CN107662949A - A kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof - Google Patents
A kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof Download PDFInfo
- Publication number
- CN107662949A CN107662949A CN201711029754.XA CN201711029754A CN107662949A CN 107662949 A CN107662949 A CN 107662949A CN 201711029754 A CN201711029754 A CN 201711029754A CN 107662949 A CN107662949 A CN 107662949A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- preparation
- loaded
- nano composite
- oxide
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The present invention relates to field of waste water treatment, disclose a kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof, the preparation method of graphene oxide-loaded ferriferrous oxide nano composite includes preparing addition Fe in graphene oxide disperse system step, and graphene oxide disperse system by what graphite powder, sodium nitrate, the concentrated sulfuric acid and potassium permanganate mixed in ice bath environment3+、Fe2+Ion, and mixed under alkaline environment the step of preparing graphene oxide ferroso-ferric oxide suspension.The preparation method technique of the present invention is simple, safety and environmental protection, and cost is cheap, and the composite of preparation has preferable adsorption capacity for heavy metal in water and organic dyestuff.
Description
Technical field
The present invention relates to field of waste water treatment, in particular to a kind of graphene oxide-loaded ferriferrous oxide nano
Composite and preparation method thereof.
Background technology
Prior art, it is to pass through hydro-thermal mostly when preparing graphene oxide-loaded ferriferrous oxide nano composite
Method or ultrasonic method are carried out, and it has many defects, is mainly reflected in：Hydro-thermal method is carried out using water heating kettle, required experiment bar
Part is more harsh, it usually needs hyperbaric environment, the security reliability of preparation manipulation are relatively low；Hydro-thermal method is typically in closed container
In reacted, whole course of reaction can not be observed, not intuitively；In the preparation process of part, Organic Alcohol (such as ethylene glycol, two are added
Glycol, cyclopentanol, cyclohexanol, isoamyl alcohol or isopropanol), crosslinking agent (such as acrylic acid, methacrylic acid or glyoxal), alkyl
Xanthates (such as ehtyl potassium xanthate, sodium ethylxanthate, amylic potassium xanthate or potassium butyl xanthate), introduce big
The impurity of amount, part organic alcohols have inflammable property, the preservation to whole experimental implementation and medicine, are required for possessing more
High requirement.
The content of the invention
It is an object of the invention to provide a kind of preparation side of graphene oxide-loaded ferriferrous oxide nano composite
Method, the characteristics of its technique is simple, safe and reliable, meanwhile, the material has excellent absorption property to organic dyestuff.
Another object of the present invention is to provide a kind of graphene oxide-loaded ferriferrous oxide nano composite, its
It is made by above-mentioned preparation method.
What embodiments of the invention were realized in：
A kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, it includes：
Prepare graphene oxide disperse system：Including by graphite powder, sodium nitrate, the concentrated sulfuric acid and potassium permanganate in ice bath ring
Mixed in border；
Prepare graphene oxide-ferroso-ferric oxide suspension：It is included in addition Fe in graphene oxide disperse system3+、Fe2+
Ion, and mixed under alkaline environment.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
Preparation Method the step of preparing graphene oxide disperse system in, graphite powder, sodium nitrate and the concentrated sulfuric acid first mix, then to mixed
Solution 15~40min of ultrasonic disperse is closed, then is mixed with potassium permanganate.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
In Preparation Method, ice bath temperature is 2~5 DEG C.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
In Preparation Method, the step of preparing graphene oxide disperse system, also includes：
The first disperse system containing graphite powder, sodium nitrate, the concentrated sulfuric acid and potassium permanganate is diluted, then in water
First set reaction is carried out under bath environment.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
In Preparation Method, the step of preparing graphene oxide disperse system, also includes：
First disperse system adds hydrogen peroxide, the second secondary response is then carried out under water bath after first set reaction.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
In Preparation Method, the step of preparing graphene oxide disperse system, also includes：
Second of reacted disperse system is washed to neutrality, recycles ultrasonic disperse.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
In Preparation Method, in the step of preparing graphene oxide-ferroso-ferric oxide suspension, Fe3+、 Fe2+Ion is with FeCl3And FeCl2
The form of mixed solution mix with graphene oxide disperse system, Fe3+、Fe2+The mol ratio of ion is 2:1.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
In Preparation Method, FeCl3And FeCl2Mixed solution before being mixed with graphene oxide disperse system, first add alkaline solution regulation
PH value.
In an embodiment of the present invention, the system of above-mentioned graphene oxide-loaded ferriferrous oxide nano composite
Preparation Method also includes：
Clean dry：The sediment of graphene oxide-ferroso-ferric oxide suspension is separated and removed, then carries out freezing and does
It is dry.
A kind of graphene oxide-loaded ferriferrous oxide nano composite, it passes through above-mentioned graphene oxide-loaded
The preparation method of ferriferrous oxide nano composite is made.
The beneficial effect of the embodiment of the present invention is：
The preparation method of graphene oxide-loaded ferriferrous oxide nano composite is disperseed including preparing graphene oxide
The step of being and prepare graphene oxide-step of ferroso-ferric oxide suspension two, preparing graphene oxide disperse system includes will
Graphite powder, sodium nitrate, the concentrated sulfuric acid and potassium permanganate mix in ice bath environment；Graphene oxide-ferroso-ferric oxide is prepared to hang
The step of turbid, is included in addition Fe in graphene oxide disperse system3+、Fe2+Ion, and mixed under alkaline environment.The preparation
Method need not react in being pressed into property of closed container high temperature height, and experiment is simple to operation, and the requirement to experiment equipment is relatively low；
In overall process is tested, poisonous and hazardous material will not be produced, other excessive materials will not be introduced, environment will not be caused
Secondary pollution, belong to environmentally friendly；The cost of whole preparation process is relatively low simultaneously, and raw material are all easily obtained.
Embodiment
A kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite of present invention offer, including with
Lower step：
First, graphene oxide disperse system is prepared
A certain proportion of graphite powder and sodium nitrate are placed in three-neck flask, the addition concentrated sulfuric acid, ultrasonic disperse 15~
40min, then three-neck flask is placed in ice bath environment and stirred 30 minutes, potassium permanganate is slowly added in three-neck flask, 2
Stirred 8~12 hours in~5 DEG C of ice bath environment, obtain the first disperse system.Ice bath can be that a low temperature is built in whole reaction
Environment, slow down reaction rate, make whole oxidizing process is uniform and stable slowly to occur so that the graphene oxide of preparation disperses
System has preferably dispersed and single layer structure.
Deionized water is slowly added dropwise in the first disperse system, then flask is placed in water-bath, by temperature adjustment to 50~
60 DEG C, and after 8~12h of stirring reaction, bath temperature is adjusted to 35 DEG C, continues reaction 10~12 hours；
Hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then existed with hydrochloric acid
Washed under the conditions of high speed centrifugation, it is in neutrality then to continue washing pH of mixed into flask with pure water, then small with ultrasonic disperse 3
When, obtain graphene oxide disperse system.In an embodiment of the present invention, the concentration of hydrochloric acid is 5%, and washing times are 10 times, just
The graphene oxide prepared is a kind of colloidal solution, is first in order to destroy micella (can not be filtered with pure water), by greatly with pickling
The residual acid and metal ion of amount are washed off.Containing many hydrophilic functional groups on graphene oxide, such as hydroxyl and carboxylic
Base, this causes graphene oxide to be easier to disperse in water or other solvents.Solubility of the graphene oxide in hydrochloric acid
It is low, the impurity in solution can be preferably removed using common-ion effect, such as sulfate ion and metal ion.Therefore, use
The salt acid elution that concentration is 5% 10 times, and be centrifuged at a high speed, it can fast and effectively go the removal of impurity.
2nd, graphene oxide-ferroso-ferric oxide suspension is prepared
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, in order to ensure graphene oxide is not reunited,
Activity will not be impacted, it is necessary first to for adjusting the pH value of mixed solution so that pH value will not be too low, in the reality of the present invention
Apply in example, be adjusted using 12mol/L ammoniacal liquor.
Under nitrogen protection, by FeCl3And FeCl2Mixed solution is added in three-neck flask, adds appropriate amount of deionized water
After dilution, 0.8mL ammoniacal liquor is added, 100~115mL graphene oxide disperse systems is added afterwards, rapidly joins 40mL ammoniacal liquor, water
Bath is heated to 80 DEG C, after persistently stirring 3h, obtains graphene oxide/ferroso-ferric oxide suspension.In the present invention, add suitable
Deionized water dilution FeC13 and FeCl2 mixed solutions are measured, by being diluted to FeC13 and FeCl2 mixed solutions, are reduced
The concentration of FeC13 and FeCl2 mixed solutions, can be more uniform with graphene oxide disperse system by it in subsequent reactions
It is scattered；And in the environment of low concentration, slowing down whole course of reaction, the amorphous ferriferrous oxide particles formed are more equal
It is grown in evenly on graphene oxide.This step add ammoniacal liquor be because in the basic conditions, ferric ion and ferrous iron from
Son can generate ferroso-ferric oxide, and ferriferrous oxide particles are connected to above graphene oxide by the covalent effect with carboxyl, by
In the positioning action of carboxyl, the reunion of ferriferrous oxide particles is weakened.
The method of heating water bath is used to be carried for the co-precipitation step in situ of ferroso-ferric oxide crystalline forming and graphene oxide
It for corresponding conditionses, and will control in the reaction time at 3 hours, both can guarantee that the brilliant tool of graphene oxide-loaded ferriferrous oxide nano
There is excellent magnetic, and can ensures that it has good absorption property.
3rd, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
Finally 30h is freeze-dried again, it is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite.
Embodiment 1
The present embodiment provides a kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, including
Following steps：
S1, prepare graphene oxide disperse system
2g graphite powders and 1.2g sodium nitrate are placed in three-neck flask, add the 65mL concentrated sulfuric acids, with super after flask is sealed
Sound is scattered 15 minutes, then flask is placed in ice bath environment and stirred, and 8.8g potassium permanganate is slowly added in flask, in 2 DEG C of ice
Stirred 12 hours in bath environment；
75mL deionized waters are slowly added dropwise, then flask is placed in water-bath, by temperature adjustment to 60 DEG C and stirring reaction
12 hours, water-bath pot temperature is adjusted to 35 DEG C, continues reaction 12 hours；
22mL hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then with 5%
Hydrochloric acid washs under the conditions of 9000r/min high speed centrifugation, then continues washing to pH of mixed in neutrality with pure water, then use
Ultrasonication is scattered 4 hours, obtains graphene oxide disperse system；
S2, prepare graphene oxide-ferroso-ferric oxide suspension
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, under nitrogen protection, by FeCl3And FeCl2It is mixed
Close solution to be added in three-neck flask, after adding appropriate amount of deionized water dilution, and be added dropwise to 0.8mL ammoniacal liquor regulation pH, add
115mL graphene oxide disperse systems, rapidly join 40mL ammoniacal liquor, flask are placed in water-bath, by temperature adjustment to 80 DEG C；
After persistently stirring 3h, graphene oxide-ferroso-ferric oxide suspension is obtained.
S3, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
It is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite finally in freeze-drying 30h.
Embodiment 2
The present embodiment provides a kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, including
Following steps：
S1, prepare graphene oxide disperse system
2g graphite powders and 1.2g sodium nitrate are placed in three-neck flask, add the 65mL concentrated sulfuric acids, with super after flask is sealed
Sound is scattered 20 minutes, then flask is placed in ice bath environment and stirred, and 8.8g potassium permanganate is slowly added in flask, in 3 DEG C of ice
Stirred 10 hours in bath environment；
74mL deionized waters are slowly added dropwise, then flask is placed in water-bath, by temperature adjustment to 50 DEG C and stirring reaction
10 hours, water-bath pot temperature is adjusted to 35 DEG C, continues reaction 10 hours；
22mL hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then with 5%
Hydrochloric acid washs under the conditions of 9000r/min high speed centrifugation, then continues washing to pH of mixed in neutrality with pure water, then use
Ultrasonication is scattered 4 hours, obtains graphene oxide disperse system；
S2, prepare graphene oxide-ferroso-ferric oxide suspension
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, under nitrogen protection, by FeCl3And FeCl2It is mixed
Close solution to be added in three-neck flask, after adding appropriate amount of deionized water dilution, and be added dropwise to 0.8mL ammoniacal liquor regulation pH, add
110mL graphene oxide disperse systems, rapidly join 40mL ammoniacal liquor, flask are placed in water-bath, by temperature adjustment to 80 DEG C；
After persistently stirring 3h, graphene oxide-ferroso-ferric oxide suspension is obtained.
S3, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
It is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite finally in freeze-drying 30h.
Embodiment 3
The present embodiment provides a kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, including
Following steps：
S1, prepare graphene oxide disperse system
2g graphite powders and 1.2g sodium nitrate are placed in three-neck flask, add the 65mL concentrated sulfuric acids, with super after flask is sealed
Sound is scattered 25 minutes, then flask is placed in ice bath environment and stirred, and 8.8g potassium permanganate is slowly added in flask, in 3 DEG C of ice
Stirred 8 hours in bath environment；
73mL deionized waters are slowly added dropwise, then flask is placed in water-bath, by temperature adjustment to 55 DEG C and stirring reaction
8 hours, water-bath pot temperature is adjusted to 35 DEG C, continues reaction 8 hours；
22mL hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then with 5%
Hydrochloric acid washs under the conditions of 9000r/min high speed centrifugation, then continues washing to pH of mixed in neutrality with pure water, then use
Ultrasonication is scattered 4 hours, obtains graphene oxide disperse system；
S2, prepare graphene oxide-ferroso-ferric oxide suspension
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, under nitrogen protection, by FeCl3And FeCl2It is mixed
Close solution to be added in three-neck flask, after adding appropriate amount of deionized water dilution, and be added dropwise to 0.8mL ammoniacal liquor regulation pH, add
105mL graphene oxide disperse systems, rapidly join 40mL ammoniacal liquor, flask are placed in water-bath, by temperature adjustment to 80 DEG C；
After persistently stirring 3h, graphene oxide-ferroso-ferric oxide suspension is obtained.
S3, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
It is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite finally in freeze-drying 30h.
Embodiment 4
The present embodiment provides a kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, including
Following steps：
S1, prepare graphene oxide disperse system
2g graphite powders and 1.2g sodium nitrate are placed in three-neck flask, add the 65mL concentrated sulfuric acids, with super after flask is sealed
Sound is scattered 30 minutes, then flask is placed in ice bath environment and stirred, and 8.8g potassium permanganate is slowly added in flask, in 4 DEG C of ice
Stirred 10 hours in bath environment；
72mL deionized waters are slowly added dropwise, then flask is placed in water-bath, by temperature adjustment to 55 DEG C and stirring reaction
8 hours, water-bath pot temperature is adjusted to 35 DEG C, continues reaction 8 hours；
22mL hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then with 5%
Hydrochloric acid washs under the conditions of 9000r/min high speed centrifugation, then continues washing to pH of mixed in neutrality with pure water, then use
Ultrasonication is scattered 4 hours, obtains graphene oxide disperse system；
S2, prepare graphene oxide-ferroso-ferric oxide suspension
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, under nitrogen protection, by FeCl3And FeCl2It is mixed
Close solution to be added in three-neck flask, after adding appropriate amount of deionized water dilution, and be added dropwise to 0.8mL ammoniacal liquor regulation pH, add
105mL graphene oxide disperse systems, rapidly join 40mL ammoniacal liquor, flask are placed in water-bath, by temperature adjustment to 80 DEG C；
After persistently stirring 3h, graphene oxide-ferroso-ferric oxide suspension is obtained.
S3, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
It is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite finally in freeze-drying 30h.
Embodiment 5
The present embodiment provides a kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, including
Following steps：
S1, prepare graphene oxide disperse system
2g graphite powders and 1.2g sodium nitrate are placed in three-neck flask, add the 65mL concentrated sulfuric acids, with super after flask is sealed
Sound is scattered 35 minutes, then flask is placed in ice bath environment and stirred, and 8.8g potassium permanganate is slowly added in flask, in 5 DEG C of ice
Stirred 12 hours in bath environment；
71mL deionized waters are slowly added dropwise, then flask is placed in water-bath, by temperature adjustment to 60 DEG C and stirring reaction
10 hours, water-bath pot temperature is adjusted to 35 DEG C, continues reaction 10 hours；
22mL hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then with 5%
Hydrochloric acid washs under the conditions of 9000r/min high speed centrifugation, then continues washing to pH of mixed in neutrality with pure water, then use
Ultrasonication is scattered 4 hours, obtains graphene oxide disperse system；
S2, prepare graphene oxide-ferroso-ferric oxide suspension
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, under nitrogen protection, by FeCl3And FeCl2It is mixed
Close solution to be added in three-neck flask, after adding appropriate amount of deionized water dilution, and be added dropwise to 0.8mL ammoniacal liquor regulation pH, add
100mL graphene oxide disperse systems, rapidly join 40mL ammoniacal liquor, flask are placed in water-bath, by temperature adjustment to 80 DEG C；
After persistently stirring 3h, graphene oxide-ferroso-ferric oxide suspension is obtained.
S3, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
It is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite finally in freeze-drying 30h.
Embodiment 6
The present embodiment provides a kind of preparation method of graphene oxide-loaded ferriferrous oxide nano composite, including
Following steps：
S1, prepare graphene oxide disperse system
2g graphite powders and 1.2g sodium nitrate are placed in three-neck flask, add the 65mL concentrated sulfuric acids, with super after flask is sealed
Sound is scattered 40 minutes, then flask is placed in ice bath environment and stirred, and 8.8g potassium permanganate is slowly added in flask, in 5 DEG C of ice
Stirred 12 hours in bath environment；
70mL deionized waters are slowly added dropwise, then flask is placed in water-bath, by temperature adjustment to 60 DEG C and stirring reaction
12 hours, water-bath pot temperature is adjusted to 35 DEG C, continues reaction 10 hours；
22mL hydrogen peroxide is slowly dropped in flask, continues reaction 4 hours at a temperature of 35 DEG C of water-baths, then with 5%
Hydrochloric acid washs under the conditions of 9000r/min high speed centrifugation, then continues washing to pH of mixed in neutrality with pure water, then use
Ultrasonication is scattered 4 hours, obtains graphene oxide disperse system；
S2, prepare graphene oxide-ferroso-ferric oxide suspension
Prepare with 2:1 proportioning configuration FeCl3And FeCl2Mixed solution, under nitrogen protection, by FeCl3And FeCl2It is mixed
Close solution to be added in three-neck flask, after adding appropriate amount of deionized water dilution, and be added dropwise to 0.8mL ammoniacal liquor regulation pH, add
100mL graphene oxide disperse systems, rapidly join 40mL ammoniacal liquor, flask are placed in water-bath, by temperature adjustment to 80 DEG C；
After persistently stirring 3h, graphene oxide-ferroso-ferric oxide suspension is obtained.
S3, clean dry
After cooling down solution to room temperature, washed each 3 times by gained black precipitate Magneto separate and with deionized water and ethanol,
It is polished to obtain graphene oxide-loaded ferriferrous oxide nano composite finally in freeze-drying 30h.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made is any
Modification, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
- A kind of 1. preparation method of graphene oxide-loaded ferriferrous oxide nano composite, it is characterised in that the oxidation The preparation method of graphene-supported ferriferrous oxide nano composite includes：Prepare graphene oxide disperse system：Including graphite powder, sodium nitrate, the concentrated sulfuric acid and potassium permanganate are mixed in ice bath environment Close；Prepare graphene oxide-ferroso-ferric oxide suspension：It is included in addition Fe in the graphene oxide disperse system3+、Fe2+From Son, and mixed under alkaline environment.
- 2. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 1, it is special Sign is, in described the step of preparing graphene oxide disperse system, the graphite powder, the sodium nitrate and the concentrated sulfuric acid are first Mixing, then to mixed solution 15~40min of ultrasonic disperse, then mix with the potassium permanganate.
- 3. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 1, it is special Sign is that the ice bath temperature is 2~5 DEG C.
- 4. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 1, it is special Sign is that described the step of preparing graphene oxide disperse system also includes：To being mixed with the graphite powder, the sodium nitrate, the concentrated sulfuric acid and the potassium permanganate under ice bath environment One disperse system is diluted, and first set reaction is then carried out under water bath.
- 5. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 4, it is special Sign is that described the step of preparing graphene oxide disperse system also includes：First disperse system adds hydrogen peroxide after the first set reaction, is then carried out under water bath anti-for the second time Should.
- 6. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 5, it is special Sign is that described the step of preparing graphene oxide disperse system also includes：Second of reacted disperse system is washed to neutrality, recycles ultrasonic disperse.
- 7. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 1, it is special Sign is, in described the step of preparing graphene oxide-ferroso-ferric oxide suspension, the Fe3+、Fe2+Ion is with FeCl3With FeCl2The form of mixed solution mix with the graphene oxide disperse system, the Fe3+、Fe2+The mol ratio of ion is 2: 1。
- 8. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 7, it is special Sign is, the FeCl3And FeCl2Mixed solution before being mixed with the graphene oxide disperse system, first add alkaline solution Adjust pH value.
- 9. the preparation method of graphene oxide-loaded ferriferrous oxide nano composite according to claim 1, it is special Sign is that the preparation method of the graphene oxide-loaded ferriferrous oxide nano composite also includes：Clean dry：The sediment of the graphene oxide-ferroso-ferric oxide suspension is separated and removed, then carries out freezing and does It is dry.
- 10. a kind of graphene oxide-loaded ferriferrous oxide nano composite, it is characterised in that it passes through claim 1 to 9 Any one of the preparation method of graphene oxide-loaded ferriferrous oxide nano composite be made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711029754.XA CN107662949A (en) | 2017-10-27 | 2017-10-27 | A kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711029754.XA CN107662949A (en) | 2017-10-27 | 2017-10-27 | A kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107662949A true CN107662949A (en) | 2018-02-06 |
Family
ID=61144165
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711029754.XA Pending CN107662949A (en) | 2017-10-27 | 2017-10-27 | A kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107662949A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109248687A (en) * | 2018-10-08 | 2019-01-22 | 扬州工业职业技术学院 | A kind of novel graphene/ferroso-ferric oxide composite nano materials and its application in the dodecyl diacid list tert-butyl ester is prepared in catalysis |
| CN111847521A (en) * | 2020-07-08 | 2020-10-30 | 湖南科技大学 | Three-dimensional graphite alkyne/Fe3O4Preparation method and application of nano composite material |
| CN112246243A (en) * | 2020-10-20 | 2021-01-22 | 哈尔滨理工大学 | Preparation method of hydrophilic graphene/spinel type ferrite composite material |
| CN114939395A (en) * | 2022-05-05 | 2022-08-26 | 湖南艾布鲁环保科技股份有限公司 | Non-point source pollution adsorbent and preparation method and application thereof |
| CN115090277A (en) * | 2022-06-08 | 2022-09-23 | 台州学院 | Preparation of magnetic graphene oxide and adsorption application of magnetic graphene oxide to amide compounds |
| CN115810747A (en) * | 2022-12-21 | 2023-03-17 | 扬州工业职业技术学院 | Method for synthesizing ferroferric oxide and reducing graphene oxide through covalent bond coupling and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173189A (en) * | 2013-03-06 | 2013-06-26 | 西北工业大学 | Method for preparing reduced graphene oxide/ferroferric oxide nano-grade wave-absorbing materials |
| CN104673475A (en) * | 2015-02-16 | 2015-06-03 | 中北大学 | Graphene @Fe3O4 compound water base magnetorheological fluid and preparation method thereof |
| CN104877192A (en) * | 2015-06-03 | 2015-09-02 | 中北大学 | Fe3O4@GO/NR magnetic elastomer composite material and preparation method |
| CN106753237A (en) * | 2016-11-28 | 2017-05-31 | 深圳大学 | A kind of Graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof |
-
2017
- 2017-10-27 CN CN201711029754.XA patent/CN107662949A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103173189A (en) * | 2013-03-06 | 2013-06-26 | 西北工业大学 | Method for preparing reduced graphene oxide/ferroferric oxide nano-grade wave-absorbing materials |
| CN104673475A (en) * | 2015-02-16 | 2015-06-03 | 中北大学 | Graphene @Fe3O4 compound water base magnetorheological fluid and preparation method thereof |
| CN104877192A (en) * | 2015-06-03 | 2015-09-02 | 中北大学 | Fe3O4@GO/NR magnetic elastomer composite material and preparation method |
| CN106753237A (en) * | 2016-11-28 | 2017-05-31 | 深圳大学 | A kind of Graphene/ferroso-ferric oxide composite wave-suction material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘琼等: "Fe3O4纳米粒子-氧化石墨烯纳米复合物的制备、表征及体外毒性评价", 《中国医药工业杂志》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109248687A (en) * | 2018-10-08 | 2019-01-22 | 扬州工业职业技术学院 | A kind of novel graphene/ferroso-ferric oxide composite nano materials and its application in the dodecyl diacid list tert-butyl ester is prepared in catalysis |
| CN111847521A (en) * | 2020-07-08 | 2020-10-30 | 湖南科技大学 | Three-dimensional graphite alkyne/Fe3O4Preparation method and application of nano composite material |
| CN111847521B (en) * | 2020-07-08 | 2022-08-02 | 湖南科技大学 | Three-dimensional graphite alkyne/Fe 3 O 4 Preparation method and application of nano composite material |
| CN112246243A (en) * | 2020-10-20 | 2021-01-22 | 哈尔滨理工大学 | Preparation method of hydrophilic graphene/spinel type ferrite composite material |
| CN114939395A (en) * | 2022-05-05 | 2022-08-26 | 湖南艾布鲁环保科技股份有限公司 | Non-point source pollution adsorbent and preparation method and application thereof |
| CN114939395B (en) * | 2022-05-05 | 2023-10-13 | 湖南艾布鲁环保科技股份有限公司 | Non-point source pollution adsorbent and preparation method and application thereof |
| CN115090277A (en) * | 2022-06-08 | 2022-09-23 | 台州学院 | Preparation of magnetic graphene oxide and adsorption application of magnetic graphene oxide to amide compounds |
| CN115810747A (en) * | 2022-12-21 | 2023-03-17 | 扬州工业职业技术学院 | Method for synthesizing ferroferric oxide and reducing graphene oxide through covalent bond coupling and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107662949A (en) | A kind of graphene oxide-loaded ferriferrous oxide nano composite and preparation method thereof | |
| Esmaeili et al. | Modified single-phase hematite nanoparticles via a facile approach for large-scale synthesis | |
| Zhang et al. | Solvothermal synthesis of magnetic Fe3O4 microparticles via self-assembly of Fe3O4 nanoparticles | |
| CN109019656B (en) | Method for producing nano rare earth oxide powder | |
| Chen et al. | A microwave-triggered controllable drug delivery system based on hollow-mesoporous cobalt ferrite magnetic nanoparticles | |
| CN101599335B (en) | Oxidation resistant dimethyl silicon oil based magnetic fluid and preparation method thereof | |
| CN103157413B (en) | Method for preparing sodium alginate microcapsule-supported nanoscale zero-valent iron particles | |
| CN102633307A (en) | Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles | |
| CN104001474A (en) | Carbon-coated ferroferric oxide core-shell nano particle and preparation method thereof | |
| CN104058380B (en) | The preparation method of the elliposoidal ion doping type hydroxyapatite micro-sphere of porous surface | |
| CN105271431B (en) | Method for preparing ferriferrous oxide magnetic material and composite material thereof | |
| CN102557149B (en) | Method for preparing water-soluble nanometer iron oxide | |
| CN101723655A (en) | Preparation method of Mn-Zn ferrite cobalt-doped nano material | |
| CN104475132A (en) | Preparation method of flower-like BiOBr and application of flower-like BiOBr in rhodamine degradation reaction | |
| CN106216710A (en) | A kind of preparation method of high-tap density high-crystallinity silver powder | |
| Pan et al. | Constructing two-dimensional lamellar monometallic carbon nanocomposites by sodium chloride hard template for lightweight microwave scattering and absorption | |
| CN103469290A (en) | Synthesis method of superparamagnetic Fe3O4 nanocrystal | |
| Zhang et al. | Heterogeneous Fenton-like magnetic nanosphere coated with vanadium oxide quantum dots for enhanced organic dyes decolorization | |
| Zhao et al. | A general and facile method for improving carbon coat on magnetic nanoparticles with a thickness control | |
| CN106315684B (en) | The preparation method of the controllable spherical MnZn ferrite magnetic nano particle of size | |
| Wang et al. | Morphology-controlled synthesis and magnetic property of pseudocubic iron oxide nanoparticles | |
| CN102974285B (en) | Producing method of magnetic microsphere with hierarchical-pore structure and adjustable uniform grain size | |
| Gunatilake et al. | Ex situ and in situ magnetic phase synthesised magneto-driven alginate beads | |
| CN105950148A (en) | Preparation method for preparing ferroferric oxide hollow ball-based fluorescent magnetic composite material | |
| CN105948135B (en) | A kind of monodisperse porous magnetic sub-micro ball and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180206 |