CN109569515A - A kind of preparation method of magnetic oxygenated graphene - Google Patents
A kind of preparation method of magnetic oxygenated graphene Download PDFInfo
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- CN109569515A CN109569515A CN201811590869.0A CN201811590869A CN109569515A CN 109569515 A CN109569515 A CN 109569515A CN 201811590869 A CN201811590869 A CN 201811590869A CN 109569515 A CN109569515 A CN 109569515A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Hydrology & Water Resources (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of magnetic oxygenated graphene, this method disperses deionized water for graphene oxide, FeCl is then added3And FeCl2, it is uniformly mixed, and with ammonium hydroxide or sodium hydroxide regulation system pH=9~11, is again heated to 60~100 DEG C and reflects 3~6 hours, obtain magnetic oxygenated graphene.Preparation method of the present invention is simple, low energy consumption, it is easy to accomplish industrialization improves magnetic graphene production efficiency, reduce production cost, and the magnetic oxygenated graphene large specific surface area of preparation, adsorption capacity is strong, can effectively remove the heavy metal ion in sewage, performance is stablized, it is easy to be separated by solid-liquid separation, the rate of recovery is good, and product is nontoxic environmental-friendly.
Description
Technical field
The invention belongs to adsorbent material technical fields, and in particular to a kind of preparation method of magnetic oxygenated graphene.
Background technique
Heavy metal ion, which is often stored in, to be difficult to decompose in water body environment, is the important sources of composing environment pollution, a processing huge sum of money
There are many technology of category, and wherein absorption method was widely used because of the advantages that its is at low cost, easy to operate, high-efficient.Adsorption effect
The excellent selection for depending primarily on adsorbent material, i.e. key technology.Adsorbent adsorbs heavy metal, and adsorption mechanism depends primarily on
Functional group on adsorbent, such as carboxyl, phosphate, sulfonic group and quaternary ammonium salt group, it is main to pass through an ion exchange adsorption huge sum of money
Belong to；Mainly by the way that chemisorption occurs with the complexing of heavy metal, amino by complexing but also can not only pass through carboxyl etc.
Electrostatic attraction adsorbs zwitterion heavy metal.Surface of graphene oxide contains a large amount of carboxyl, hydroxyl, carbonyl and epoxy group, institute
With the mechanism of the heavy metals such as magnetic oxygenated graphene absorption cadmium mainly has ion exchange, electrostatic attraction and complexing.And it aoxidizes
Graphene shows good performance for adsorbing heavy metal ion, but the disadvantage is that be difficult to separate, is unfavorable for recycling.Needle
To this problem, this research loads ferroferric oxide magnetic nano-particles using graphene oxide as matrix, by coprecipitation
To its surface, magnetic oxygenated graphene composite material (MGO) is prepared.
In recent years, magnetic adsorbent had become surrounding purifying material of new generation, because Magneto separate merely relates to apply outside
Adsorbent is extracted in magnetic field.It is compared with traditional method, such as filtering, centrifugation with Gravity Separation, Magneto separate needs less energy
Amount.Therefore it is to provide by the nanocomposite of the graphene combined with magnetite nanometric particles and overcomes relevant to graphite point
Effective ways from problem.
But the preparation process of magnetic oxygenated graphene is many and diverse in the prior art, and the adsorption capacity of prepared adsorbent needs
It improves, the rate of adsorption needs to be accelerated, and the technologies such as large-scale serial production are recycled and reused and be not suitable for there are adsorbent
Problem.
Summary of the invention
It is easy to operate quickly that the object of the present invention is to provide one kind, and preparation process requires low, low energy consumption, and Large ratio surface
The preparation method of long-pending, strong adsorption capacity, stability and the good magnetic oxygenated graphene of the rate of recovery,
For above-mentioned purpose, the technical scheme adopted by the invention is that: deionized water is dispersed by graphene oxide, then
FeCl is added3And FeCl2, it is uniformly mixed, and with ammonium hydroxide or sodium hydroxide regulation system pH=9~11, it is again heated to 60~
It 100 DEG C, stirs 3~6 hours, is cooled to room temperature, is filtered, washed, dries, obtain magnetic oxygenated graphene.
In above-mentioned preparation method, preferably the mass volume ratio of graphene oxide and deionized water is 1mg:0.5~2mL.
In above-mentioned preparation method, preferably graphene oxide and FeCl2Mass ratio be 1:1~3.
In above-mentioned preparation method, preferably FeCl2And FeCl3Molar ratio be 1:2~4.5.
In above-mentioned preparation method, the heating stirring 4h further preferably at 70~90 DEG C.
Beneficial effects of the present invention are as follows:
The present invention is simple, low energy consumption, and the magnetic oxygenated graphene large specific surface area prepared, and adsorption capacity is strong, the present invention
Preparation method is easy to operate, and preparation process requires low, low energy consumption, and preparation speed is fast, it is easy to accomplish industrialization, and improve magnetism
Graphene production efficiency, reduces production cost.The magnetic oxygenated graphene large specific surface area of the method for the present invention preparation, adsorption energy
Power is strong, can effectively remove the heavy metal ion in sewage, and performance is stablized, is easy to be separated by solid-liquid separation, the rate of recovery is good, the nontoxic nothing of product
It is harmful, environmental-friendly.
Detailed description of the invention
Fig. 1 is graphene oxide field emission scanning electron microscope figure.
Fig. 2 is the field emission scanning electron microscope figure of magnetic oxygenated graphene prepared by embodiment 1.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
400mL deionized water is added in 1g graphene oxide (GO), ultrasonic disperse 10min obtains GO suspension；By 25mL
Containing 3.24g (20mmol) FeCl3With 1.27g (10mmol) FeCl2Mixed aqueous solution be slowly added into GO suspension, and
It instills the ammonium hydroxide that mass fraction is 30% and adjusts pH value of solution=9, heated solution is to 70 DEG C, and after persistently stirring 3 hours, color becomes
Black is cooled to room temperature.Dark solution is filtered, is obtained magnetic oxygenated with deionized water and ethanol wash finally in 70 DEG C of dryings
Graphene.
Fig. 1 shows that graphene oxide is the sheet two-dimensional structure nano material with smooth surface, surface there are many fold,
Specific surface area can be increased, be conducive to magnetic particle load on the surface thereof with increase adsorption capacity.It can clearly be seen by Fig. 2
It arrives, white particles that there are many surface of graphene oxide show that magnetic nano-particle has succeeded here it is iron oxide particle
It has been supported on surface of graphene oxide.
Embodiment 2
400mL deionized water is added in 0.5g GO, ultrasonic disperse 10min obtains GO suspension；25mL is contained into 3.24g
(20mmol)FeCl3With 1.27g (10mmol) FeCl2Mixed aqueous solution be slowly added into GO suspension, and instill quality
The ammonium hydroxide that score is 30% adjusts pH value of solution=11, and heated solution is to 80 DEG C, and after persistently stirring 5 hours, color becomes black, cold
But to room temperature.Dark solution is filtered, obtains magnetic oxygenated graphene finally in 70 DEG C of dryings with deionized water and ethanol wash.
Embodiment 3
400mL deionized water is added in 0.7g graphene oxide, ultrasonic disperse 10min obtains GO suspension；25mL is contained
3.24g(20mmol)FeCl3With 1.27g (10mmol) FeCl2Mixed aqueous solution be slowly added into GO suspension, and drip
Enter the ammonium hydroxide that mass fraction is 30% and adjust pH value of solution=10, heated solution is to 90 DEG C, and after persistently stirring 4 hours, color becomes
Black is cooled to room temperature.Dark solution is filtered, is obtained magnetic oxygenated with deionized water and ethanol wash finally in 70 DEG C of dryings
Graphene.
Claims (5)
1. a kind of preparation method of magnetic oxygenated graphene, it is characterised in that: disperse deionized water for graphene oxide, then
FeCl is added3And FeCl2, it is uniformly mixed, and with ammonium hydroxide or sodium hydroxide regulation system pH=9~11, it is again heated to 60~
It 100 DEG C, stirs 3~6 hours, is cooled to room temperature, is filtered, washed, dries, obtain magnetic oxygenated graphene.
2. the preparation method of magnetic oxygenated graphene according to claim 1, it is characterised in that: the graphene oxide with
The mass volume ratio of deionized water is 1mg:0.5~2mL.
3. the preparation method of magnetic oxygenated graphene according to claim 1 or 2, it is characterised in that: the graphite oxide
Alkene and FeCl2Mass ratio be 1:1~3.
4. the preparation method of magnetic oxygenated graphene according to claim 3, it is characterised in that: the FeCl2And FeCl3
Molar ratio be 1:2~4.5.
5. the preparation method of magnetic oxygenated graphene according to claim 1, it is characterised in that: heated at 70~90 DEG C
Stir 4h.
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| CN201811590869.0A CN109569515A (en) | 2018-12-25 | 2018-12-25 | A kind of preparation method of magnetic oxygenated graphene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045123A (en) * | 2014-07-10 | 2014-09-17 | 湖南大学 | Method for removing divalent cadmium in wastewater by using carboxylated magnetic graphene oxide |
| CN104724787A (en) * | 2015-03-23 | 2015-06-24 | 湖南大学 | Method for removing hexavalent chromium in wastewater by using cyclohexane diamine-tetracetic acid modified magnetic graphene oxide |
| CN104923161A (en) * | 2015-07-09 | 2015-09-23 | 山东大学 | Preparation method of magnetic graphene oxide and application thereof |
| CN106902739A (en) * | 2017-03-13 | 2017-06-30 | 浙江大学 | A kind of preparation method and application of magnetic oxygenated Graphene |
-
2018
- 2018-12-25 CN CN201811590869.0A patent/CN109569515A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045123A (en) * | 2014-07-10 | 2014-09-17 | 湖南大学 | Method for removing divalent cadmium in wastewater by using carboxylated magnetic graphene oxide |
| CN104724787A (en) * | 2015-03-23 | 2015-06-24 | 湖南大学 | Method for removing hexavalent chromium in wastewater by using cyclohexane diamine-tetracetic acid modified magnetic graphene oxide |
| CN104923161A (en) * | 2015-07-09 | 2015-09-23 | 山东大学 | Preparation method of magnetic graphene oxide and application thereof |
| CN106902739A (en) * | 2017-03-13 | 2017-06-30 | 浙江大学 | A kind of preparation method and application of magnetic oxygenated Graphene |
Non-Patent Citations (1)
| Title |
|---|
| 陈黄豪等: ""磁性氧化石墨烯对水中镍的吸附研究"", 《材料科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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