533 A CN 201710311533A CN 106987925 A CN106987925 A CN 106987925A
- Authority
- CN
- China
- Prior art keywords
- ion exchange
- preparation
- graphene oxide
- rgo
- functionalization graphene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 59
- 238000005342 ion exchange Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000007306 functionalization reaction Methods 0.000 title claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 63
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000002166 wet spinning Methods 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 230000009467 reduction Effects 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000001112 coagulating effect Effects 0.000 claims description 4
- 238000009987 spinning Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 229910052786 argon Inorganic materials 0.000 description 7
- 239000011149 active material Substances 0.000 description 6
- 238000004070 electrodeposition Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000007654 immersion Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- -1 graphite alkene Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000009133 cooperative interaction Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003759 clinical diagnosis Methods 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt(II) nitrate Inorganic materials [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Inorganic materials [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Fibers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention is a kind of preparation method of functionalization graphene fiber based on ion exchange；Described functionalization graphene fiber is, using graphene oxide as presoma, ion exchange, prepared by final high temperature is reduced to be carried out after wet spinning, then with metal salt solution.Preparation method includes following part：Graphene oxide fiber is prepared by wet spinning；Graphene oxide fiber is soaked in metal salt solution (solvent is second alcohol and water) (soak time 30min 7h)；Under an inert gas, different functionalization graphene fibers, such as Cu/rGO, Fe are prepared by Muffle furnace high temperature reduction2O3The functionalization graphene fiber such as/rGO, CoO/rGO, NiO/rGO.
Description
Technical field
The present invention is belonged to based on ion-exchange field, is specifically related to the preparation field of functionalization graphene fiber.
Technical background
In recent years, with multi-functional fibrous electronics such as sensing, driving, energy conversion, storage, data storage/transmission
Textile turns into a fast-developing research field, and in medical treatment, clinical diagnosis, live medical monitoring, intelligence is wearable
There is superior application prospect in clothes, military affairs etc..Due to carbon fiber (Typical Representative graphene fiber) have lighter quality,
The features such as good pliability, environmental stability, high mechanical strength and electric conductivity, the device of some fibre shape is successfully applied to,
Such as electro-catalysis, ultracapacitor, solar cell.
All the time, graphene fiber is made due to occurring arrangement and overlapping accumulation by the graphene nanometer sheet of thermal reduction
It is similar to the solid fibrous carbon of naturally occurring, all it is difficult further optimization, so as to limit its high-performance and multi-functional application.
It is worth noting that, composite graphite alkene can reach collaboration effect with other nano materials (such as polymer, metal, metal oxide etc.)
Should, so as to obtain abundant unprecedented application.In recent years, researchers did many trials, and such as electrochemical deposition is common
The methods such as spinning prepare multifunctional graphite vinyl compound.But the graphene complex obtained by both preparation methods all fails
Have the layer architecture of composite fibre on nanometer micro-scale, thus limit graphene nanometer sheet and electrochemical active material it
Between cooperative interaction.Wet spinning is carried out again for example, first mixing active material with graphene by the method for cospinning, can be existed
Active material is difficult to be well mixed with graphene, and easily occurs agglomeration, and we are effectively kept away based on ion-exchange
This problem is exempted from, such as Fig. 1 is the SEM figures of Ag/rGO fibers prepared by cospinning method.Not only cost is high for same electrochemical deposition method,
Energy expenditure is big, and functionalization graphene prepared by the method, and active material only adsorbs only on graphenic surface and easy
In the presence of absorption non-uniform phenomenon, and not only cost is low for our this preparation methods based on ion exchange, consumes energy small, and activity
Material not only adsorbs only on graphenic surface, is also present between graphene sheet, so that it is overlapping to be effectively improved graphene sheet
Problem, realizes more fully functionalization, and such as Fig. 2 is ZrO prepared by electrochemical deposition method2The SEM figures of/rGO compounds.
The content of the invention
It is an object of the invention to provide a kind of preparation side of the novel multifunctional graphite vinyl fiber based on ion exchange
Method, by the cooperative interaction between active material and graphene sheet, is effectively improved graphene sheet overlap problem, realizes stone
Black alkene more fully functionalization.
The preparation method for the multifunctional graphite vinyl fiber that the present invention is provided, comprises the following steps：
Graphene oxide is prepared, graphene oxide fiber is prepared by wet spinning；
Configure 1~5wt% Cu (NO3)2, or Fe (NO3)3, or Co (NO3)2, or Ni (NO3)2Ethanol water, will be above-mentioned
The graphene oxide fiber of preparation is soaked in metal salt solution (solvent：Second alcohol and water) in；
After the graphene oxide fiber that the metal ion of above-mentioned preparation is combined is spontaneously dried, pass through Muffle furnace thermal reduction.
Cu/GO fibers 800 DEG C of heat treatment 1-2h under the conditions of argon gas hydrogen gas mixture, Fe/GO, Co/GO, Ni/GO fibers exist respectively
400 DEG C of heat treatment 1-2h, obtain multi-functional graphene fiber under the conditions of argon gas；
The soak time 30min-7h is (in Cu (NO3)230min, Fe (NO are soaked in ethanol water3)3Ethanol is water-soluble
7h is soaked in liquid)；
The metal salt solution solvent is that the volume ratio of ethanol and water is 2:1.
Beneficial effect：
The synthetic method of the present invention uses common and resourceful raw material, so that with relatively low cost, and it is low to consume energy；
The method reaction condition of spontaneous carry out ion exchange is gentle in the solution, and technique is simple, and favorable reproducibility is not only prevented effectively from cospinning
The agglomeration traits of middle appearance, moreover it is possible to be effectively improved active material in electrochemical deposition method and adsorb non-uniform phenomenon, more fully in fact
Existing graphene functionalized.
Brief description of the drawings
Fig. 1 is the SEM figures of Ag/rGO fibers prepared by cospinning method；
Fig. 2 is ZrO prepared by electrochemical deposition method2The SEM figures of/rGO compounds；
Fig. 3 is the SEM figures of graphene fiber prepared by the wet spinning of embodiment 2；
The SEM figures for the Cu/rGO fibers that Fig. 4 for embodiment 3 prepare after ion exchange；
The SEM figures for the Cu/rGO fibers that Fig. 5 for embodiment 3 prepare after ion exchange
The XPS figures for the Cu/rGO fibers that Fig. 6 for embodiment 3 prepare after ion exchange；
Fig. 7 is the Fe that embodiment 4 prepared after ion exchange2O3The SEM figures of/rGO fibers；
Fig. 8 is the Fe that embodiment 4 prepared after ion exchange2O3The XPS figures of/rGO fibers；
The XPS figures for the CoO/rGO fibers that Fig. 9 for embodiment 5 prepare after ion exchange；
The XPS figures for the NiO/rGO fibers that Figure 10 for embodiment 6 prepare after ion exchange；
Embodiment：
Present disclosure is further illustrated below in conjunction with example, as known by the technical knowledge, the present invention also can be by other
The scheme of the technology of the present invention feature is not departed to describe, it is therefore all within the scope of the present invention or in the equivalent scope of the invention
Change is included in the invention.
Embodiment 1：
The preparation of graphene oxide：Under ice bath, 2g graphite powder is distributed to the dense sulphur that 100mL mass fractions are 98%
In acid, be slowly added to mixing time~1 hour at 10-12g potassium permanganate, 30 DEG C under stirring, then be slowly added dropwise 160mL go from
Sub- water, heating stirring 30 minutes to 1 hour under 90 DEG C of oil baths adds 400mL deionized waters, finally adds 12-15mL mass
The H of concentration 30%2O2, stir 30 minutes, with obtaining gluey oxygen after mass concentration~5%HCl solution, deionized water cyclic washing
Graphite alkene.
| Sequence number | Graphite powder (g) | 98% concentrated sulfuric acid ml | Potassium permanganate (g) | Deionized water ml is added for the first time | Second of addition deionized water ml | H2O2ml |
| 1 | 2 | 100 | 10 | 160 | 400 | 12 |
| 2 | 2 | 100 | 12 | 160 | 400 | 15 |
| 3 | 2 | 100 | 12 | 160 | 400 | 12 |
Embodiment 2：
The preparation of graphene fiber：First by wet spinning spin processes, the 16-30mg/mL GO aqueous solution is passed through into syringe pump
(ejection of syringe pump speed is 10-30 μ L/min) is expelled in coagulating bath, and coagulating bath uses the saturation ethanol solution of potassium hydroxide,
Prepare graphene oxide fiber.By Muffle furnace, under argon gas and hydrogen gas mixture environment, with 2-10 DEG C/min speed
Heat up, maintain 2-4 hours redox graphene fibers to obtain the preferable graphene fiber of electric conductivity at 400 DEG C -800 DEG C；
To the present embodiment product using its microscopic appearance of scanning electron microscopic observation, as a result as shown in figure 3, being 2 hours at 800 DEG C
The graphene fiber partial enlarged drawing of reduction；
Embodiment 3：
The preparation of Cu/rGO fibers：As described in Example 2, graphene oxide fiber is first prepared, being immersed in 1~
5wt%Cu (NO3)230 minutes to 3 hours in ethanol water, the volume ratio of ethanol and water is 2:1, by the fiber after immersion certainly
So dry, finally under the conditions of argon gas and hydrogen gas mixture, heated up, maintained at 800-1000 DEG C with 2-10 DEG C/min speed
Cu/rGO fibers are made in reduction in 2-4 hours.
| Sequence number | Cu(NO3)2Mass fraction (%) | Soak time (h) |
| 1 | 1 | 3 |
| 2 | 3 | 3 |
| 3 | 5 | 0.5 |
To the present embodiment product using scanning electron microscopic observation its microscopic appearance, as a result such as Fig. 4, shown in 5, Cu nano particles into
Being distributed on graphene fiber for work(, XPS tests are carried out to it, as a result as Fig. 6 further proves that the product is Cu/rGO fibers；
Embodiment 4：
Fe2O3The preparation of/rGO fibers：As described in Example 2, graphene oxide fiber is first prepared, being immersed in 1~
5wt%Fe (NO3)33-7 hours in ethanol water, the volume ratio of ethanol and water is 2:1, the fiber after immersion is spontaneously dried,
Finally under the conditions of argon gas, heated up with 2-10 DEG C/min speed, maintain reduction in 2-4 hours that Fe is made at 400 DEG C -500 DEG C2O3/
RGO fibers.
| Sequence number | Fe(NO3)3Mass fraction (%) | Soak time (h) |
| 1 | 1 | 3 |
| 2 | 3 | 3 |
| 3 | 5 | 7 |
To the present embodiment product using its microscopic appearance of scanning electron microscopic observation, as a result as shown in fig. 7, Fe2O3Nano particle is not
Graphenic surface is only successfully distributed in, and is also present between graphene film plate, XPS tests are carried out to it, as a result such as Fig. 8
It is Fe further to prove the product2O3/ rGO fibers；
Embodiment 5：
The preparation of CoO/rGO fibers：As described in Example 2, graphene oxide fiber is first prepared, being immersed in 1~
5wt%Co (NO3)230 minutes to 3 hours in ethanol water, the volume ratio of ethanol and water is 2:1, by the fiber after immersion certainly
So dry, finally under the conditions of argon gas, heated up with 2-10 DEG C/min speed, 2-4 hours reduction systems are maintained at 400 DEG C -500 DEG C
Obtain CoO/rGO fibers.
| Sequence number | Co(NO3)2Mass fraction (%) | Soak time (h) |
| 1 | 1 | 3 |
| 2 | 3 | 3 |
| 3 | 5 | 0.5 |
XPS tests are carried out to the present embodiment product, as a result as shown in Figure 9, it was demonstrated that the product is CoO/rGO fibers；
Embodiment 6：
The preparation of NiO/rGO fibers：As described in Example 2, graphene oxide fiber is first prepared, being immersed in 1~
5wt%Ni (NO3)230 minutes to 3 hours in ethanol water, the volume ratio of ethanol and water is 2:1, by the fiber after immersion certainly
So dry, finally under the conditions of argon gas, heated up with 2-10 DEG C/min speed, 2-4 hours reduction systems are maintained at 400 DEG C -500 DEG C
Obtain NiO/rGO fibers.
| Sequence number | Ni(NO3)2Mass fraction (%) | Soak time (h) |
| 1 | 1 | 3 |
| 2 | 3 | 3 |
| 3 | 5 | 0.5 |
XPS tests are carried out to the present embodiment product, as a result as shown in Figure 10, it was demonstrated that the product is NiO/rGO fibers.
Claims (9)
1. a kind of preparation method of the functionalization graphene based on ion exchange, it is characterised in that functionalization graphene fiber is
Using graphene oxide as presoma, ion exchange is carried out after wet spinning, then with metal salt solution, final high temperature is reduced and is made
, specifically include following steps：
(1) wet spinning is used, using graphene oxide water solution as spinning solution, spinning solution is expelled to by coagulating bath by syringe pump
In, prepare graphene oxide fiber；
(2) the graphene oxide fiber of collection is soaked in metal salt solution；
(3) under an inert gas, Muffle furnace high temperature reduction.
2. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that：
Graphene oxide fiber is prepared using wet spinning in step (1), spinning solution is the graphene oxide that solubility is 16-30mg/mL
The aqueous solution.
3. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that：
Graphene oxide fiber is prepared using wet spinning in step (1), coagulating bath is the saturation ethanol solution of potassium hydroxide.
4. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that：
Graphene oxide fiber is prepared using wet spinning in step (1), the injection rate of syringe pump is 10-30 μ L/min.
5. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that：
Metal salt solution is Cu (NO in step (2)3)2Ethanol water or Fe2(NO3)3Ethanol water or Co (NO3)2Second
Alcohol solution or Ni (NO3)2Ethanol water, soak time 30 minutes to 7 hours, the body of ethanol and water in ethanol water
Product is than being 2:1.
6. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that
Soak time is 30 minutes to 7 hours in step (2).
7. a kind of preparation method of functionalization graphene based on ion exchange according to claims 1, its feature exists
In：The mass fraction of metal salt is 1-5wt% in metal salt solution in step (2).
8. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that：
Metal salt solution is Cu (NO in step (2)3)2, then Cu/rGO fibers are the heating rates in 2-10 DEG C/min in step (3),
Maintained 2-4 hours at 800-1000 DEG C, H2It is made under the conditions of-Ar mixed gas.
9. a kind of preparation method of functionalization graphene based on ion exchange according to claim 1, it is characterised in that：
Metal salt solution is Fe in step (2)2(NO3)3Or Co (NO3)2Or Ni (NO3)2, then Fe in step (3)2O3/rGO,CoO/rGO,
NiO/rGO fibers are maintained 2-4 hour at the heating rate in 2-10 DEG C/min, 400-500 DEG C, obtained under the conditions of Ar gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710311533.5A CN106987925B (en) | 2017-05-05 | 2017-05-05 | Functionalized graphene preparation method based on ion exchange |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710311533.5A CN106987925B (en) | 2017-05-05 | 2017-05-05 | Functionalized graphene preparation method based on ion exchange |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106987925A true CN106987925A (en) | 2017-07-28 |
| CN106987925B CN106987925B (en) | 2020-06-12 |
Family
ID=59418698
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710311533.5A Active CN106987925B (en) | 2017-05-05 | 2017-05-05 | Functionalized graphene preparation method based on ion exchange |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106987925B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107489018A (en) * | 2017-08-07 | 2017-12-19 | 中国科学技术大学 | A kind of new poly-dopamine coated graphite alkene composite fibre and preparation method thereof |
| CN111705419A (en) * | 2020-06-28 | 2020-09-25 | 南京工业大学 | Metal-loaded carbon nitride-doped graphene-based flexible non-woven fabric and preparation method and application thereof |
| CN113443885A (en) * | 2020-07-10 | 2021-09-28 | 青岛理工大学 | Grouting material and preparation and application thereof |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050079119A1 (en) * | 2003-01-23 | 2005-04-14 | Canon Kabushiki Kaisha | Method for producing nano-carbon materials |
| CN102534869A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Method for preparing high-strength conductive graphene fiber by large-size graphene oxide sheet |
| CN102534865A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Ion-enhanced graphene fiber and preparation method thereof |
| CN102874799A (en) * | 2012-09-25 | 2013-01-16 | 南京工业大学 | Method for preparing graphene and titanium dioxide composite material by vapor phase reduction method |
| CN103225203A (en) * | 2013-05-09 | 2013-07-31 | 西北工业大学 | Preparation method of carbon fiber-graphene oxide-carbon nanotube multi-scale reinforcement |
| CN104099687A (en) * | 2013-04-10 | 2014-10-15 | 华为技术有限公司 | Graphene fiber and preparation method thereof |
| CN104451952A (en) * | 2014-10-28 | 2015-03-25 | 大连理工大学 | Reductive graphene coated cobaltosic oxide composite nano fiber and preparation process thereof |
| KR20150090605A (en) * | 2014-01-29 | 2015-08-06 | 한국과학기술연구원 | Single step multi-atom doping method of carbon materials and use thereof |
| CN104975368A (en) * | 2015-07-27 | 2015-10-14 | 天津工业大学 | Multiwalled carbon nanotube and graphene reinforced modified regenerated protein fiber and preparation method thereof |
| CN105256408A (en) * | 2015-11-29 | 2016-01-20 | 南京新月材料科技有限公司 | Graphene oxide fibers and preparation method thereof |
| CN105544017A (en) * | 2016-01-27 | 2016-05-04 | 浙江大学 | High-conductivity graphene fiber and preparation method thereof |
| US20160301096A1 (en) * | 2015-04-13 | 2016-10-13 | Aruna Zhamu | Zinc Ion-Exchanging Energy Storage Device |
| CN106032585A (en) * | 2015-03-13 | 2016-10-19 | 中国科学院上海应用物理研究所 | Graphene-inorganic nanometer particle composite fiber and preparing method thereof |
| US20170084924A1 (en) * | 2015-09-23 | 2017-03-23 | University Of Virginia Patent Foundation | Process of forming electrodes and products thereof from biomass |
-
2017
- 2017-05-05 CN CN201710311533.5A patent/CN106987925B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050079119A1 (en) * | 2003-01-23 | 2005-04-14 | Canon Kabushiki Kaisha | Method for producing nano-carbon materials |
| CN102534869A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Method for preparing high-strength conductive graphene fiber by large-size graphene oxide sheet |
| CN102534865A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Ion-enhanced graphene fiber and preparation method thereof |
| CN102874799A (en) * | 2012-09-25 | 2013-01-16 | 南京工业大学 | Method for preparing graphene and titanium dioxide composite material by vapor phase reduction method |
| CN104099687A (en) * | 2013-04-10 | 2014-10-15 | 华为技术有限公司 | Graphene fiber and preparation method thereof |
| CN103225203A (en) * | 2013-05-09 | 2013-07-31 | 西北工业大学 | Preparation method of carbon fiber-graphene oxide-carbon nanotube multi-scale reinforcement |
| KR20150090605A (en) * | 2014-01-29 | 2015-08-06 | 한국과학기술연구원 | Single step multi-atom doping method of carbon materials and use thereof |
| CN104451952A (en) * | 2014-10-28 | 2015-03-25 | 大连理工大学 | Reductive graphene coated cobaltosic oxide composite nano fiber and preparation process thereof |
| CN106032585A (en) * | 2015-03-13 | 2016-10-19 | 中国科学院上海应用物理研究所 | Graphene-inorganic nanometer particle composite fiber and preparing method thereof |
| US20160301096A1 (en) * | 2015-04-13 | 2016-10-13 | Aruna Zhamu | Zinc Ion-Exchanging Energy Storage Device |
| CN104975368A (en) * | 2015-07-27 | 2015-10-14 | 天津工业大学 | Multiwalled carbon nanotube and graphene reinforced modified regenerated protein fiber and preparation method thereof |
| US20170084924A1 (en) * | 2015-09-23 | 2017-03-23 | University Of Virginia Patent Foundation | Process of forming electrodes and products thereof from biomass |
| CN105256408A (en) * | 2015-11-29 | 2016-01-20 | 南京新月材料科技有限公司 | Graphene oxide fibers and preparation method thereof |
| CN105544017A (en) * | 2016-01-27 | 2016-05-04 | 浙江大学 | High-conductivity graphene fiber and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| HASAN BAGHERIA,ET AL: "《Composite of Cu metal nanoparticles-multiwall carbonnanotubes-reduced graphene oxide as a novel and high performanceplatform of the electrochemical sensor for simultaneousdetermination of nitrite and nitrate", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107489018A (en) * | 2017-08-07 | 2017-12-19 | 中国科学技术大学 | A kind of new poly-dopamine coated graphite alkene composite fibre and preparation method thereof |
| CN111705419A (en) * | 2020-06-28 | 2020-09-25 | 南京工业大学 | Metal-loaded carbon nitride-doped graphene-based flexible non-woven fabric and preparation method and application thereof |
| CN111705419B (en) * | 2020-06-28 | 2021-08-31 | 南京工业大学 | Metal-loaded carbon nitride-doped graphene-based flexible non-woven fabric and preparation method and application thereof |
| CN113443885A (en) * | 2020-07-10 | 2021-09-28 | 青岛理工大学 | Grouting material and preparation and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106987925B (en) | 2020-06-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104838051B (en) | A kind of oxygen and nitrogen co-doped polyacrylonitrile-based carbon fibre and preparation method thereof | |
| CN104724699B (en) | Method for preparing biomass graphene employing cellulose as raw material | |
| CN107393725B (en) | A kind of carbon material supported NiCo of porous, electrically conductive2O4Composite material and its preparation method and application | |
| Zhang et al. | A review: carbon nanofibers from electrospun polyacrylonitrile and their applications | |
| CN104269566B (en) | A kind of preparation method and application of N doping porous carbon nanosheet composite material | |
| Li et al. | Electrosynthesis of hydrogen peroxide via two-electron oxygen reduction reaction: A critical review focus on hydrophilicity/hydrophobicity of carbonaceous electrode | |
| CN102580549B (en) | Method for preparing carbon nano tube modified bipolar membrane with anion groups | |
| CN105088749A (en) | Graphene/cotton cloth flexible conducting fabric and preparing method of graphene/cotton cloth flexible conducting fabric | |
| CN102586952A (en) | Method for preparing graphene-reinforced polyacrylonitrile carbon fibers | |
| CN107601624A (en) | A kind of preparation and application of the electric Fenton cathode material based on carried-type active Carbon fibe | |
| CN106987925A (en) | A kind of functionalization graphene preparation method based on ion exchange | |
| CN103225203A (en) | Preparation method of carbon fiber-graphene oxide-carbon nanotube multi-scale reinforcement | |
| CN109267325A (en) | A kind of graphene/nanometer material that surface is evenly dispersed coating fiber and preparation method thereof | |
| CN106120027A (en) | A kind of preparation method of high porosity mesopore nano-graphene fiber | |
| CN107383405A (en) | A kind of compound proton exchange membrane and preparation method thereof | |
| CN105948038A (en) | Activated carbon microspheres and preparation method thereof | |
| CN110820005B (en) | Preparation method of efficient and stable ruthenium dioxide based acidic oxygen evolution electrocatalyst | |
| CN109755033A (en) | A kind of carbon fiber loaded cobalt/cobalt oxide composite material and preparation method and application | |
| CN109647355A (en) | A kind of preparation method of the efficient adsorbents for lead ion pyrolytic of growth in situ manganese dioxide | |
| CN110534757A (en) | High performance carbon electrode and preparation method thereof | |
| CN111592737A (en) | Microwave-assisted efficient construction method for high-strength interface of carbon-based reinforcement/resin composite material | |
| CN113564913B (en) | Modification treatment method for surface of high-performance carbon fiber | |
| CN108607569A (en) | It improves electro-catalysis and restores CO2The synthetic method of the catalyst of CO selectivity in the process | |
| CN111170307A (en) | Nano-carbon modified hollow activated carbon micro-tube and preparation method and application thereof | |
| Qi et al. | Doping engineering strategies for electrodes and catalysts in vanadium redox flow battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |