CN107561130A - The Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Load nano combined sensing material of nitrogen-doped graphene and preparation method thereof - Google Patents
The Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Load nano combined sensing material of nitrogen-doped graphene and preparation method thereof Download PDFInfo
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- CN107561130A CN107561130A CN201610510423.7A CN201610510423A CN107561130A CN 107561130 A CN107561130 A CN 107561130A CN 201610510423 A CN201610510423 A CN 201610510423A CN 107561130 A CN107561130 A CN 107561130A
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Abstract
The invention discloses a kind of Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Nano combined sensing material of nitrogen-doped graphene and preparation method thereof is loaded, its step is：Under ultrasound, the alcohol suspension of graphene oxide is prepared using oxidation graphite solid；Add PDDA to stir into suspension, continuously add FeCl2·4H2O stirs；By said mixture and NH3·H2Hydro-thermal reaction is carried out immediately after O mixing, wherein, graphite oxide and NH3·H2O ratio is 1:1~1:5 mg/μl；Reaction temperature is 160 ~ 200 DEG C；Washing, described sensing material is obtained after drying, the preparation of the nano combined sensing material is a kind of science integration nano-metal-oxide growth in situ, graphene oxide synchronization reduction and one pot of hydro-thermal assemble method of polymer overmold Functionalization.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 polydiene propyl group two
Ammonio methacrylate（PDDA）The Fe of cladding1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano combined sensing material and its
Preparation method, belong to field of material preparation.
Background technology
Nitrite is widely present in human environment, is most common nitrogen-containing compound in nature, green plants
Nitrogen source, frequently as food additive and preservative in food industry.The pollution of nitrite in drinking water can cause many diseases
Sick such as methemoglobinemia, blue baby's syndrome also has stomach cancer, and these diseases are all by nitrite and amine substance reaction
Caused by the nitrosamine generated.Because nitrite is to environment and the adverse effect of human health, therefore for nitrite
Sensitive detection has caused the attention of height.
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.
It is carbon nano-structured（Including fullerene, CNT and graphene etc.）Possess in terms of Electrochemical Detection a large amount of
Application.Because these materials possess high conductivity, wide electrochemical window, possess good chemical stability in most of electrolyte
And surface the advantages of easily regenerating.In carbon material, graphene（Graphene）, as new two-dimension nano materials, to seek
Preferable nanostructured is asked to provide important channel.The synergy of graphene and other components can assign material new spy
Property cause material that there is different potential applications, such as metal-metallic oxide nano-particle, polymer for different demands
And the binary catalyst system such as biomolecule.However, although the load of the nano-particle with catalytic activity is shown well
Chemical property, but nano-particle is immobilized on the top layer of graphene the characteristics of due in its structure, causes poor in dispersiveness.
PDDA（PDDA）, a kind of cationic polyelectrolyte of line style, material scatter can be effectively improved.And
In the prior art, structure trielement composite material generally requires the technique of complexity, has wasted largely manpower, material resources, the three wastes compared with
It is high.Thus, realize that multicomponent mixture structure nanosensor also turns into work that is most important at present and most challenging using simple technique
One of.（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 polydiene third
Base alkyl dimethyl ammonium chloride（PDDA）The Fe of cladding1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano combined sensing material
And preparation method thereof.
The technical solution for realizing the object of the invention is：A kind of Fe of diallyl dimethyl ammoniumchloride cladding1.833
(OH)0.5O2.5The nano combined sensing material of nitrogen-doped graphene is loaded, its general structure is as follows：
。
A kind of Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5Load nitrogen-doped graphene nanometer is answered
The preparation method of sensing material is closed, by handling natural graphite powder deep oxidation to obtain oxidation graphite solid, then through in ethanol
Middle ultrasonic disperse, graphene oxide alcohol dispersion liquid is obtained, add PDDA and FeCl2·4H2O is after stirring, one pot of hydro-thermal is closed
Into can be prepared by crude product.After filtering and drying, the nano combined sensing material of functionalization graphene is obtained.Its specific work
Skill 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；
Stirred in step 3, the suspension added in PDDA to step 2, continuously add FeCl2·4H2O stirs；
Step 4, the mixture and NH for obtaining step 33·H2O mixing after carry out hydro-thermal reaction immediately, wherein, graphite oxide and
NH3·H2O ratio is 1:1 ~ 1:5 mg/μl；Reaction temperature is 160 ~ 200 DEG C；
Step 5, washing, obtain described sensing material Fe after drying1.833(OH)0.5O2.5/NG@PDDA。
Further, in step 2, described ultrasonic time is 5 ~ 24 h.
Further, in step 2, the ratio of graphite oxide and ethanol is 1 ~ 0.2 mg/ml.
Further, in step 3, graphite oxide and PDDA ratio are 1:1 ~ 1:10 mg/μl；Graphite oxide and
FeCl2·4H2O mass ratio is 1:3 ~ 2:1.
Further, in step 4, the 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）PDDA introducing is effectively improved the dispersive property of sensing material, makes it advantageously in it as electrification
Learn sensing material.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 diallyl dimethyl ammoniumchloride prepared by the present invention（PDDA）Coat Fe1.833(OH)0.5O2.5Load nitrogen
Doped graphene（NG）The preparation process schematic diagram of nano combined sensing material.
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 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, diallyl dimethyl ammoniumchloride（PDDA）The Fe of cladding1.833(OH)0.5O2.5Load nitrogen
Doped graphene（NG）Nano combined sensing material 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 alcohol 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；
Stirred in step 3, the suspension added in PDDA to step 2, graphite oxide and PDDA ratio are 1:1 ~ 1:10
mg/μl；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 diallyl dimethyl ammoniumchloride after drying（PDDA）The Fe of cladding1.833(OH)0.5O2.5
Load nitrogen-doped graphene（NG）Nano combined sensing material.
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,
Obtain graphene oxide（GO）Suspension；
3rd step, after 400 μ L PDDA of addition stir into the suspension in step 2, add 0.05 g FeCl2·
4H2O stirs into suspension;
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 polydiene propyl group after drying
Alkyl dimethyl ammonium chloride（PDDA）The Fe of cladding1.833(OH)0.5O2.5Load nitrogen-doped graphene（NG）Nano combined sensing material.
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.
I-t curve such as Fig. 4 institute of the nano combined sensing material modified glassy carbon electrode of functionalization graphene for nitrite
Show, it was demonstrated that the nano-hybrid material has good electro-catalysis response to nitrite.
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, after 500 μ l PDDA of addition stir into the suspension in step 2, add 0.15 g FeCl2·
4H2O stirs into suspension;
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, after 50 μ l PDDA of addition stir into the suspension in step 2, add 0.025 g FeCl2·
4H2O stirs into suspension;
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, after 400 μ l PDDA of addition stir into the suspension in step 2, add 0.10 g FeCl2·
4H2O stirs into suspension;
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, after 300 μ l PDDA of addition stir into the suspension in step 2, add 0.10 g FeCl2·
4H2O stirs into suspension;
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, after 400 μ L PDDA of addition stir into the suspension in step 2, add 0.025 g
FeCl2·4H2O stirs into suspension;
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, after 400 μ L PDDA of addition stir into the suspension in step 2, add 0.10 g
FeCl2·4H2O stirs into suspension;
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, after 400 μ L PDDA of addition stir into the suspension in step 2, add 0.15 g
FeCl2·4H2O stirs into suspension;
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 and
PDDA cladding.After synthesis, as long as passing through the routine operations such as simple centrifuge washing, filtering, you can be prepared.This hair simultaneously
The functionalization graphene nano hybridization sensing material of bright preparation 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.PDDA introducing is effective
Ground improves the dispersive property of sensing material, makes it advantageously in it as electrochemical sensing material.The preparation side of the present invention
The requirement of the nearly Green Chemistry of the choice specimen of calligraphy, it is easily controllable, be advantageous to industrialized mass production.
Claims (9)
- A kind of 1. Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5It is nano combined to load nitrogen-doped graphene Sensing material, it is characterised in that its general structure is as follows：Wherein, NG represents nitrogen-doped graphene, and PDDA represents diallyl dimethyl ammoniumchloride.
- A kind of 2. Fe of diallyl dimethyl ammoniumchloride cladding1.833(OH)0.5O2.5It is nano combined to load nitrogen-doped graphene Sensing material, 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；Stirred in step 3, the suspension added in PDDA to step 2, continuously add FeCl2·4H2O stirs；Step 4, mixture and NH by step 33·H2Hydro-thermal reaction is carried out immediately after O mixing, wherein, graphite oxide and NH3· H2O ratio is 1:1 ~ 1:5 mg/μl；Reaction temperature is 160 ~ 200 DEG C；Step 5, washing, obtain described sensing material after drying.
- 3. sensing material as claimed in claim 1, it is characterised in that in step 2, ultrasonic time is 5 ~ 24 h.
- 4. sensing material as claimed in claim 1, it is characterised in that in step 2, the ratio of graphite oxide and ethanol for 1 ~ 0.2 mg/ml。
- 5. sensing material as claimed in claim 1, it is characterised in that in step 3, graphite oxide and PDDA ratio are 1:1 ~ 1:10 mg/μl；Graphite oxide and FeCl2·4H2O mass ratio is 1:3 ~ 2:1.
- 6. sensing material as claimed in claim 1, it is characterised in that in step 4, the reaction time is 10 ~ 24 h.
- 7. the preparation method of the sensing material as described in claim 1-6 is any.
- 8. the application of the sensing material as described in claim 1-6 is any.
- 9. application as claimed in claim 8, it is characterised in that described sensing material is applied to the electrochemistry of nitrite Catalysis detecting is with analyzing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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