CN107561137B - Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof - Google Patents
Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof Download PDFInfo
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- 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 36
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 26
- 239000000725 suspension Substances 0.000 claims abstract description 25
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- IOVCWXUNBOPUCH-UHFFFAOYSA-M nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002604 ultrasonography Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 238000011068 load Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L Iron(II) chloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 3
- 229910021382 natural graphite Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 230000002194 synthesizing Effects 0.000 abstract description 6
- 238000005580 one pot reaction Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 230000001360 synchronised Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- 239000011540 sensing material Substances 0.000 description 10
- 238000007306 functionalization reaction Methods 0.000 description 8
- 239000005456 alcohol based solvent Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- VZJVWSHVAAUDKD-UHFFFAOYSA-N Potassium permanganate Chemical compound [K+].[O-][Mn](=O)(=O)=O VZJVWSHVAAUDKD-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 206010011705 Cyanosis neonatal Diseases 0.000 description 1
- 206010017758 Gastric cancer Diseases 0.000 description 1
- -1 Graphite alkene Chemical class 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N Iron(III) oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 208000005135 Methemoglobinemia Diseases 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L Potassium persulfate Chemical class [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003894 drinking water pollution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004156 green chemistry Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910000460 iron oxide Inorganic materials 0.000 description 1
- 238000011031 large scale production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Abstract
The invention discloses a kind of Fe1.833(OH)0.5O2.5Nitrogen-doped graphene nanocomposite and preparation method thereof is loaded, the steps include: under ultrasound, the alcohol suspension of graphene oxide is prepared using oxidation graphite solid；FeCl is added2·4H2O is stirred evenly into suspension；By suspension and NH3·H2After O mixing, hydro-thermal reaction, graphite oxide and NH are carried out rapidly3·H2The ratio of O is 1:1 ~ 1:5 mg/ μ l；Reaction temperature is 160 ~ 200 DEG C；The nanocomposite is obtained after washing, drying, the preparation of the nanocomposite is a kind of science integration nano-metal-oxide growth in situ, one pot of hydro-thermal assemble method of the synchronous reduction technique of graphene oxide.The hybrid material synthesis step that the present invention synthesizes is simple, efficient, is easy to largely prepare, and is particularly suitable for application as the electrochemical catalysis detecting and analysis of nitrite.
Description
Technical field
The present invention relates to a kind of functionalization graphene nano material and preparation method thereof, especially a kind of Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene (NG) nanocomposite (Fe1.833(OH)0.5O2.5/ NG) and preparation method thereof, belong to material
Preparation field.
Background technique
The mankind largely use a large amount of discharges of formulation fertilizer containing nitrogen industrial wastewater in addition, the earth's surface used for the mankind in agro-farming
Water resource is being polluted, and such environmental problem has caused worldwide concern.Nitrite in drinking water
Pollution can lead to that many diseases such as methemoglobinemia, there are also gastric cancers etc. for blue baby's syndrome.World Health Organization's regulation drink
With the content of nitrite in water no more than 3 mgL-1.Since nitrite is to the adverse effect of environment and human health, because
This sensitively detects nitrite the attention for having caused height.
Some has included spectrophotometry, chemiluminescence, capillary electrophoresis, color by the analysis means of development and application
Spectrometry etc., these analysis methods usually require expensive instrument and equipment, complicated detecting step and consumption a large amount of time, and
These methods are compared, and electrochemical method can provide relative compact, cheap, reliable, sensitive and instant analysis detection.It is a variety of
Functional nanomaterials, which have been explored, carrys out modified electrode, to reduce overvoltage and improve the sensitivity of nitrite sensing.
Graphene (Graphene) possesses high conductivity, wide electrochemical window, most as novel two-dimension nano materials
Possess good chemical stability in number electrolyte and the advantages of surface easily regenerates, this is provided to seek ideal nanostructure
Important channel.Fe1.833(OH)0.5O2.5It is a kind of hydrated ferric oxide for filling hydroxyl in anion sub-lattice, contains 11
A Fe3+, 3 OH-With 15 O2-.It is heat-resisting to reach 1000 DEG C.Graphene and Fe1.833(OH)0.5O2.5Synergistic effect can assign
Giving the new characteristic of material makes material have different potential applications for different demands.And in the prior art, building two
First composite material generally requires complicated technique, has wasted largely manpower, material resources, and the three wastes are higher.Thus, utilize simple technique
Realize that multicomponent mixture building nanosensor also becomes one of current most important and work most challenged.(1. L. Cui, T.
Pu, Y. Liu, X. He, Electrochim. Acta 88 (2013) 559-564. 2. J. Jiang, W. Fan,
X. Du, Biosens. Bioelectron. 51 (2014) 343-348)
But method used by the above-mentioned methods, prepared by material is different from the method that the present invention uses.Generally, document
The method of middle report is mostly complicated many more manipulations, and synthesis step is cumbersome, it is difficult to industrialization large-scale production, the three wastes compared with
It is more.
Summary of the invention
The present invention provides a kind of Fe for the deficiencies of of the existing technology cumbersome, complicated, the three wastes are larger1.833
(OH)0.5O2.5Load nitrogen-doped graphene (NG) nanocomposite (Fe1.833(OH)0.5O2.5/ NG) and its one kettle way simply make
Preparation Method.
The technical solution for realizing the aim of the invention is as follows: a kind of Fe1.833(OH)0.5O2.5It loads nitrogen-doped graphene (NG)
Nanocomposite (Fe1.833(OH)0.5O2.5/ NG), general structure are as follows:
。
A kind of Fe1.833(OH)0.5O2.5The preparation method for loading nitrogen-doped graphene (NG) nanocomposite, by by day
Right graphite powder deep oxidation handles to obtain oxidation graphite solid, then through ultrasonic disperse in ethanol, obtains graphene oxide ethyl alcohol
FeCl is added in dispersion liquid2·4H2O is after stirring, one pot of hydrothermal synthesis can be prepared by crude product.After filtering and drying,
Obtain the nano combined sensing material of functionalization graphene.Its specific technique the following steps are included:
Step 1 uses improved Hummers method to prepare oxidation graphite solid with natural graphite powder；
Under step 2, ultrasound, the alcohol suspension of graphene oxide is prepared；
FeCl is added in step 32·4H2O is stirred evenly into suspension；
Step 4, suspension and NH by step 33·H2After O mixing, hydro-thermal reaction, graphite oxide and NH are carried out rapidly3·
H2The ratio of O is 1:1 ~ 1:5 mg/ μ l；Reaction temperature is 160 ~ 200 DEG C；
The Fe is obtained after step 5, washing, drying1.833(OH)0.5O2.5It is multiple to load nitrogen-doped graphene (NG) nanometer
Condensation material (Fe1.833(OH)0.5O2.5/ NG).
Further, in step 2, the ultrasonic time is 5 ~ 24 h.
Further, in step 2, the ratio of graphite oxide and alcohol solvent is 0.2 ~ 1: 1mg/ml；
Further, in step 3, graphite oxide and FeCl2·4H2The mass ratio of O is 1:3 ~ 2:1 mg/mg；
Further, in step 4, the hydro-thermal reaction time is 10 ~ 24 h.
Compared with prior art, the invention has the advantages that
(1) preparation method of the present invention avoids cumbersome multicomponent material synthesis step, it is only necessary to mixed by stirring
After conjunction, it can be synthesized using one pot of hydrothermal synthesis technology.
(2) as long as the present invention is environmentally protective by routine operations, simple processes such as simple centrifuge washing, filterings.
(3) functionalization graphene nano hybridization sensing material prepared by the present invention can be easily by adjusting reaction
Temperature and burden control Fe1.833(OH)0.5O2.5Load capacity and size on NG, and then adjust the catalytic performance of hybrid material.
(4) preparation method of the invention close to Green Chemistry requirement, it is easily controllable, be conducive to industrialized mass production.
The embodiment of the present invention is described in further detail with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is Fe prepared by the present invention1.833(OH)0.5O2.5Load nitrogen-doped graphene (NG) nanocomposite
(Fe1.833(OH)0.5O2.5/ NG) preparation process schematic diagram.
Fig. 2 is the infrared spectrogram of the nano combined sensing material synthesized in the embodiment of the present invention 1.
Fig. 3 is the TEM photo of the nano combined sensing material synthesized in the embodiment of the present invention 1.
Fig. 4 is the XRD diagram of the nano combined sensing material synthesized in the embodiment of the present invention 1.
Fig. 5 is the nano combined sensing material modified glassy carbon electrode pair of functionalization graphene in invention embodiment 1
In the i-t curve of nitrite.
Specific embodiment
The embodiment of the present invention is described in further detail with reference to the accompanying drawing, the present embodiment is with the technology of the present invention side
Implemented under the premise of case, the detailed implementation method and specific operation process are given, but protection scope of the present invention is unlimited
In following embodiments.
As shown in Figure 1, a kind of Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene (NG) nanocomposite (Fe1.833
(OH)0.5O2.5/ NG) and preparation method thereof, method includes the following steps:
Step 1 uses improved Hummers method to prepare oxidation graphite solid with natural graphite powder；
Under step 2, ultrasound, the DMF suspension of graphene oxide is prepared, the ratio of graphite oxide and alcohol solvent is 1 ~
0.2 mg/mL；Ultrasonic time is 5 ~ 24 h；
FeCl is added in step 32·4H2O is stirred evenly into suspension, graphite oxide and FeCl2·4H2The mass ratio of O
For 1: 3 ~ 2: 1 mg/mg；
Step 4, mixture and NH by step 33·H2It after O mixing, is quickly charged in hydrothermal reaction kettle, heating reaction；Oxygen
Graphite and NH3·H2The ratio of O is 1:1 ~ 1:5 mg/ μ L；Reaction temperature is 160 ~ 200 DEG C；Reaction time is 10 ~ 24
h；
Fe is obtained after step 5, washing, drying1.833(OH)0.5O2.5Load nitrogen-doped graphene (NG) nanocomposite
(Fe1.833(OH)0.5O2.5/ NG).
Embodiment 1
The first step, the preparation of oxidation graphite solid；
It is with the 30 mL concentrated sulfuric acids, 10 g potassium peroxydisulfates and 10 g phosphorus pentoxides that 20 g natural graphites are pre- at 80 DEG C
After oxidation, pH=7 are washed to, air drying is stand-by overnight；
The 460 mL concentrated sulfuric acids are cooled to 0 DEG C or so, then by 20 g pre-oxidize graphite be added thereto, slowly plus
Enter 60 g potassium permanganate, so that system temperature is no more than 20 DEG C, 35 DEG C are warming up to after addition, after stirring 2 h, and point
It criticizes and is slowly added into 920 mL deionized waters, so that system temperature is no more than 98 DEG C, be stirred for after 15 minutes, 2.8 L are added and go
30 % hydrogen peroxide of ionized water and 50 mL.Obtained glassy yellow suspension is depressurized and is filtered, washing.Until not having in filtrate
Sulfate ion, and when being in neutrality, product is dried in 60 DEG C of vacuum, obtains oxidation graphite solid；
50 mg graphite oxide powder are packed into round-bottomed flask, add 70 mL alcohol solvents, 10 h of ultrasound by second step
Afterwards, the suspension of graphene oxide (GO) is obtained；
0.05 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
4th step, by the mixture of step 3 and 100 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step is filtered the crude product that the 4th step obtains, washing, after dry, obtains Fe after washing, drying1.833
(OH)0.5O2.5Load nitrogen-doped graphene (NG) nanocomposite (Fe1.833(OH)0.5O2.5/ NG).
The infrared spectroscopy of the nano combined sensing material of functionalization graphene is as shown in Figure 2, it was demonstrated that the nano-hybrid material is
Success synthesizes.
The TEM figure of the nano combined sensing material of functionalization graphene is as shown in Figure 3, it was demonstrated that the nano-hybrid material has succeeded
Synthesis.
The XRD diagram of the nano combined sensing material of functionalization graphene is as shown in figure 4, the nano combined sensing of functionalization graphene
Material modified glassy carbon electrode is as shown in Figure 5 for the i-t curve of nitrite, it was demonstrated that the nano-hybrid material has nitrite
There is good electro-catalysis to respond.
Embodiment 2
The first step, with step 1 in embodiment 1.
50 mg graphite oxide powder are packed into round-bottomed flask, add 50 mL alcohol solvents, 24 h of ultrasound by second step
Afterwards, the suspension of graphene oxide (GO) is obtained；
0.15 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
4th step, by the mixture of step 3 and 250 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 3
The first step, with step 1 in embodiment 1.
50 mg graphite oxide powder are packed into round-bottomed flask, add 100 mL alcohol solvents, 5 h of ultrasound by second step
Afterwards, the suspension of graphene oxide (GO) is obtained；
0.025 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
4th step, by the mixture of step 3 and 150 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
24 h are reacted in 160 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 4
The first step, with step 1 in embodiment 1.
50 mg graphite oxide powder are packed into round-bottomed flask, add 70 mL alcohol solvents, 15 h of ultrasound by second step
Afterwards, the suspension of graphene oxide (GO) is obtained；
0.10 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
4th step, by the mixture of step 3 and 50 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 200 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 5
The first step, with step 1 in embodiment 1.
50 mg graphite oxide powder are packed into round-bottomed flask, add 80 mL alcohol solvents, 18 h of ultrasound by second step
Afterwards, the suspension of graphene oxide (GO) is obtained；
0.10 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
4th step, by the mixture of step 3 and 200 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 6
The first to two step, with step 1 in embodiment 1 to two.
0.025 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
Four to five step, with step 4 in embodiment 1 to five.
Embodiment 7
The first to two step, with step 1 in embodiment 1 to two.
0.10 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
Four to five step, with step 4 in embodiment 1 to five.
Embodiment 8
The first to two step, with step 1 in embodiment 1 to two.
0.15 g FeCl is added in third step2·4H2It is stirred evenly in suspension in O to step 2;
Four to five step, with step 4 in embodiment 1 to five.
Embodiment 9
The first to three step, with step 1 in embodiment 1 to three.
4th step, by the mixture of step 3 and 50 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 10
The first to three step, with step 1 in embodiment 1 to three.
4th step, by the mixture of step 3 and 150 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 11
The first to three step, with step 1 in embodiment 1 to three.
4th step, by the mixture of step 3 and 200 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step, with step 5 in embodiment 1.
Embodiment 12
The first to three step, with step 1 in embodiment 1 to three.
4th step, by the mixture of step 3 and 250 μ L NH3·H2After O mixing, it is quickly charged in hydrothermal reaction kettle,
12 h are reacted in 180 DEG C of heating；
5th step, with step 5 in embodiment 1.
The invention avoids cumbersome multicomponent material synthesis steps, it is only necessary to after mixing by stirring, utilize one pot of hydro-thermal
Synthetic technology can synthesize.It include the growth in situ of nano metal particles, the N doping of graphene oxide in the synthesis process.It closes
Cheng Hou, as long as can be prepared by routine operations such as simple centrifuge washing, filterings.Function prepared by the present invention simultaneously
Graphite alkene nano hybridization sensing material can be easily by adjusting reaction temperature and burden control Fe1.833(OH)0.5O2.5Load capacity and size on NG, and then adjust the catalytic performance of hybrid material.Preparation method of the invention is close to green
The requirement of chemistry, it is easily controllable, be conducive to industrialized mass production.
Claims (5)
1. a kind of Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite, which is characterized in that by following steps system
It is standby:
Step 1 uses improved Hummers method to prepare oxidation graphite solid with natural graphite powder；
Under step 2, ultrasound, the alcohol suspension of graphene oxide is prepared using oxidation graphite solid, graphite oxide and ethyl alcohol are molten
The ratio of agent is 0.2 ~ 1: 1mg/ml；
FeCl is added in step 32·4H2O is stirred evenly into suspension, graphite oxide and FeCl2·4H2The mass ratio of O is 1:3
~ 2:1；
Step 4, suspension and NH by step 33·H2O mixing after, rapidly carry out 10 ~ 24 h of hydro-thermal reaction, graphite oxide and
NH3·H2The ratio of O is 1:1 ~ 1:5 mg/ μ l；Reaction temperature is 160 ~ 200 DEG C；
The nanocomposite is obtained after step 5, washing, drying.
2. nanocomposite as described in claim 1, which is characterized in that in step 2, ultrasonic time is 5 ~ 24 h.
3. the preparation method of the nanocomposite as described in claim 1-2 is any.
4. the application of the nanocomposite as described in claim 1-2 is any.
5. application as claimed in claim 4, which is characterized in that by the nanocomposite applications in the electricity of nitrite
In chemical catalysis detecting and analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610510452.3A CN107561137B (en) | 2016-07-01 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610510452.3A CN107561137B (en) | 2016-07-01 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107561137A CN107561137A (en) | 2018-01-09 |
| CN107561137B true CN107561137B (en) | 2019-07-16 |
Family
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|---|---|---|---|---|
| CN102145282A (en) * | 2010-05-28 | 2011-08-10 | 南京理工大学 | Preparation method of graphene-supported nano MnOOH composite material |
| CN104984693A (en) * | 2015-07-24 | 2015-10-21 | 扬州大学 | Preparation method of nanometer magnetism capsule |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145282A (en) * | 2010-05-28 | 2011-08-10 | 南京理工大学 | Preparation method of graphene-supported nano MnOOH composite material |
| CN104984693A (en) * | 2015-07-24 | 2015-10-21 | 扬州大学 | Preparation method of nanometer magnetism capsule |
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| Title |
|---|
| One-pot preparation of Au-RGO/PDDA nanocomposites and their application for nitrite sensing;Shoufeng Jiao 等;《Sensors and Actuators B: Chemical》;20141113;第208卷;全文 |
| Solvent-free mechanochemical synthesis of graphene oxide and Fe3O4–reduced grapheme oxide nanocomposites for sensitive detection of nitrite;G. Bharath 等;《Journal of Materials Chemistry A》;20150617;第5卷;第15529-15532页，图3 |
| The Effect of Bio-Coal on the Carbothermic Reduction of Laterite Ores;Guan-Jhou Chen 等;《Materials Transactions》;20150325;第56卷(第4期);第550页 |
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