CN107081128A - The method for preparing redox graphene/nano ferriferrous oxide composite magnetic adsorbent - Google Patents
The method for preparing redox graphene/nano ferriferrous oxide composite magnetic adsorbent Download PDFInfo
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- CN107081128A CN107081128A CN201710286765.XA CN201710286765A CN107081128A CN 107081128 A CN107081128 A CN 107081128A CN 201710286765 A CN201710286765 A CN 201710286765A CN 107081128 A CN107081128 A CN 107081128A
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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
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- 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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Abstract
The invention discloses a kind of method for preparing redox graphene/nano ferriferrous oxide composite magnetic adsorbent, its scheme is（1）Configure reactant system and be well mixed and obtain reactant mixed solution, the reactant system includes water/ethylene glycol binary solvent, graphene oxide, ferric chloride hexahydrate, sodium citrate and sodium acetate；（2）Using water/ethylene glycol, hot method prepares composite magnetic adsorbent altogether.The present invention is improved to traditional solvent-thermal method, using water and the hot method of ethylene glycol binary solvent, makes the rGO/Fe of preparation3O4With good magnetic response ability.
Description
Technical field
The invention belongs to sorbent material preparation field, redox graphene/nano ferriferrous oxide is specifically prepared
The method of composite magnetic adsorbent.
Background technology
Graphene is a kind of novel carbon material, with special two-dimensional structure, contains abundant and novel physical phenomenon,
Many excellent properties are shown, including electricity, optics, calorifics and mechanical property.As the research to graphene is more next
More deep, scientists think, graphene is expected to thoroughly change materials science field.The property of graphene is widely applied for it
Scope is laid a good foundation, and is expected in high-performance nano electronic device, composite, field emmision material, gas sensor and energy
The fields such as storage obtain extensive use.
Redox graphene（rGO）It is one of main derivative of graphene, refers to by the method such as chemically or thermally
Not exclusively remove a kind of two-dimentional carbon material obtained after the oxygen-containing functional group in graphene oxide.RGO physicochemical properties are situated between
Between graphene and graphene oxide, but structurally and functionally showing many unique advantages.As catalysis
The specific surface area bigger than graphene and GO and electro-chemical activity can be shown during carrier（Referring to Wang Zegao, graphene film with
The controllable preparation of redox graphene powder and Study of effects of doping,University of Electronic Science and Technology Ph.D. Dissertation, 2014）.Most
Recent studies on finds that rGO has excellent absorption property, is a kind of very promising sorbent material（Referring to Ding Wang
et.al, Pt Nanocatalysts Supported on Reduced Graphene Oxide for Selective
Conversion of Cellulose or Cellobiose to Sorbitol, ChemSusChem 2014, 7: 1398-
1406）.
Ferroso-ferric oxide（Fe3O4）Nanoparticle has good magnetic response ability, is a kind of adsorbent being commonly used
Carrier.Adsorbent and Fe3O4After compound, superparamagnetism is endowed, can be directly dispersing in aqueous phase and object is inhaled
It is attached, then separated using externally-applied magnetic field, not only simplify operation sequence, while adsorption efficiency is greatly improved.Therefore, it is various
Type rGO and nanometer Fe3O4Study hotspot of the preparation as adsorbent research field of composite magnetic adsorbent.
Solvent-thermal method is a kind of rGO/Fe commonly used at present3O4Preparation method.For example, soup Zhenhua etc. is with graphite oxide
And FeCl3For raw material, diethylene glycol is solvent, the rGO/Fe using a step solvent structure3O4Compound, and be applied to have
The absorption and detection of machine phosphorus insecticide（Referring to soup Zhenhua etc., ferroferric oxide/reduced graphene oxide synthesis and its in organophosphor agriculture
Application study during medicine inspection is surveyed,Food industry science and technology, 2014,35 (21): 306-309）；Qiu Xiaqin etc. with graphite oxide and
FeSO4For raw material, ethylene glycol is solvent, prepares rGO/Fe3O4Nano-complex and the absorption for being applied to pyrethrin pesticide in fruits and vegetables
With detection（Referring to Qiu Xiaqin etc., application study of the magnetic graphene nano-complex in the residual detection of chrysanthemum esters agriculture,Food industry Science and technology, 2016,37 (12): 76-79）.Solvent-thermal method prepares rGO/Fe3O4Have the advantages that it is simple to operate, be easily mastered, but
It is to exist to react uneven, the low problem of graphene oxide reduction efficiency, causes rGO/Fe3O4Composite structure unstability, enters
And influence magnetic response ability.This defect seriously hinders rGO/Fe3O4Preparation and application, it would be highly desirable to solve.
The content of the invention
The invention aims to overcome the shortcoming and defect that prior art is present, and provide a kind of operating procedure letter
The method for preparing redox graphene/nano ferriferrous oxide composite magnetic adsorbent of single, economic and environment-friendly, magnetic well.
To achieve the above object, the technical scheme is that to prepare redox graphene/nano ferriferrous oxide multiple
The method for closing magnetic adsorbent, comprises the following steps：
（1）Configure reactant system and be well mixed and obtain reactant mixed solution, the reactant system includes water/ethylene glycol
Binary solvent, graphene oxide, ferric chloride hexahydrate, sodium citrate and sodium acetate, wherein, water and ethylene glycol addition volume ratio are
1/5, the addition of graphene oxide and water/ethylene glycol binary solvent is compared for 3 mg/mL, and the quality of ferric chloride hexahydrate is oxidation stone
2-5 times of black alkene quality, ferric chloride hexahydrate, sodium citrate, sodium acetate three mass ratio are 1/0.4/3；
Reactant mixed solution is transferred in reactor；
（2）Using water/ethylene glycol, hot method prepares composite magnetic adsorbent altogether, reactor is placed in Muffle furnace, reaction temperature is
180-200 DEG C, the reaction time is 8-12 hours, and reaction product is fully cleaned and vacuum drying obtains reduction-oxidation after Magneto separate
Graphene/nanometer ferroso-ferric oxide composite magnetic adsorbent.
It is the step further to set（1）In reactant system by being thoroughly mixed and ultrasonic disperse 30 minutes
Method be well mixed.
It is the step further to set（2）In reaction product fully cleaned by ultra-pure water and ethanol.
The present invention is improved to traditional solvent-thermal method, using water and the hot method of ethylene glycol binary solvent, makes preparation
rGO/Fe3O4With good magnetic response ability.Referring specifically to the vibration magnetic strength in the embodiment of the present invention with accompanying drawing（VSM）Test
As a result.
The inventive method this use water and the hot method of ethylene glycol binary solvent（The hot method of conventional solvent is only with a kind of solvent）, carry
The high uniformity of reaction system, improves the reduction effect of GO and iron chloride, the yield of ferroso-ferric oxide is improved, therefore, production
Thing has good magnetic response ability.
Using the such scheme of the inventive method, the reduction effect of GO and iron chloride can be significantly improved, make its structure and
Performance is more stablized, and then greatly improves magnetic response ability, referring specifically to embodiment experimental data.In addition, the present invention uses water portion
Divide and instead of organic solvent, not only reduce financial cost, and it is more environmentally-friendly.
The present invention is described further with reference to specification drawings and specific embodiments.
Brief description of the drawings
The rGO/Fe that Fig. 1 preferred embodiment of the present invention and traditional preparation methods are obtained3O4VSM（Vibrate magnetic strength）Test knot
Fruit compares figure；
The rGO/Fe that Fig. 2 embodiment of the present invention 1 is prepared3O4VSM（Vibrate magnetic strength）Test result figure；
The rGO/Fe that Fig. 3 embodiment of the present invention 2 is prepared3O4VSM（Vibrate magnetic strength）Test result figure；
The rGO/Fe that Fig. 4 embodiment of the present invention 3 is prepared3O4VSM（Vibrate magnetic strength）Test result figure；
The rGO/Fe that Fig. 5 embodiment of the present invention 4 is prepared3O4VSM（Vibrate magnetic strength）Test result figure；
The rGO/Fe that Fig. 6 embodiment of the present invention 5 is prepared3O4VSM（Vibrate magnetic strength）Test result figure；
Fig. 7 preparation method schematic diagrams of the present invention.
Embodiment
The present invention is specifically described below by embodiment, is served only for that the present invention is further described, no
It is understood that for limiting the scope of the present invention, the technician in the field can be according to the content of foregoing invention to the present invention
Make some nonessential modifications and adaptations.
Preferred embodiment
RGO/Fe is prepared using this method method3O4（b）Condition：Solvent is 25 mL ethylene glycol and 5 mL water, GO 90
Mg, the mg of ferric chloride hexahydrate 260, the mg of sodium citrate 104, the mg of sodium acetate 796,180 DEG C of reaction temperature, reaction time 12
Hour；RGO/Fe is prepared using conventional method3O4（a）Condition：Solvent is 30 mL ethylene glycol, and remaining condition is with preparing rGO/
Fe3O4（b）Unanimously.
It is to give the rGO/Fe that the inventive method and traditional preparation methods are obtained referring to Fig. 13O4VSM（Vibrate magnetic strength）
Test result（Note：VSM is presently most used Magnetic Test method）.VSM results show, the rGO/ that conventional method is prepared
Fe3O4（a）Saturation magnetic intensity is only 11.7 emu/g；The present embodiment method prepares rGO/Fe3O4（b）Saturation magnetic intensity
28.1 emu/g, illustrate that this method significantly improves rGO/Fe3O4Magnetic response ability.
Actual Magneto separate experiment display, the rGO/Fe that conventional method is prepared3O4Separate 183 s (three average values, under
After together), supernatant still has obvious dark gray, shows that its separation is complete not yet；The present embodiment method prepares rGO/Fe3O4
It is 33 s the time required to separation to complete, and supernatant clear, colorless after separation illustrates rGO/Fe prepared by this method3O4In actual magnetic
There is more preferable effect in separation application.Magneto separate experimental implementation flow is as follows：20 mg rGO/Fe3O4It is dispersed in 20 mL
Water, uses surface magnetic intensity to be separated for the magnet of 0.4 tesla.
Embodiment 1
Prepare water/ethylene glycol binary solvent（25 mL ethylene glycol and 5 mL water）, sequentially add 97.5 mg GO, the water of 195 mg six
Close iron chloride（Quality is 2 times of GO）, 78 mg sodium citrates, 597 mg sodium acetates, be thoroughly mixed, 30 points of ultrasonic disperse
Clock, is transferred in reactor；Reactor is placed in Muffle furnace, reaction temperature is 180 DEG C, the reaction time is 8 hours；Reaction
After end, product is fully cleaned with ultra-pure water and ethanol, and vacuum drying obtains rGO/Fe after Magneto separate3O4。
VSM tests are carried out to preparing product, as a result as shown in Figure 2.From VSM results, rGO/Fe3O4Saturation magnetic strength
Spend for 9.5 emu/g.Actual Magneto separate experimental result shows, rGO/Fe3O4Time needed for being kept completely separate from the aqueous solution is
Supernatant is clarified after 147 s, separation.It these results suggest that rGO/Fe3O4Preparation work well, rGO/Fe3O4Structure and property
Can be stable, magnetic response is functional.
Embodiment 2
rGO/Fe3O4Experiment be the same as Example 1 is prepared, difference is the consumption of ferric chloride hexahydrate, sodium citrate, sodium acetate
Change：520 mg ferric chloride hexahydrates（Quality is 5 times of GO）, 208 mg sodium citrates, 1592 mg sodium acetates.
VSM tests are carried out to preparing product, as a result as shown in Figure 3.From VSM results, rGO/Fe3O4Saturation magnetic strength
Spend for 18.9 emu/g.Actual Magneto separate experimental result shows, rGO/Fe3O4Time needed for being kept completely separate from the aqueous solution is
Supernatant is clarified after 70 s, separation.It these results suggest that rGO/Fe3O4Preparation work well, rGO/Fe3O4Structure and property
Can be stable, magnetic response is functional.
Embodiment 3
rGO/Fe3O4Experiment be the same as Example 1 is prepared, difference is the consumption of ferric chloride hexahydrate, sodium citrate, sodium acetate
Change：260 mg ferric chloride hexahydrates（Quality is 2.5 times of GO）, 104 mg sodium citrates, 796 mg sodium acetates.
VSM tests are carried out to preparing product, as a result as shown in Figure 4.From VSM results, rGO/Fe3O4Saturation magnetic strength
Spend for 11.8 emu/g.Actual Magneto separate experimental result shows, rGO/Fe3O4Time needed for being kept completely separate from the aqueous solution is
Supernatant is clarified after 75 s, separation.It these results suggest that rGO/Fe3O4Preparation work well, rGO/Fe3O4Structure and property
Can be stable, magnetic response is functional.
Embodiment 4
rGO/Fe3O4Experiment be the same as Example 3 is prepared, difference is that reaction temperature changes, 200 DEG C are changed into from 180.
VSM tests are carried out to preparing product, as a result as shown in Figure 5.From VSM results, rGO/Fe3O4Saturation magnetic strength
Spend for 66.1 emu/g.Actual Magneto separate experimental result shows, rGO/Fe3O4Time needed for being kept completely separate from the aqueous solution is
Supernatant is clarified after 19 s, separation.It these results suggest that rGO/Fe3O4Preparation work well, rGO/Fe3O4Structure and property
Can be stable, magnetic response is functional.
Embodiment 5
rGO/Fe3O4Experiment be the same as Example 3 is prepared, difference is that the reaction time changes, was changed into from 8 hours 12 hours
℃。
VSM tests are carried out to preparing product, as a result as shown in Figure 6.From VSM results, rGO/Fe3O4Saturation magnetic strength
Spend for 28.1 emu/g.Actual Magneto separate experimental result shows, rGO/Fe3O4Time needed for being kept completely separate from the aqueous solution is
Supernatant is clarified after 33 s, separation.It these results suggest that rGO/Fe3O4Preparation work well, rGO/Fe3O4Structure and property
Can be stable, magnetic response is functional.
Claims (3)
1. a kind of method for preparing redox graphene/nano ferriferrous oxide composite magnetic adsorbent, it is characterised in that bag
Include following steps：
（1）Configure reactant system and be well mixed and obtain reactant mixed solution, the reactant system includes water/ethylene glycol
Binary solvent, graphene oxide, ferric chloride hexahydrate, sodium citrate and sodium acetate, wherein, water and ethylene glycol addition volume ratio are
1/5, the addition of graphene oxide and water/ethylene glycol binary solvent is compared for 3 mg/mL, and the quality of ferric chloride hexahydrate is oxidation stone
2-5 times of black alkene quality, ferric chloride hexahydrate, sodium citrate, sodium acetate three mass ratio are 1/0.4/3；
Reactant mixed solution is transferred in reactor；
（2）Using water/ethylene glycol, hot method prepares composite magnetic adsorbent altogether, reactor is placed in Muffle furnace, reaction temperature is
180-200 DEG C, the reaction time is 8-12 hours, and reaction product is fully cleaned and vacuum drying obtains reduction-oxidation after Magneto separate
Graphene/nanometer ferroso-ferric oxide composite magnetic adsorbent.
2. one kind according to claim 1 prepares redox graphene/nano ferriferrous oxide composite magnetic adsorbent
Method, it is characterised in that：The step（1）In reactant system by being thoroughly mixed and ultrasonic disperse 30 minutes
Method is well mixed.
3. one kind according to claim 1 prepares redox graphene/nano ferriferrous oxide composite magnetic adsorbent
Method, it is characterised in that：The step（2）In reaction product fully cleaned by ultra-pure water and ethanol.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165233A (en) * | 2017-12-12 | 2018-06-15 | 王景硕 | A kind of pavement snow melting agent and preparation method thereof |
| CN108837799A (en) * | 2018-06-05 | 2018-11-20 | 中国科学院兰州化学物理研究所 | It is a kind of can Magnetic Isolation ferroso-ferric oxide/phosphorylation graphene composite nano material and its application |
| CN108854962A (en) * | 2018-07-09 | 2018-11-23 | 内蒙古科技大学 | Heavy-metal adsorption material and the preparation method and application thereof based on magnetic oxygenated graphene |
| CN109317124A (en) * | 2018-11-13 | 2019-02-12 | 湖北文理学院 | A kind of three-dimensional grapheme magnetic stirring bar and its analysis application |
| CN109880122A (en) * | 2019-01-15 | 2019-06-14 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | A kind of supersonically preparation method of magnetic response graphene oxide hydrogel |
| CN110105919A (en) * | 2019-05-21 | 2019-08-09 | 中国工程物理研究院化工材料研究所 | A kind of extra small Fe3O4The supper-fast preparation method of low temperature of/RGO compound |
| CN114516632A (en) * | 2022-01-20 | 2022-05-20 | 安徽科技学院 | Three-dimensional magnetic reduced graphene and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165233A (en) * | 2017-12-12 | 2018-06-15 | 王景硕 | A kind of pavement snow melting agent and preparation method thereof |
| CN108837799A (en) * | 2018-06-05 | 2018-11-20 | 中国科学院兰州化学物理研究所 | It is a kind of can Magnetic Isolation ferroso-ferric oxide/phosphorylation graphene composite nano material and its application |
| CN108854962A (en) * | 2018-07-09 | 2018-11-23 | 内蒙古科技大学 | Heavy-metal adsorption material and the preparation method and application thereof based on magnetic oxygenated graphene |
| CN109317124A (en) * | 2018-11-13 | 2019-02-12 | 湖北文理学院 | A kind of three-dimensional grapheme magnetic stirring bar and its analysis application |
| CN109880122A (en) * | 2019-01-15 | 2019-06-14 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | A kind of supersonically preparation method of magnetic response graphene oxide hydrogel |
| CN110105919A (en) * | 2019-05-21 | 2019-08-09 | 中国工程物理研究院化工材料研究所 | A kind of extra small Fe3O4The supper-fast preparation method of low temperature of/RGO compound |
| CN110105919B (en) * | 2019-05-21 | 2022-02-22 | 中国工程物理研究院化工材料研究所 | Ultra-small Fe3O4Low-temperature ultra-fast preparation method of/RGO compound |
| CN114516632A (en) * | 2022-01-20 | 2022-05-20 | 安徽科技学院 | Three-dimensional magnetic reduced graphene and preparation method thereof |
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