CN107561137A - Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nano composite material and preparation method thereof - Google Patents
Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nano composite material and preparation method thereof Download PDFInfo
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- CN107561137A CN107561137A CN201610510452.3A CN201610510452A CN107561137A CN 107561137 A CN107561137 A CN 107561137A CN 201610510452 A CN201610510452 A CN 201610510452A CN 107561137 A CN107561137 A CN 107561137A
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Abstract
The invention discloses a kind of Fe1.833(OH)0.5O2.5Nitrogen-doped graphene nano composite material and preparation method thereof is loaded, its step is：Under ultrasound, the alcohol suspension of graphene oxide is prepared using oxidation graphite solid；Add FeCl2·4H2O stirs into suspension；By suspension and NH3·H2After O mixing, hydro-thermal reaction, graphite oxide and NH are carried out rapidly3·H2O ratio is 1:1~1:5 mg/μl；Reaction temperature is 160 ~ 200 DEG C；Washing, obtain described nano composite material after drying, the preparation of the nano composite material is a kind of science integration nano-metal-oxide growth in situ, one pot of hydro-thermal assemble method of graphene oxide synchronization reduction technique.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, particularly a kind of Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano composite material（Fe1.833(OH)0.5O2.5/NG）And preparation method thereof, belong to material
Preparation field.
Background technology
The mankind in agro-farming largely using a large amount of discharges of formulation fertilizer containing nitrogen industrial wastewater in addition, the earth's surface for being available for the mankind to use
Water resource is polluted, and such environmental problem has caused worldwide concern.Nitrite in drinking water
Pollution can cause many diseases such as methemoglobinemia, blue baby's syndrome to also have stomach cancer etc..World Health Organization's regulation drink
With the content of water nitrite no more than 3 mgL-1.Because nitrite is to environment and the adverse effect of human health, because
This has caused the attention of height for the sensitive detection of nitrite.
Some analysis means for being developed application include AAS, chemiluminescence, capillary electrophoresis, color
Spectrometry etc., these analysis methods usually require the instrument and equipment, complicated detecting step and consumption substantial amounts of time of costliness, 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, come the sensitivity for reducing overvoltage and improving nitrite sensing.
Graphene（Graphene）, as new two-dimension nano materials, possess high conductivity, wide electrochemical window, most
Possess good chemical stability in number electrolyte and the advantages of surface easily regenerates, this is provided to seek preferable nanostructured
Important channel.Fe1.833(OH)0.5O2.5It is a kind of hydrated ferric oxide that hydroxyl is filled in anion sub-lattice, contains 11
Individual Fe3+, 3 OH-With 15 O2-.It is heat-resisting to reach 1000 DEG C.Graphene and Fe1.833(OH)0.5O2.5Synergy can be with
Assigning the new characteristic of material causes material to have different potential applications for different demands.And in the prior art, structure
Binary composite generally requires the technique of complexity, has wasted largely manpower, material resources, and the three wastes are higher.Thus, using simple
Technology realizes that multicomponent mixture structure nanosensor also turns into one of work that is most important at present and most challenging.（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 is different from the method that the present invention uses used by the above-mentioned methods, prepared by material.Usually, reported in document
The method in road is mostly complicated many more manipulations, and synthesis step is cumbersome, it is difficult to which industrialization large-scale production, the three wastes are more.
The content of the invention
A kind of the deficiencies of present invention is cumbersome, complicated existing for prior art, and the three wastes are larger, there is provided Fe1.833
(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano composite material（Fe1.833(OH)0.5O2.5/NG）And its one kettle way is simply made
Preparation Method.
The technical solution for realizing the object of the invention is：A kind of Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）
Nano composite material（Fe1.833(OH)0.5O2.5/NG）, its general structure is：
。
A kind of Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）The preparation method of nano composite material, by by day
Right graphite powder deep oxidation handles to obtain oxidation graphite solid, then through ultrasonic disperse in ethanol, obtains graphene oxide ethanol
Dispersion liquid, add FeCl2·4H2O 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 comprises the following steps：
Step 1, the Hummers methods after improvement are used to prepare oxidation graphite solid with natural graphite powder；
Under step 2, ultrasound, the alcohol suspension of graphene oxide is prepared；
Step 3, add FeCl2·4H2O stirs into suspension；
Step 4, suspension and NH by step 33·H2After O mixing, hydro-thermal reaction, graphite oxide and NH are carried out rapidly3·H2O
Ratio be 1:1 ~ 1:5 mg/μl；Reaction temperature is 160 ~ 200 DEG C；
Step 5, washing, obtain described Fe after drying1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）It is nano combined
Material（Fe1.833(OH)0.5O2.5/NG）.
Further, in step 2, described 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 FeCl2·4H2O mass ratio is 1:3 ~ 2:1 mg/mg；
Further, in step 4, the hydro-thermal reaction time is 10 ~ 24 h.
Compared with prior art, it is an advantage of the invention that：
（1）Preparation method of the present invention avoids cumbersome multicomponent material synthesis step, it is only necessary to after being stirred,
It can be synthesized using one pot of Hydrothermal Synthesiss technology.
（2）For the present invention as long as by routine operations such as simple centrifuge washing, filterings, technique is simple, green.
（3）Functionalization graphene nano hybridization sensing material prepared by the present invention easily can be reacted by adjusting
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）The preparation method of the present invention presses close to the requirement of Green Chemistry, easily controllable, is advantageous to industrialized mass production.
Embodiments of the invention are described in further detail below in conjunction with the accompanying drawings.
Brief description of the drawings
Fig. 1 is Fe prepared by the present invention1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano composite material
（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 photos of the nano combined sensing material synthesized in the embodiment of the present invention 1.
Fig. 4 is the XRD 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 curves of nitrite.
Embodiment
Embodiments of the invention are described in further detail below in conjunction with the accompanying drawings, the present embodiment is with the technology of the present invention side
Implemented under the premise of case, give detailed embodiment and specific operating process, but protection scope of the present invention is unlimited
In following embodiments.
A kind of as shown in figure 1, Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano composite material（Fe1.833
(OH)0.5O2.5/NG）And preparation method thereof, this method comprises the following steps：
Step 1, the Hummers methods after improvement are used 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；
Step 3, add FeCl2·4H2O stirs into suspension, graphite oxide and FeCl2·4H2O mass ratio is 1:
3 ~ 2 : 1 mg/mg；
Step 4, mixture and NH by step 33·H2After O mixing, it is quickly charged with hydrothermal reaction kettle, heating response；Oxidation
Graphite and NH3·H2O ratio is 1:1 ~ 1:5 mg/μL；Reaction temperature is 160 ~ 200 DEG C；Reaction time is 10 ~ 24
h；
Step 5, washing, obtain Fe after drying1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano composite material
（Fe1.833(OH)0.5O2.5/NG）.
Embodiment 1
The first step, the preparation of oxidation graphite solid；
At 80 DEG C, 20 g native graphites are pre-oxidized with the 30 mL concentrated sulfuric acids, 10 g potassium peroxydisulfates and 10 g phosphorus pentoxides
Afterwards, 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 the 20 g graphite pre-oxidized is added thereto, is slowly added into 60
G potassium permanganate so that system temperature is no more than 20 DEG C, and 35 DEG C are warming up to after addition, after stirring 2 h, and it is in batches slow
It is slow to add 920 mL deionized waters so that system temperature is no more than 98 DEG C, is stirred for after 15 minutes, adds 2.8 L deionizations
Water and the % hydrogen peroxide of 50 mL 30.Obtained glassy yellow suspension is depressurized and filtered, washing.Until there is no sulfuric acid in filtrate
Radical ion, and in it is neutral when, product is dried in 60 DEG C of vacuum, obtains oxidation graphite solid；
Second step, 50 mg graphite oxides powder are loaded into round-bottomed flask, add 70 mL alcohol solvents, after 10 h of ultrasound, are obtained
To graphene oxide（GO）Suspension；
3rd step, add 0.05 g FeCl2·4H2Stirred 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 with hydrothermal reaction kettle, 180
DEG C h of heating response 12；
5th step, by the crude product that the 4th step obtains through filtering, washing, after drying, washing, obtain Fe after drying1.833
(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano composite material（Fe1.833(OH)0.5O2.5/NG）.
The infrared spectrum 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 figures of the nano combined sensing material of functionalization graphene are as shown in Figure 3, it was demonstrated that the nano-hybrid material has succeeded
Synthesis.
The XRD 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 curves of nitrite, it was demonstrated that the nano-hybrid material has to nitrite
There is good electro-catalysis response.
Embodiment 2
The first step, with step 1 in embodiment 1.
Second step, 50 mg graphite oxides powder are loaded into round-bottomed flask, add 50 mL alcohol solvents, 24 h of ultrasound
Afterwards, graphene oxide is obtained（GO）Suspension；
3rd step, add 0.15 g FeCl2·4H2Stirred 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 with hydrothermal reaction kettle, 180
DEG C h of heating response 12；
5th step, with step 5 in embodiment 1.
Embodiment 3
The first step, with step 1 in embodiment 1.
Second step, 50 mg graphite oxides powder are loaded into round-bottomed flask, add 100 mL alcohol solvents, 5 h of ultrasound
Afterwards, graphene oxide is obtained（GO）Suspension；
3rd step, add 0.025 g FeCl2·4H2Stirred 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 with hydrothermal reaction kettle, 160
DEG C h of heating response 24；
5th step, with step 5 in embodiment 1.
Embodiment 4
The first step, with step 1 in embodiment 1.
Second step, 50 mg graphite oxides powder are loaded into round-bottomed flask, add 70 mL alcohol solvents, 15 h of ultrasound
Afterwards, graphene oxide is obtained（GO）Suspension；
3rd step, add 0.10 g FeCl2·4H2Stirred 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 with hydrothermal reaction kettle, 200
DEG C h of heating response 12；
5th step, with step 5 in embodiment 1.
Embodiment 5
The first step, with step 1 in embodiment 1.
Second step, 50 mg graphite oxides powder are loaded into round-bottomed flask, add 80 mL alcohol solvents, 18 h of ultrasound
Afterwards, graphene oxide is obtained（GO）Suspension；
3rd step, add 0.10 g FeCl2·4H2Stirred 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 with hydrothermal reaction kettle, 180
DEG C h of heating response 12；
5th step, with step 5 in embodiment 1.
Embodiment 6
The first to two step, with step 1 in embodiment 1 to two.
3rd step, add 0.025 g FeCl2·4H2Stirred 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.
3rd step, add 0.10 g FeCl2·4H2Stirred 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.
3rd step, add 0.15 g FeCl2·4H2Stirred 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 with hydrothermal reaction kettle,
180 DEG C of h of heating response 12；
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 with hydrothermal reaction kettle,
180 DEG C of h of heating response 12；
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 with hydrothermal reaction kettle,
180 DEG C of h of heating response 12；
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 with hydrothermal reaction kettle,
180 DEG C of h of heating response 12；
5th step, with step 5 in embodiment 1.
Present invention, avoiding cumbersome multicomponent material synthesis step, it is only necessary to after being stirred, utilizes one pot of hydro-thermal
Synthetic technology can synthesize.The building-up process includes the growth in situ of nano metal particles, the N doping of graphene oxide.Close
Cheng Hou, as long as passing through the routine operations such as simple centrifuge washing, filtering, you can be prepared.The function that simultaneously prepared by the present invention
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.The preparation method of the present invention presses close to green
The requirement of chemistry, it is easily controllable, be advantageous to industrialized mass production.
Claims (9)
- A kind of 1. Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nano composite material, it is characterised in that its general structure is：。
- 2. nano composite material as claimed in claim 1, it is characterised in that prepared by following steps：Step 1, the Hummers methods after improvement are used 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；Step 3, add FeCl2·4H2O stirs into suspension；Step 4, suspension and NH by step 33·H2After O mixing, hydro-thermal reaction, graphite oxide and NH are carried out rapidly3·H2O's Than for 1:1 ~ 1:5 mg/μl；Reaction temperature is 160 ~ 200 DEG C；Step 5, washing, obtain described nano composite material after drying.
- 3. nano composite material as claimed in claim 2, it is characterised in that in step 2, described ultrasonic time be 5 ~ 24 h。
- 4. nano composite material as claimed in claim 2, it is characterised in that in step 2, graphite oxide and alcohol solvent Than for 0.2 ~ 1：1mg/ml.
- 5. nano composite material as claimed in claim 2, it is characterised in that in step 3, graphite oxide and FeCl2·4H2O Mass ratio be 1:3 ~ 2:1 mg/mg.
- 6. nano composite material as claimed in claim 2, it is characterised in that in step 4, the hydro-thermal reaction time is 10 ~ 24 h。
- 7. the preparation method of the nano composite material as described in claim 1-6 is any.
- 8. the application of the nano composite material as described in claim 1-6 is any.
- 9. application as claimed in claim 8, it is characterised in that by described nanocomposite applications in the electricity of nitrite Chemical catalysis is detected with analyzing.
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| CN201610510452.3A CN107561137B (en) | 2016-07-01 | Fe1.833(OH)0.5O2.5Load nitrogen-doped graphene nanocomposite and preparation method thereof |
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| CN107561137B CN107561137B (en) | 2019-07-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108424617A (en) * | 2018-03-15 | 2018-08-21 | 厦门大学 | A kind of preparation method and applications of iron oxide hydroxide load graphene oxide fire retardant |
| CN109317201A (en) * | 2018-08-23 | 2019-02-12 | 南京理工大学 | Cyclodextrin modified organic aryne nanobelt functionalization nitrogen-doped graphene electrochemical sensing material and preparation method thereof |
| CN109358100A (en) * | 2018-08-23 | 2019-02-19 | 南京大学盐城环保技术与工程研究院 | Ethanol amine and the graphene-based nano combined sensing material of Nano silver grain difunctionalization support type and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108424617A (en) * | 2018-03-15 | 2018-08-21 | 厦门大学 | A kind of preparation method and applications of iron oxide hydroxide load graphene oxide fire retardant |
| CN109317201A (en) * | 2018-08-23 | 2019-02-12 | 南京理工大学 | Cyclodextrin modified organic aryne nanobelt functionalization nitrogen-doped graphene electrochemical sensing material and preparation method thereof |
| CN109358100A (en) * | 2018-08-23 | 2019-02-19 | 南京大学盐城环保技术与工程研究院 | Ethanol amine and the graphene-based nano combined sensing material of Nano silver grain difunctionalization support type and preparation method thereof |
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