CN105000886B - A kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation method - Google Patents

A kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation method Download PDF

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CN105000886B
CN105000886B CN201510405177.4A CN201510405177A CN105000886B CN 105000886 B CN105000886 B CN 105000886B CN 201510405177 A CN201510405177 A CN 201510405177A CN 105000886 B CN105000886 B CN 105000886B
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郑修成
孟婧珂
刘玉山
索阳
关新新
张建民
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Zhengzhou University
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Abstract

The invention belongs to technical field of function materials, it is related to a kind of macroscopic three dimensional ferroso-ferric oxide@graphene aerogels ultra light composite and preparation method.The present invention prepares graphene oxide first using expanded graphite powder as raw material, using improved Hummers methods, and ferric trichloride pyrohydrolysis is made into ferric hydroxide colloid；Then ferric hydroxide colloid is added drop-wise in graphene oxide solution under ultrasound, ferroso-ferric oxide@graphene hydrogels is obtained after hydrothermal reduction reaction；With acquisition macroscopic three dimensional ferroso-ferric oxide@graphene aerogel ultra light composites after ammoniacal liquor hydro-thermal process, vacuum freeze drying.In percentage by weight, ferroso-ferric oxide content is 0 65%, and surplus is graphene aerogel.The ferroso-ferric oxide doped graphene aerogel composite synthetic method that the present invention is provided is simple and easy to apply, easily controllable, proportion is small simultaneously, surface area is big and porous character is protruded, available for fields such as sewage disposal, stealthy, biological medicine, new energy and electronic materials.

Description

A kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation method
Technical field
The invention belongs to technical field of function materials, more particularly to a kind of macroscopic three dimensional Fe3O4@graphene aerogels are ultralight Composite and preparation method.
Background technology
It is used as the relatively early ferrite for being found and being used by the mankind, Fe3O4With properties such as unique magnetics and electricity, and make Preparation Method is relatively easy, chemical stability is good, is widely used as magnetic material, catalyst, abrasive material, sewage-treating agent, special electricity Pole etc..Graphene is a kind of new carbon material after fullerene, CNT, is sp2The carbon atom of hydridization is in six sides Arrangement forms sheet individual layer in lattice, possesses excellent electricity, machinery and chemical property.However, two-dimensional graphene is easily led to Cross parallel mode to stack, this just substantially reduces its specific surface area, conventional Fe3O4Class there is also the small grade of specific surface area not Foot.Based on three-dimensional netted and loose structure feature graphene aerogel（Graphene aerogel, GA）Can effectively it solve Reunion between graphene.Compared with graphene, GA is a kind of bigger serface, the adjustable large scale material of external morphology, table Reveal more excellent physicochemical properties.On the one hand, on sensor and catalytic applications can for ion and molecule diffusion and Electronics transport provides number of ways；On the other hand, its loose structure is the ideal stent of organic or inorganic nano material.Thus GA Sill has a wide range of applications.
At present, some reports on GA based composites, such as GA loads SnO are had2（CN 104143631 A）, nitrogen mixes Miscellaneous GA load Cs oOx（CN 104319395 A）, GA supported Vs2O5（CN 104437277 A）.But have no relevant macroscopic three dimensional Fe3O4 The report of doped graphene aeroge ultra light composite and preparation method, and by Fe3O4It is complex as having concurrently and can improves with GA The functional material of the two characteristic, there is potential in terms of sewage disposal, stealthy, biological medicine, new energy and electronic material Using.
The content of the invention
It is an object of the invention to provide a kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation side Method, described composite has concurrently and improves Fe3O4With the respective characteristic of graphene aerogel, current block ferrite material is solved The problems such as material specific surface area is small and graphene-based material is easily reunited.
To reach above-mentioned purpose, the technical solution adopted by the present invention is as follows：
A kind of macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites, by weight percentage Fe3O4Content For 0-65%, and it is not 0%, Fe3O4Content be preferably 25-55%, surplus is graphene aerogel.
Further, described a kind of macroscopic three dimensional Fe3O4The density of@graphene aerogel ultra light composites is 0.05- 0.10g/cm3, average pore size is that 3.00-7.00nm, total pore volume are 0.12-0.52cm3/ g, specific surface area are 180-400m2/g。
Further, described a kind of macroscopic three dimensional Fe3O4The macroscopic three dimensional structure of@graphene aerogel ultra light composites For column structure, diameter 1-3cm, height 2-7cm.
A kind of macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites, its preparation method comprises the following steps：
Step one, pretreating graphite powder：
First by concentrated nitric acid and the concentrated sulfuric acid by volume 1:(1-5), preferably 1:3 are mixed and made into mix acid liquor, in room Graphite powder is put into mix acid liquor under temperature, (5-12) part graphite powder is put into according to 100 parts of mix acid liquors, 16-32h is stirred, it is excellent Elect 100 parts of mix acid liquors as and be put into 10 parts of graphite powders, stir 24h, then diluted with high purity water；It it is again 0.45 μm with filter sizes Filter cake is made to pH=7 in the glass core filter filtering and washing of micropore, by gained filter cake in dry 1-3 at 50-70 DEG C My god, dried 2 days at preferably 60 DEG C；Filter cake is ground after 950-1150 DEG C of calcination process 10-50s, preferably 1100 DEG C again 30s is handled, that is, pretreating graphite powder is made；
Step 2, prepares graphene oxide solution
Using pretreating graphite powder made from step one as raw material, graphite oxide is first prepared using traditional Hummer methods molten Liquid, is then peeled off with ultrasound and graphene oxide solution is made again；
Step 3, prepares Fe (OH)3Colloid
At room temperature, according to 1 part of FeCl3·6H2O is dissolved in 1-8 parts of high purity waters, preferably 5 parts meters, by FeCl3·6H2O is dissolved in In high purity water, FeCl is obtained3The aqueous solution；Again by FeCl3The aqueous solution is added dropwise in the water of 30 parts of boilings, keeps solution boiling 1- The preferred 2min of 4min, that is, be made Fe (OH)3Colloid；
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
1. it is preferably 2.0mg/ with graphene oxide solution made from high purity water dilution step two to 1.0-4.0mg/mL ML, it is preferably pH=9 that its pH value is adjusted with ammoniacal liquor to 8-10, and dilution graphene oxide solution is made；
2. at room temperature by Fe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide solution In, control Fe (OH)3With diluting the mass ratio of graphene oxide solution for (0-3):1 is preferably 1:1, and stir 0.5-3h Preferably 1h, is made reaction solution；
3. it 2. obtained reaction solution will move into water heating kettle, 15-30h, preferably 180 are stood under the conditions of 150-220 DEG C 24h is stood under the conditions of DEG C, then water heating kettle is cooled to room temperature and produces Fe2O3@graphene hydrogels；
4. by obtained Fe2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 5-20% volume basis, are preferably 10%, the hydro-thermal process 1-5h at 80-130 DEG C, hydro-thermal process 3h at preferably 120 DEG C；
5. the Fe treated in 4.2O3@graphenes hydrogel is in subzero 48~subzero 58 DEG C, pressure 5~30Pa conditions Under, preferably subzero 53 DEG C, pressure 10Pa, cold drying Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 700-900 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 3-8h, preferably To be calcined 5h at 800 DEG C, the macroscopic three dimensional Fe is produced3O4@graphene aerogel ultra light composites.
Beneficial effect：
1st, the present invention relates to a kind of macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites, mainly solve block Fe3O4Surface area per unit volume accumulates the problem of small and graphene-based material is easily reunited.In its preparation, the present invention is used with FeCl3·6H2O The Fe (OH) prepared for raw material3Colloid is Fe3O4Predecessor, is added on using pretreating graphite powder as raw material, using traditional In graphene oxide solution prepared by Hummer methods, obtained using hydrothermal reduction method combination ammoniacal liquor hydro-thermal process and cold dry technology. Reaction condition is relatively mild, prepares fairly simple, it is easy to accomplish relatively large production.
2nd, macroscopic three dimensional Fe provided by the present invention3O4@graphene aerogel ultra light composites, while having concurrently and improving The characteristic of ferroso-ferric oxide and graphene aerogel, can be used as organic dyestuff sewage and adsorbent for heavy metal, super capacitor And electrode material of lithium battery, absorbing material, biological agent material etc..
Brief description of the drawings
Fig. 1（a）、（b）Respectively Fe (OH)3It is 1 with graphene oxide rate of charge:1 and 1:1.5 and in High Purity Nitrogen Fe obtained by 800 DEG C of roasting 5h in atmosphere is enclosed3O4The photo in kind of@graphene aerogel composites, it can be seen that be combined Material is macroscopical columnar three-dimensional structure；
Fig. 2 is made graphene oxide, graphene aerogel, Fe2O3And Fe (OH)3It is 1 with graphene oxide rate of charge :The Fe obtained under the conditions of 12O3@graphene aerogels and by its high pure nitrogen atmosphere 800 DEG C roasting 5h obtained by Fe3O4@graphite The XRD spectra of alkene aerogel composite, it can be seen that graphene oxide more thoroughly is converted into by hydrothermal reduction process Graphene, and Fe after high-temperature process2O3It is reduced to Fe3O4；
Fig. 3（a）、（b）Respectively Fe (OH)3It is 1 with graphene oxide rate of charge:1st, 800 DEG C in high pure nitrogen atmosphere It is calcined Fe obtained by 5h3O4The SEM photograph of@graphene aerogel composites, it can be seen that Fe3O4It is homogeneously dispersed in graphene In aeroge framework；
Fig. 4 is graphene aerogel and Fe (OH)3It is 1 with graphene oxide rate of charge:1st, 800 in high pure nitrogen atmosphere DEG C roasting 5h obtained by Fe3O4The Raman spectrum of@graphene aerogel materials, it can be seen that iron species draws during hydrothermal reduction Enter not significantly affect the reduction of graphene oxide；
Fig. 5 is Fe (OH)3It is 1 with graphene oxide rate of charge:1st, in high pure nitrogen atmosphere obtained by 800 DEG C of roasting 5h Fe3O4Nitrogen adsorption-desorption isotherm and corresponding texture parameter of the@graphene aerogels composite at -196 DEG C（Insertion）, It can be seen that the composite shows typical mesoporous material isotherm characteristic, average pore size about 5.00nm.
Embodiment
The present invention is expanded on further with reference to specific embodiment：
Embodiment 1
Step one, pretreating graphite powder
Under the conditions of room temperature, magnetic agitation, 35 g graphite powders are added on to the mix acid liquor of 520mL concentrated nitric acids and the concentrated sulfuric acid（1 : 3）And stir 24h.Increase pure water and be diluted to 1.5L, then taken out with filter sizes for the glass core filter of 0.45 μm of micropore Filter washing is to neutrality（pH = 7）, filter cake is made, gained filter cake is ground after being dried 2 days at 60 DEG C, and in batches in 1100 DEG C Processing 30s is that pretreating graphite powder is made.
Step 2, prepares graphene oxide solution
The pretreating graphite powder obtained is made as raw material using step one, graphite oxide is prepared using traditional Hummer methods molten Liquid, is then peeled off with ultrasound and graphene oxide solution is made, concentration is about 4.0mg/mL again.
Step 3, prepares ferric hydroxide colloid
At room temperature, 1gFeCl3·6H2O is dissolved in 5mL high purity waters, obtains FeCl3The aqueous solution；Again by FeCl3The aqueous solution In the water for being added dropwise to 25mL boilings, solution boiling 2min is kept, that is, ferric hydroxide colloid is made；Concentration is about 33.3mg/mL.
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
Fe(OH)3It is 0.5 with graphene oxide mass ratio:1,
1. take graphene oxide solution 15mL made from step 2 to be diluted with 15mL high purity waters, then used under magnetic agitation Ammoniacal liquor adjusts its pH=9, is then sonicated 1h, and dilution graphene oxide solution is made；
2. at room temperature by 0.8mLFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide In solution, and stir 1h reaction solution is made；
3. it 2. obtained reaction solution will move into 50mL water heating kettles, 24h is stood under the conditions of 180 DEG C；Then by water heating kettle It is cooled to room temperature and produces Fe2O3@graphene hydrogels；
4. by the Fe of acquisition2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, the water at 120 DEG C It is heat-treated 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is cold drying under the conditions of subzero 53 DEG C, pressure 10Pa Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, are produced described grand See three-dimensional Fe3O4@graphene aerogel ultra light composite composites.
Embodiment 2
Step one is to step 3 be the same as Example 1.
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
Fe(OH)3Mass ratio with graphene oxide is 1:1,
1. take graphene oxide solution 15mL made from step 2 to be diluted with 15mL high purity waters, then used under magnetic agitation Ammoniacal liquor adjusts its pH=9, is then sonicated 1h, and dilution graphene oxide solution is made；
2. at room temperature by 1.8mLFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide In solution, and stir 1h reaction solution is made；
3. it 2. obtained reaction solution will move into 50mL water heating kettles, 24h is stood under the conditions of 180 DEG C；Then by water heating kettle It is cooled to room temperature and produces Fe2O3@graphene hydrogels；
4. by the Fe of acquisition2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, the water at 120 DEG C It is heat-treated 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is cold drying under the conditions of subzero 53 DEG C, pressure 10Pa Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, are produced described grand See three-dimensional Fe3O4@graphene aerogel ultra light composite composites.
Embodiment 3
Step one is to step 3 be the same as Example 1.
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
Fe(OH)3Mass ratio with graphene oxide is 1.5:1,
1. take graphene oxide solution 15mL made from step 2 to be diluted with 15mL high purity waters, then used under magnetic agitation Ammoniacal liquor adjusts its pH=9, is then sonicated 1h, and dilution graphene oxide solution is made；
2. at room temperature by 2.7mLFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide In solution, and stir 1h；
3. it 2. obtained reaction solution will move into 50mL water heating kettles, 24h is stood under the conditions of 180 DEG C；Then by water heating kettle It is cooled to room temperature and produces Fe2O3@graphene hydrogels；
4. by the Fe of acquisition2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, the water at 120 DEG C It is heat-treated 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is cold drying under the conditions of subzero 53 DEG C, pressure 10Pa Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, are produced described grand See three-dimensional Fe3O4@graphene aerogel ultra light composite composites.
Embodiment 4
Step one is to step 3 be the same as Example 1.
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
Fe(OH)3It is 2 with graphene oxide mass ratio:1,
1. take graphene oxide solution 15mL made from step 2 to be diluted with 15mL high purity waters, then used under magnetic agitation Ammoniacal liquor adjusts its pH=9, is then sonicated 1h, and dilution graphene oxide solution is made；
2. at room temperature by 3.6mLFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide In solution, and 1h is stirred, reaction solution is made；
3. it 2. obtained reaction solution will move into 50mL water heating kettles, 24h is stood under the conditions of 180 DEG C；Then by water heating kettle It is cooled to room temperature and produces Fe2O3@graphene hydrogels,
4. by the Fe of acquisition2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, the water at 120 DEG C It is heat-treated 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is cold drying under the conditions of subzero 53 DEG C, pressure 10Pa Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, are produced described grand See three-dimensional Fe3O4@graphene aerogel ultra light composite composites.
Embodiment 5
Step one is to step 3 be the same as Example 1.
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
Fe(OH)3It is 2.5 with graphene oxide mass ratio:1,
1. take graphene oxide solution 15mL made from step 2 to be diluted with 15mL high purity waters, then used under magnetic agitation Ammoniacal liquor adjusts its pH=9, is then sonicated 1h, and dilution graphene oxide solution is made；
2. at room temperature by 4.5mLFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide In solution, and stir 1h；
3. it 2. obtained reaction solution will move into 50mL water heating kettles, 24h is stood under the conditions of 180 DEG C；Then by water heating kettle It is cooled to room temperature and produces Fe2O3@graphene hydrogels；
4. by obtained Fe2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, the water at 120 DEG C It is heat-treated 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is cold drying under the conditions of subzero 53 DEG C, pressure 10Pa Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, are produced described grand See three-dimensional Fe3O4@graphene aerogel ultra light composite composites.
Embodiment 6
Step one is to step 3 embodiment 1.
Step 4, prepares macroscopic three dimensional Fe3O4@graphene aerogel ultra light composites：
Fe(OH)3It is 3 with graphene oxide mass ratio:1,
1. take graphene oxide solution 15mL made from step 2 to be diluted with 15mL high purity waters, then used under magnetic agitation Ammoniacal liquor adjusts its pH=9, is then sonicated 1h, and dilution graphene oxide solution is made；
2. at room temperature by 5.4mLFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide In solution, and 1h is stirred, reaction solution is made；
3. it 2. obtained reaction solution will move into 50mL water heating kettles, 24h is stood under the conditions of 180 DEG C；Then by water heating kettle It is cooled to room temperature and produces Fe2O3@graphene hydrogels；
4. by obtained Fe2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, the water at 120 DEG C It is heat-treated 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is cold drying under the conditions of subzero 53 DEG C, pressure 10Pa Fe2O3@graphene aerogels；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, are produced described grand See three-dimensional Fe3O4@graphene aerogel ultra light composite composites.
Although above the present invention is described in detail with a general description of the specific embodiments, On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.

Claims (1)

1. a kind of macroscopic three dimensional Fe3O4The preparation method of@graphene aerogel ultra light composites, it is characterised in that described system Preparation Method comprises the following steps：
Step one, pretreating graphite powder
Under the conditions of room temperature, magnetic agitation, 35g graphite powders are added on 520ml concentrated nitric acids: concentrated sulfuric acid volume ratio is 1: 3 mixing In acid solution and 24h is stirred, increase pure water and be diluted to 1.5L, then with the glass core filter that filter sizes are 0.45 μm of micropore Filter cake is made to pH=7 in filtering and washing, is ground after gained filter cake is dried 2 days under the conditions of 60 DEG C, and in batches in 1100 DEG C Processing 30s is that pretreating graphite powder is made；
Step 2, prepares graphene oxide solution
The pretreating graphite powder obtained is made as raw material using step one, graphite oxide solution is prepared using traditional Hummer methods, so Peeled off again with ultrasound afterwards and graphene oxide solution is made, concentration is 4.0mg/ml；
Step 3, prepares ferric hydroxide colloid
At room temperature, 1gFeCl3·6H2O is dissolved in 5ml high purity waters, obtains FeCl3The aqueous solution, then by FeCl3The aqueous solution is added dropwise to In the water of 25ml boilings, solution boiling 2min is kept, that is, the ferric hydroxide colloid that concentration is 33.3mg/ml is made；
Step 4, prepares Fe (OH)3With the macroscopic three dimensional Fe that graphene oxide mass ratio is 0.5: 13O4@graphene aerogels surpass Light composite：
1. take graphene oxide solution 15ml made from step 2 to be diluted with 15ml high purity waters, then use ammoniacal liquor under magnetic agitation Its pH=9 is adjusted, 1h is then sonicated, dilution graphene oxide solution is made；
2. at room temperature by 0.8mlFe made from step 3 (OH)3Colloid is added drop-wise to 1. obtained dilution graphene oxide solution In, and stir 1h reaction solution is made；
3. it 2. obtained reaction solution will move into 50ml water heating kettles, 24h is stood under the conditions of 180 DEG C；Then water heating kettle is cooled down Fe is produced to room temperature2O3@graphene hydrogels；
4. by the Fe of acquisition2O3@graphene hydrogels are moved in the ammoniacal liquor that concentration is 10% volume basis, at 120 DEG C at hydro-thermal Manage 3h；
5. the Fe treated in 4.2O3@graphenes hydrogel is under the conditions of subzero 53 DEG C, pressure 10Pa, cold drying Fe2O3@ Graphene aerogel；
6. 5. obtained Fe is calcined under the conditions of 800 DEG C, High Purity Nitrogen atmosphere2O3@graphene aerogel 5h, produce described macroscopical three Tie up Fe3O4@graphene aerogel ultra light composite composites.
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