CN103977748B - A kind of magnetic aeroge and preparation method thereof - Google Patents
A kind of magnetic aeroge and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of magnetic aerogel material and preparation method thereof, be carrier loaded ferroferric oxide magnetic nano-particles with graphene oxide, take CNT as skeleton or strengthen its morphological stability by calcium ion crosslinking effect, obtain graphene oxide magnetic aeroge through freeze drying, Graphene magnetic aeroge can be obtained further by electronation.Gained aerogel material is on the basis keeping tri-iron tetroxide magnetic effect, the advantage having had more that density is low, intensity is large, high temperature resistant, specific area is large standby, design feature determines it and has superpower adsorption capacity, absorbing property and electric conductivity, can be applicable to the fields such as sewage disposal, target administration, absorbing material, photoelectric material, is a kind of novel functional magnetic material.
Description
Technical field
The present invention relates to a kind of magnetic aerogel material and preparation method thereof, belong to technical field of function materials.
Background technology
Magnetic porous material can be used for the fields such as sewage disposal, target administration, microwave absorption (as: radar absorbing material), and Research Significance is large, is subject to extensive concern.The feature that above application all requires respective material to possess, and density is low, specific area large, high adsorption capacity, delivered payload capability are strong, good magnetic property be then meet that material easily reclaims, target ability is strong, realize the necessary requirement of microwave absorption, and current material is often difficult to meet many-sided performance requirement simultaneously.For absorbing material, because it is to the high request of electromagnetic property, tri-iron tetroxide one of main component being still absorbing material so far that magnetic property is good, absorbing material is completely many to be made up of single ferrite, ferrite mostly is the coating material existed with the form such as powder and particle, although with low cost, technique is simple, but it is light to be difficult to meet quality, absorption band is wide waits requirement, and greatly easily cause under poor high temperature stability and hot environment and the shortcoming such as absorbing property difference in high band range because of its density, its application in the specific environments such as aircraft is caused to be very restricted.Equally, in the field such as sewage disposal and target administration, the porous magnetic material of light weight is easier to reclaim, easily realize target control.Therefore, overcoming this defect to meet multi-field application demand, needing to prepare low-density, bigger serface, high strength and resistant to elevated temperatures magnetic material to satisfy the demands.
Aerogel material is a kind of novel porous material, and have the character of the multiple uniquenesses such as specific density is low, refractive index is low, porosity is high, surface area is large, adsorptivity is strong, multiple research field is widely used.Graphene oxide is a kind of monolayer carbon atom two-dimension nano materials that native graphite obtains after chemical oxidation and stripping, its flakiness ratio is up to 1000, specific area is large, mechanical strength is high, surface and edge random distribution a large amount of oxy radical (in the middle of lamella :-OH, C-O-C, edge :-C=O,-COOH), have amphipathic, present hydrophilic to hydrophobic property distribution from chip edge to central authorities, demonstrate good wettability and surface-active, and in water, show superior dispersiveness, become after Graphene more to show excellent electric conductivity through electronation, these features are all the reasons that it is widely used in composite and prepares.CNT can be regarded that graphene sheet layer is curling as and form, and can be divided into: SWCN and multi-walled carbon nano-tubes according to the number of plies of graphene film.Because carbon atom in CNT takes SP2 hydridization, compare SP3 hydridization, in SP2 hydridization, S orbital composition is larger, CNT is made to have high-modulus, high strength and high tenacity, show good mechanical property, being the material with most high specific strength can prepared at present, is also that in known materials, fusing point is the highest.Therefore, CNT has unique advantage for the aspect such as intensity, elasticity, fatigue resistance improving composite.
The advantage of above-mentioned material is combined with the magnetic aerogel material that graphene oxide/Graphene is carrier, take CNT as skeleton, relative to common ferriferrous oxide particles, it is on the basis keeping original magnetic effect, possessed that density is low, specific area be large, high adsorption capacity, the advantage that conducts electricity very well, significantly improve, better to tackle the application demand of different field in photoelectricity, electromagnetism, storage hydrogen, bio-sensing, absorption property, target administration, absorbing property etc.
At present, have no about being carrier with graphene oxide/Graphene, taking CNT as the magnetic aerogel material of skeleton and the report of preparation method in document, therefore, the preparation based on the magnetic aerogel material of Graphene has far-reaching influence for the performance of optimization magnetic material and the application of expansion material.
Summary of the invention
Problem to be solved by this invention is the finiteness of aerogel material and preparation method in prior art, provides a kind of magnetic aeroge new material based on graphene oxide/Graphene and preparation method thereof, is conducive to performance optimization and the application of expanding magnetic material.
In order to realize foregoing invention target, the technical solution used in the present invention is to provide a kind of preparation method of magnetic aeroge, comprises the steps:
(1) be dissolved in deionized water by graphite oxide, be mixed with the graphite oxide aqueous solution that concentration is 0.02g/L ~ 100 g/L, ultrasonic disperse, obtains graphene oxide water solution;
(2) by tri-iron tetroxide ultrasonic disperse in deionized water, be mixed with the tri-iron tetroxide aqueous solution that concentration is 0.02g/L ~ 100 g/L; Be under the stirring condition of 10 ~ 30 DEG C in temperature, be 1:100 ~ 100:1 in mass ratio, the tri-iron tetroxide aqueous solution be slowly added dropwise in graphene oxide water solution, stir, obtain the binary complex liquid of graphene oxide/tri-iron tetroxide;
(3) calcium salt is dissolved or dispersed in deionized water, is mixed with the calcium saline solution that concentration is 0.1g/L ~ 100 g/L; It is 20 ~ 50 DEG C in temperature, under 100r/min ~ 1000r/min stirs, calcium saline solution is dropwise added dropwise in the binary complex liquid of graphene oxide/tri-iron tetroxide, the mass ratio controlling calcium salt and graphene oxide/ferroferric oxide compound is 1:10 ~ 1:200, after stirring 1 ~ 60min again, obtain the binary complex of the graphene oxide/tri-iron tetroxide of thickness;
(4), after binary complex stirring 1 ~ 10 min of graphene oxide/tri-iron tetroxide step (3) obtained, through freeze drying, a kind of graphene oxide magnetic aeroge is obtained, the density>=0.1mg/cm of described graphene oxide magnetic aeroge
3.
The present invention also comprises graphene oxide magnetic aeroge step (5) obtained and is placed in the reducing agent aqueous solution that reducing agent steam or concentration are 0.01g/L ~ 10g/L, and described reducing agent is the one in sodium borohydride, potassium borohydride, hydrazine hydrate, hydroiodic acid, vitamin C, reproducibility glucose; The mass ratio of reducing agent and graphene oxide is 10:1 ~ 1:100, is, after reacting 1 ~ 24h under the condition of 10 DEG C ~ 90 DEG C, through freeze drying, to obtain a kind of Graphene magnetic aeroge, the density>=0.1mg/cm of described Graphene magnetic aeroge in temperature
3.
In technique scheme, can add CNT in the binary complex liquid of the graphene oxide/tri-iron tetroxide of step (2), the mass ratio of CNT and graphene oxide is 1:1 ~ 1:100.
Tri-iron tetroxide of the present invention is dispersed nano tri-iron tetroxide or polydispersion nano ferriferrous oxide; Described calcium salt is the one in calcium carbonate and diluted acid mixture, calcium chloride, or multiple; Described diluted acid is the one in watery hydrochloric acid, dust technology, acetic acid, or multiple.
Technical solution of the present invention also comprises a kind of graphene oxide magnetic aeroge obtained by above-mentioned preparation method.
Graphene oxide of the present invention is prepare through Hummers method or modified Hummers method, is single-layer graphene oxide, multilayer graphene oxide or the mixture of the two.Following concrete method can be adopted to prepare graphene oxide: by the raw graphite of 1 part of weight, the phosphoric acid of the concentrated sulfuric acid of 1 ~ 100 part of weight and 1 ~ 10 part, ice bath mixing, stir 10 ~ 60min; Slowly add the potassium permanganate of 1 ~ 10 part of weight, maintenance system temperature, not higher than 20 DEG C, stirs 20 ~ 60min; Withdraw ice bath, reaction system is transferred in 30 ~ 50 DEG C, fully stirs 2 ~ 5h; In reactant, slowly drip the deionized water of 1 ~ 100 part of weight, when system temperature no longer rises, transfer them to rapidly in 98 DEG C, stir 15 ~ 30min; 10 ~ 200 parts of weight deionized waters are added successively in system, the hydrogen peroxide of 1 ~ 30 part of weight, product is taken out after 5 ~ 20min, filter while hot, filter cake, after the watery hydrochloric acid cyclic washing that 10 ~ 500 parts of concentration are 1wt% ~ 5wt%, is scattered in the deionized water of 10 ~ 1000 parts of weight again, dialysis 72h, take out product, through centrifugal, collection, freeze drying, obtain product.
Compared with prior art, the invention has the advantages that:
(1) graphene oxide has amphipathic, and good wettability and surface-active make it in water He in composite, have superior dispersiveness, are easy to other component effect, and can obtain the grapheme material of electric conductivity excellence through electronation.The present invention take graphene oxide as carrier, by its extra specific surface area advantage, spread loads is carried out to single dispersing or polydispersion nano ferriferrous oxide, can add or not add a small amount of CNT as material " skeleton " composition simultaneously, and further calcium ion crosslinking process is carried out to system, directly can obtain graphene oxide magnetic aeroge through freeze-drying, or obtain graphene conductive magnetic aeroge through electronation, freeze-drying.This technological design both ensure that being uniformly distributed of magnetism of material, also can maintain material structure to greatest extent and stablize, strengthens its mechanical property.
(2) relative to the magnetic material of the types such as common ferriferrous oxide particles, magnetic aeroge of the present invention is on the basis keeping original magnetic effect, had more that density is low, intensity is large standby, high temperature resistant, specific area large, high adsorption capacity, the advantage that conducts electricity very well, can be significantly improved in photoelectricity, electromagnetism, storage hydrogen, bio-sensing, absorption property etc., can be used for the field such as sewage disposal (recyclable adsorbent), target administration, absorbing material, and be expected to the user demand meeting all kinds of extreme environment.
(3) according to different application demand, this method can be selected directly to obtain graphene oxide magnetic aeroge or obtains graphene conductive magnetic aeroge through reduction.The two respectively has superiority for fields such as sewage disposal, target administration, absorbing material, hydrogen storage material, photoelectric materials, and then can reach the object of required design.
Accompanying drawing explanation
Fig. 1 is SEM figure (amplifying 120 times) of the graphene oxide magnetic aeroge that the embodiment of the present invention obtains;
Fig. 2 is the XRD spectra of the graphene oxide magnetic aeroge that the embodiment of the present invention obtains;
Fig. 3 and Fig. 4 is the SEM figure of ferriferrous oxide nano-particle in the embodiment of the present invention, Fig. 3 is amplification 80K times, and Fig. 4 is for amplifying 90K doubly;
Fig. 5 is the graphene oxide magnetic aeroge of embodiment of the present invention acquisition and the infrared spectrogram of material oxidation Graphene.
Detailed description of the invention
Do concrete introduction below in conjunction with the drawings and specific embodiments to the present invention, the raw material not making specified otherwise in the present invention is commercial.
Embodiment 1:
(1) get 2g graphite powder and be placed in three products flask, ice bath adds the mixture of the 41.4ml concentrated sulfuric acid and 4.6ml phosphoric acid under stirring, and after stirring 15min, slowly adds 12g potassium permanganate, and maintenance system temperature, not higher than 20 DEG C, stirs 30min; Withdraw ice bath, reaction system is placed in 35 DEG C of water-baths, fully stirs 2h, reactant becomes dark brown pastel; Get 20ml deionized water to be slowly added in reactant, hierarchy of control temperature, not higher than 98 DEG C, when temperature no longer rises, transfers them to rapidly in 98 DEG C of water-baths, stirs 15min; In reactant, add 280ml, the deionized water of 50 DEG C and 20ml 30% hydrogen peroxide successively, reactant is glassy yellow by brown stain; After stirring 5min, take out and filter while hot, obtain product yellowish-brown filter cake, 300ml, 3% hydrochloric acid by product centrifuge washing 3 times, then use deionized water cyclic washing to faintly acid, by product dilution to 200ml, dialysis 72h(bag filter interception 14KDa) after, freeze drying obtains graphite oxide.
(2) (NH is got
4)
2fe (SO
4)
2.6H
2o 0.784g is dissolved in 20mL deionized water, and the amphiphilic hyper-branched polyglycidyl ether of 0.5g is dissolved in 10mL chloroform, under rapid stirring, amphiphilic hyper-branched poly epihydric alcohol ethereal solution is slowly dropped to (NH
4)
2fe (SO
4)
2.6H
2in the O aqueous solution, mix to obtain Fe
2+precursor solution; Getting 1g NaOH is dissolved in 10mL ethanol, and gained NaOH solution dropwise joins above-mentioned Fe
2+in precursor solution, gained Fe after stirring 30min
2+presoma complex liquid be transferred in hydrothermal reaction kettle, after 180 DEG C of reaction 10h, take out product successively through deionized water, absolute ethyl alcohol at 6000r/min centrifuge washing, product is scattered in deionized water again, obtains the ferriferrous oxide nano-particle solution of average grain diameter at 8 ~ 35nm.
(3) getting 0.1g graphite oxide is dissolved in 10mL deionized water, and ultrasonic disperse compound concentration is the graphene oxide water solution of 10g/L; Get the tri-iron tetroxide aqueous solution 1ml of concentration 30g/L, slowly drop in above-mentioned graphene oxide solution under 25 DEG C of stirrings, stir, obtain the binary complex liquid of graphene oxide/tri-iron tetroxide; Under 30 DEG C of high-speed stirred, the calcium chloride water getting 1mL concentration 10g/L is dropwise added dropwise in the binary complex liquid of graphene oxide/tri-iron tetroxide, stir 20min, packing is carried out to the binary complex of gained graphene oxide/tri-iron tetroxide, obtains density through freeze drying and be about 5.9mg/cm
3graphene oxide magnetic aeroge.Graphene oxide magnetic aeroge is placed in the hydrazine hydrate aqueous solution that concentration is 0.01g/L, reacts 2h at 50 DEG C, freeze drying obtains density and is about 5.9mg/cm
3graphene conductive magnetic aeroge.
See accompanying drawing 1, it is the SEM figure of the magnetic aeroge that the present embodiment obtains.Clearly, this magnetic aerogel material inside is typical porous laminated structure, interlamellar spacing is evenly distributed and is less than 100 μm, and layer and interlayer have tablet to rise to isolate and supporting role, and this three-layer laminated loose structure ensure that the feature of material low-density, high strength and high-specific surface area.
See accompanying drawing 2, it is the XRD spectra of the magnetic aeroge that the present embodiment obtains.Contrast known with tri-iron tetroxide XRD standard card (JCPDS No.26-1136), its XRD diffraction maximum is completely corresponding with the standard spectrogram of tri-iron tetroxide XRD, 9 diffraction maximums correspond to the diffraction maximum of (111), (220), (311) of tri-iron tetroxide, (222), (400), (422), (511), (440) and (533) crystal face respectively, show in aeroge prepared by the present invention really containing tri-iron tetroxide.
Accompanying drawing 3, Fig. 4 are all SEM figure of tri-iron tetroxide used in the present embodiment.From Fig. 3 (amplifying 80K doubly), Fig. 4 (amplifying 90K doubly), tri-iron tetroxide particle dispersion is good and be evenly distributed, single tri-iron tetroxide average particle size is at about 10nm, part tri-iron tetroxide presents the clustering phenomena of some individual particles (many particles), average grain diameter is at about 35nm, and observe obvious nucleocapsid structure, because of tri-iron tetroxide surface wrap up by both sexes hyperbranched polyglycidyl ether caused by, this is confirmed in this seminar early-stage Study.
Fig. 5 be the present embodiment obtain graphene oxide magnetic aeroge (curve b) (curve infrared spectrum a) contrasts and schemes with material oxidation Graphene.Analyze known, originally belong in magnetic aeroge (curve b) material oxidation Graphene (curve a) in the flexural vibrations peak (1050cm of-O-H on carboxyl
-1) disappear, meanwhile, at 1118 cm
-1there is a broad peak, having analyzed the ester bond absworption peak into being formed by the both sexes hyperbranched polyglycidyl ether esterification of carboxyl in graphene oxide and tri-iron tetroxide surface, overlapping with the ehter bond absworption peak on tri-iron tetroxide surface and cause.Illustrate that tri-iron tetroxide is loaded on graphene oxide in the mode of chemical bonding, which ensure that the uniformly dispersed of tri-iron tetroxide and stability, make aerogel material possess uniform and stable magnetic property.
Embodiment 2:
(1) get 1g graphite powder and be placed in three products flask, ice bath adds the mixture of the 20.7ml concentrated sulfuric acid and 2.3ml phosphoric acid under stirring, and after stirring 15min, slowly adds 6g potassium permanganate, and maintenance system temperature, not higher than 20 DEG C, stirs 30min; Withdraw ice bath, reaction system is placed in 35 DEG C of water-baths, fully stirs 2h, reactant becomes dark brown pastel; Get 10ml deionized water to be slowly added in reactant, hierarchy of control temperature, not higher than 98 DEG C, when temperature no longer rises, transfers them to rapidly in 98 DEG C of water-baths, stirs 15min; In reactant, add 140ml, the deionized water of 50 DEG C and 10ml 30% hydrogen peroxide successively, reactant is glassy yellow by brown stain; After stirring 5min, take out and filter while hot, obtain product yellowish-brown filter cake, 150ml, 3% hydrochloric acid by product centrifuge washing 3 times, then use deionized water cyclic washing to faintly acid, by product dilution to 100ml, dialysis 72h(bag filter interception 14KDa) after, freeze drying obtains graphite oxide.
(2) FeSO is got
47H
2o 1.112g is dissolved in 40mL deionized water, and 1g amphipathic end amino superbranching polymer is dissolved in 20mL ethanol, under rapid stirring, amphipathic end amino superbranching polymer solution is slowly dropped to FeSO
47H
2in the O aqueous solution, mix to obtain Fe
2+precursor solution; Getting 2g NaOH is dissolved in 20mL n-butanol, and gained NaOH solution dropwise joins above-mentioned Fe
2+in precursor solution, gained Fe after stirring 40min
2+presoma complex liquid be transferred in hydrothermal reaction kettle, after 160 DEG C of reaction 13h, take out product successively through deionized water, acetone at 8000r/min centrifuge washing, product is scattered in deionized water again, obtains the ferriferrous oxide nano-particle solution that particle diameter is 8nm.
(3) getting 0.2g graphite oxide is dissolved in 10mL deionized water, and ultrasonic disperse compound concentration is the graphene oxide water solution of 20g/L; Getting 0.05g hydroxylating multi-walled carbon nano-tubes is scattered in 10mL deionized water, and configuration concentration is the carbon nano-tube aqueous solutions of 5g/L.Under stirring, carbon nano-tube aqueous solutions is slowly joined in graphene oxide solution, mix the binary complex liquid obtaining graphene oxide/CNT; Get the tri-iron tetroxide aqueous solution 1ml of concentration 50g/L, slowly drop in the binary complex liquid of above-mentioned graphene oxide/CNT under 25 DEG C of stirrings, stir, obtain the tri compound liquid of graphene oxide/CNT/tri-iron tetroxide; Under 25 DEG C of high-speed stirred, the calcium chloride water getting 1mL concentration 5g/L is dropwise added dropwise in the tri compound liquid of graphene oxide/CNT/tri-iron tetroxide, stir 30min, packing is carried out to the ternary complex of gained graphene oxide/CNT/tri-iron tetroxide, obtains density through freeze drying and be about 10mg/cm
3graphene oxide magnetic aeroge.Graphene oxide magnetic aeroge is placed in the vitamin C aqueous solution that concentration is 0.05g/L, and react 5h at 60 DEG C, freeze drying obtains density and is about 10mg/cm
3graphene conductive magnetic aeroge.
Magnetic aeroge based on graphene oxide/Graphene prepared by the present invention, on the original magnetic effect basis of maintenance, the advantage that it has had more standby, and density is low, intensity is large, high temperature resistant, specific area is large, design feature determines that it can be used for the field such as sewage disposal (recyclable adsorbent), target administration, absorbing material, and possess unique advantage, be expected to the user demand meeting all kinds of extreme environment.
Claims (6)
1. a preparation method for magnetic aeroge, is characterized in that comprising the steps:
(1) be dissolved in deionized water by graphite oxide, be mixed with the graphite oxide aqueous solution that concentration is 0.02g/L ~ 100 g/L, ultrasonic disperse, obtains graphene oxide water solution;
(2) by tri-iron tetroxide ultrasonic disperse in deionized water, be mixed with the tri-iron tetroxide aqueous solution that concentration is 0.02g/L ~ 100 g/L; Be under the stirring condition of 10 ~ 30 DEG C in temperature, be 1:100 ~ 100:1 in mass ratio, the tri-iron tetroxide aqueous solution be slowly added dropwise in graphene oxide water solution, stir, obtain the binary complex liquid of graphene oxide/tri-iron tetroxide;
(3) calcium salt is dissolved or dispersed in deionized water, is mixed with the calcium saline solution that concentration is 0.1g/L ~ 100 g/L; It is 20 ~ 50 DEG C in temperature, under 100r/min ~ 1000r/min stirs, calcium saline solution is dropwise added dropwise in the binary complex liquid of graphene oxide/tri-iron tetroxide, the mass ratio controlling calcium salt and graphene oxide/ferroferric oxide compound is 1:10 ~ 1:200, after stirring 1 ~ 60min again, obtain the binary complex of the graphene oxide/tri-iron tetroxide of thickness;
(4), after binary complex stirring 1 ~ 10 min of graphene oxide/tri-iron tetroxide step (3) obtained, through freeze drying, a kind of graphene oxide magnetic aeroge is obtained, the density>=0.1mg/cm of described graphene oxide magnetic aeroge
3.
2. the preparation method of a kind of magnetic aeroge according to claim 1, it is characterized in that: in the binary complex liquid of the graphene oxide/tri-iron tetroxide of step (2), add CNT, the mass ratio of CNT and graphene oxide is 1:1 ~ 1:100.
3. the preparation method of a kind of magnetic aeroge according to claim 1, is characterized in that, described tri-iron tetroxide is dispersed nano tri-iron tetroxide or polydispersion nano ferriferrous oxide.
4. the preparation method of a kind of magnetic aeroge according to claim 1, is characterized in that, described calcium salt is the one in calcium carbonate and diluted acid mixture, calcium chloride, or multiple; Described diluted acid is the one in watery hydrochloric acid, dust technology, acetic acid, or multiple.
5. the preparation method of a kind of magnetic aeroge according to claim 1, it is characterized in that, graphene oxide magnetic aeroge step (4) obtained is placed in the reducing agent aqueous solution that reducing agent steam or concentration are 0.01g/L ~ 10g/L, and described reducing agent is the one in sodium borohydride, potassium borohydride, hydrazine hydrate, hydroiodic acid, vitamin C, reproducibility glucose; The mass ratio of reducing agent and graphene oxide is 10:1 ~ 1:100, is, after reacting 1 ~ 24h under the condition of 10 DEG C ~ 90 DEG C, through freeze drying, to obtain a kind of Graphene magnetic aeroge, the density>=0.1mg/cm of described Graphene magnetic aeroge in temperature
3.
6. by a kind of graphene oxide magnetic aeroge that claim 1 preparation method obtains.
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| CN102941042A (en) * | 2012-10-25 | 2013-02-27 | 北京理工大学 | Graphene/metal oxide hybrid aerogel, preparation method and applications thereof |
| CN102910625A (en) * | 2012-11-14 | 2013-02-06 | 北京理工大学 | Graphene oxide aerogel, preparation method and application |
| CN103432994A (en) * | 2013-09-09 | 2013-12-11 | 中国科学院新疆理化技术研究所 | Preparation method of magnetic graphene based oil absorption foam material |
| CN103551091A (en) * | 2013-11-25 | 2014-02-05 | 北京化工大学 | Method for drying aerogel |
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