CN103977748A - Magnetic aerogel and preparation method thereof - Google Patents
Magnetic aerogel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses magnetic aerogel and a preparation method thereof. The preparation method comprises the following steps: loading ferroferric oxide magnetic nanoparticles by taking graphene oxide as a carrier, improving the morphological stability by taking a carbon nano tube as a framework or by using a calcium ion cross-linking effect, freezing and drying to obtain graphene oxide magnetic aerogel, and performing chemical reduction so as to obtain the graphene magnetic aerogel. On the basis of maintaining the ferroferric oxide magnetic effect, the aerogel also has the advantages of low density, great strength, high-temperature resistance and large specific surface area; due to the structure characteristic, the aerogel has the super strong absorption capacity, wave absorption capacity and conductivity; the magnetic aerogel can be used in the fields of sewage treatment, target administration, wave absorption materials and photoelectric materials. The magnetic aerogel is a 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, has been subject to extensive concern.Above application all requires that respective material possesses that density is low, specific area is large, high adsorption capacity, feature that delivered payload capability is strong, good magnetic property be meet that material easily reclaims, target ability is strong, realize the essential condition of microwave absorption, and current material is often difficult to meet many-sided performance demand simultaneously.Take absorbing material as example, because of its high request to electromagnetic property, the tri-iron tetroxide that magnetic property is good is still one of main component of absorbing material so far, how absorbing material is completely made by single ferrite, ferrite mostly is the coating material existing with forms such as powder and particles, although with low cost, technique is simple, but it is light to be difficult to meet quality, the requirement of the wide grade of absorption band, and because of its density greatly easily cause under poor high temperature stability and hot environment and high band range in the shortcomings such as absorbing property is poor, cause its application in the specific environments such as aircraft to be very restricted.Equally, in fields such as sewage disposal and target administrations, the porous magnetic material of light weight is easier to reclaim, easily realizes target control.Therefore, in order to meet multi-field application demand, overcome this defect, need 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, has 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, and a plurality of research fields are widely used.Graphene oxide is that native graphite is through chemical oxidation and a kind of monolayer carbon atom two-dimensional nano material obtaining after peeling off, 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 radicals (in the middle of lamella :-OH, C-O-C, edge :-C=O,-COOH), have amphipathic, from chip edge to central authorities, present hydrophilic to hydrophobic property distribution, demonstrate good wettability and surface-active, and in water, show superior dispersiveness, after becoming Graphene, electronation more shows excellent electric conductivity, these features are all that it is widely used in reason prepared by composite.CNT can be regarded that graphene sheet layer is curling as and form, 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 is taked SP2 hydridization, compare SP3 hydridization, in SP2 hydridization, S orbital composition is larger, make CNT there is high-modulus, high strength and high tenacity, show good mechanical property, being the material with high specific strength that can prepare at present, is also that in known materials, fusing point is the highest.Therefore, CNT has unique advantage for improving the aspects such as intensity, elasticity, fatigue resistance of composite.
The magnetic aerogel material that the graphene oxide/Graphene of take is skeleton as carrier, the CNT of take combines the advantage of above-mentioned material, with respect to common ferriferrous oxide particles, it is keeping on the basis of original magnetic effect, possessed that density is low, specific area is large, high adsorption capacity, the advantage that conducts electricity very well, at aspects such as photoelectricity, electromagnetism, storage hydrogen, bio-sensing, absorption property, target administration, absorbing properties, significantly improve, better to tackle the application demand of different field.
At present, in document, have no relevant and take graphene oxide/Graphene as carrier, the CNT of the take magnetic aerogel material that is skeleton and preparation method's report, therefore, the preparation of the magnetic aerogel material based on 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, the performance optimization and the application that are conducive to expand 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) graphite oxide is dissolved in deionized water, being mixed with concentration is the graphite oxide aqueous solution of 0.02g/L～100 g/L, and ultrasonic dispersion, obtains graphite oxide aqueous solution;
(2) be scattered in deionized water tri-iron tetroxide is ultrasonic, being mixed with concentration is the tri-iron tetroxide aqueous solution of 0.02g/L～100 g/L; In temperature, be, under the stirring condition of 10～30 ℃, to be 1:100～100:1 in mass ratio, the tri-iron tetroxide aqueous solution is slowly splashed in graphite oxide aqueous 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; In temperature, it is 20～50 ℃, under 100r/min～1000r/min stirs, calcium saline solution is dropwise splashed in the binary complex liquid of graphene oxide/tri-iron tetroxide, the mass ratio of controlling calcium salt and graphene oxide/ferroferric oxide compound is 1:10～1:200, stir again after 1～60min, obtain the binary complex of the graphene oxide/tri-iron tetroxide of thickness;
(4) binary complex of graphene oxide/tri-iron tetroxide step (3) being obtained stirs after 1～10 min, through freeze drying, obtains a kind of graphene oxide magnetic aeroge, the density>=0.1mg/cm of described graphene oxide magnetic aeroge
3.
The present invention also comprises that the graphene oxide magnetic aeroge that step (5) is 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 a kind of 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 to react after 1～24h under the condition of 10 ℃～90 ℃ in temperature, through freeze drying, obtains a kind of Graphene magnetic aeroge, the density>=0.1mg/cm of described Graphene magnetic aeroge
3.
In technique scheme, in the binary complex liquid of the graphene oxide/tri-iron tetroxide of step (2), can add CNT, 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 a kind of in calcium carbonate and diluted acid mixture, calcium chloride, or multiple; Described diluted acid is a kind of in watery hydrochloric acid, rare nitric acid, acetic acid, or multiple.
Technical solution of the present invention also comprises a kind of graphene oxide magnetic aeroge obtaining by above-mentioned preparation method.
Graphene oxide of the present invention is to prepare through Hummers method or modified Hummers method, is mono-layer graphite oxide alkene, multilayer graphene oxide or the mixture of the two.Can adopt following concrete method to prepare graphene oxide: by the raw material 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 mixes, stirs 10～60min; The potassium permanganate that slowly adds 1～10 part of weight, maintenance system temperature, not higher than 20 ℃, stirs 20～60min; Withdraw ice bath, reaction system is transferred in 30～50 ℃, fully stir 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 ℃, stir 15～30min; In system, add 10～200 parts of weight deionized waters successively, the hydrogen peroxide of 1～30 part of weight, after 5～20min, take out product, filter while hot, after the watery hydrochloric acid cyclic washing that filter cake is 1wt%～5wt% through 10～500 parts of concentration, be again scattered in the deionized water of 10～1000 parts of weight, 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, good wettability and surface-active makes it in water He in composite, have superior dispersiveness, is easy to other component effect, and through electronation, can obtains the grapheme material of electric conductivity excellence.The present invention be take graphene oxide as carrier, by its super large specific area advantage, single dispersion or polydispersion nano ferriferrous oxide are carried out to spread loads, can add or not add a small amount of CNT as material " skeleton " composition simultaneously, and further system is carried out to calcium ion crosslinking processing, through freeze-drying, can directly obtain graphene oxide magnetic aeroge, or obtain graphene conductive magnetic aeroge through electronation, freeze-drying.This technological design had both guaranteed being uniformly distributed of magnetism of material, also can maintain to greatest extent material structure and stablize, strengthens its mechanical property.
(2) with respect to the magnetic material of the common types such as ferriferrous oxide particles, magnetic aeroge of the present invention is keeping on the basis of original magnetic effect, have more that density is low, intensity is large, high temperature resistant, specific area large standby, high adsorption capacity, the advantage that conducts electricity very well, at aspects such as photoelectricity, electromagnetism, storage hydrogen, bio-sensing, absorption properties, can be significantly improved, can be used for the fields such as sewage disposal (recyclable adsorbent), target administration, absorbing material, and be expected to meet the user demand of all kinds of extreme environments.
(3) can, according to different application demand, select this method directly to obtain graphene oxide magnetic aeroge or obtain 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 the SEM figure (amplifying 120 times) of the graphene oxide magnetic aeroge of embodiment of the present invention acquisition;
Fig. 2 is the XRD spectra of the graphene oxide magnetic aeroge of embodiment of the present invention acquisition;
Fig. 3 and Fig. 4 are the SEM figure of ferriferrous oxide nano-particle in the embodiment of the present invention, and Fig. 3 is for amplifying 80K doubly, 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 feed oxygen functionalized graphene.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is done to concrete introduction, the raw material of 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, stir after 15min, slowly adds 12g potassium permanganate, and maintenance system temperature, not higher than 20 ℃, stirs 30min; Withdraw ice bath, reaction system is placed in to 35 ℃ of water-baths, fully stir 2h, reactant becomes dark brown pastel; Get 20ml deionized water and be slowly added in reactant, hierarchy of control temperature, not higher than 98 ℃, when temperature no longer rises, transfers them to rapidly in 98 ℃ of water-baths, stirs 15min; To adding 280ml, deionized water and 20ml 30% hydrogen peroxide of 50 ℃ in reactant, reactant is glassy yellow by brown stain successively; Stir after 5min, take out while hot and filter, obtain product yellowish-brown filter cake, 300ml, 3% hydrochloric acid be product centrifuge washing 3 times, then use deionized water cyclic washing to faintly acid, and product is diluted to 200ml, dialysis 72h(bag filter interception 14KDa), after, freeze drying obtains graphite oxide.
(2) get (NH
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; Get 1g NaOH and be dissolved in 10mL ethanol, 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 ℃ 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 average grain diameter at the ferriferrous oxide nano-particle solution of 8 ~ 35nm.
(3) get 0.1g graphite oxide and be dissolved in 10mL deionized water, the graphite oxide aqueous solution that ultrasonic dispersion compound concentration is 10g/L; The tri-iron tetroxide aqueous solution 1ml that gets concentration 30g/L, slowly drops in above-mentioned graphene oxide solution under 25 ℃ of stirrings, stirs, and obtains the binary complex liquid of graphene oxide/tri-iron tetroxide; Under 30 ℃ of high-speed stirred, the calcium chloride water of getting 1mL concentration 10g/L dropwise splashes in the binary complex liquid of graphene oxide/tri-iron tetroxide, stir 20min, the binary complex of gained graphene oxide/tri-iron tetroxide is carried out to packing, through freeze drying, obtain density and be about 5.9mg/cm
3graphene oxide magnetic aeroge.Graphene oxide magnetic aeroge is placed in to the hydrazine hydrate aqueous solution that concentration is 0.01g/L, reacts 2h at 50 ℃, freeze drying obtains density and is about 5.9mg/cm
3graphene conductive magnetic aeroge.
Referring to accompanying drawing 1, it is the SEM figure of the magnetic aeroge of the present embodiment acquisition.Clearly, this magnetic aerogel material inside is typical porous laminated structure, interlamellar spacing is evenly distributed and is less than 100 μ m, and layer has tablet to play isolation and supporting role with interlayer, and this three-layer laminated loose structure has guaranteed the feature of material low-density, high strength and high-specific surface area.
Referring to accompanying drawing 2, it is the XRD spectra of the magnetic aeroge of the present embodiment acquisition.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 respectively (111), (220), (311), (222), (400), (422), (511) of tri-iron tetroxide, the diffraction maximum of (440) and (533) crystal face, show really to contain tri-iron tetroxide in aeroge prepared by the present invention.
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 good dispersion and being evenly distributed, single tri-iron tetroxide average particle size is in 10nm left and right, part tri-iron tetroxide presents the clustering phenomena of some individual particles (many particles), average grain diameter is in 35nm left and right, and observe obvious nucleocapsid structure, due to tri-iron tetroxide surface wrapped up by both sexes hyperbranched polyglycidyl ether, in Zhe Ben seminar early-stage Study, be confirmed.
Fig. 5 is that (curve infrared spectrum a) contrasts figure to the graphene oxide magnetic aeroge (curve b) that obtains of the present embodiment with feed oxygen functionalized graphene.Analyze known, originally belong in magnetic aeroge (curve b) feed oxygen functionalized graphene (curve a) on carboxyl-the flexural vibrations peak (1050cm of O-H
-1) disappeared, meanwhile, at 1118 cm
-1there is a broad peak, analyzed the ester bond absworption peak that the both sexes hyperbranched polyglycidyl ether esterification into carboxyl in graphene oxide and tri-iron tetroxide surface forms, overlapping and cause with the ehter bond absworption peak on tri-iron tetroxide surface.Illustrate that tri-iron tetroxide is that mode with chemical bonding is loaded on graphene oxide, the uniformly dispersed and stability that this has guaranteed tri-iron tetroxide, makes 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, stir after 15min, slowly adds 6g potassium permanganate, and maintenance system temperature, not higher than 20 ℃, stirs 30min; Withdraw ice bath, reaction system is placed in to 35 ℃ of water-baths, fully stir 2h, reactant becomes dark brown pastel; Get 10ml deionized water and be slowly added in reactant, hierarchy of control temperature, not higher than 98 ℃, when temperature no longer rises, transfers them to rapidly in 98 ℃ of water-baths, stirs 15min; To adding 140ml, deionized water and 10ml 30% hydrogen peroxide of 50 ℃ in reactant, reactant is glassy yellow by brown stain successively; Stir after 5min, take out while hot and filter, obtain product yellowish-brown filter cake, 150ml, 3% hydrochloric acid be product centrifuge washing 3 times, then use deionized water cyclic washing to faintly acid, and product is diluted to 100ml, dialysis 72h(bag filter interception 14KDa), after, freeze drying obtains graphite oxide.
(2) get FeSO
47H
2o 1.112g is dissolved in 40mL deionized water, and the amphipathic end amino superbranching of 1g 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; Get 2g NaOH and be dissolved in 20mL n-butanol, 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 ℃ of reaction 13h, take out product successively through deionized water, acetone at 8000r/min centrifuge washing, product is scattered in deionized water again, obtaining particle diameter is the ferriferrous oxide nano-particle solution of 8nm.
(3) get 0.2g graphite oxide and be dissolved in 10mL deionized water, the graphite oxide aqueous solution that ultrasonic dispersion compound concentration is 20g/L; Get 0.05g hydroxylating multi-walled carbon nano-tubes and be scattered in 10mL deionized water, the carbon nano-tube aqueous solutions that configuration concentration is 5g/L.Under stirring, carbon nano-tube aqueous solutions is slowly joined in graphene oxide solution, mix the binary complex liquid that obtains graphene oxide/CNT; The tri-iron tetroxide aqueous solution 1ml that gets concentration 50g/L, slowly drops under 25 ℃ of stirrings in the binary complex liquid of above-mentioned graphene oxide/CNT, stirs, and obtains the tri compound liquid of graphene oxide/CNT/tri-iron tetroxide; Under 25 ℃ of high-speed stirred, the calcium chloride water of getting 1mL concentration 5g/L dropwise splashes in the tri compound liquid of graphene oxide/CNT/tri-iron tetroxide, stir 30min, the ternary complex of gained graphene oxide/CNT/tri-iron tetroxide is carried out to packing, through freeze drying, obtain density and be about 10mg/cm
3graphene oxide magnetic aeroge.Graphene oxide magnetic aeroge is placed in to the vitamin C aqueous solution that concentration is 0.05g/L, reacts 5h at 60 ℃, 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, keeping on original magnetic effect basis, it has had more the advantage that density is low, intensity is large, high temperature resistant, specific area is large standby, design feature determines that it can be used for the fields such as sewage disposal (recyclable adsorbent), target administration, absorbing material, and possess unique advantage, be expected to meet the user demand of all kinds of extreme environments.
Claims (6)
1. a preparation method for magnetic aeroge, is characterized in that comprising the steps:
(1) graphite oxide is dissolved in deionized water, being mixed with concentration is the graphite oxide aqueous solution of 0.02g/L～100 g/L, and ultrasonic dispersion, obtains graphite oxide aqueous solution;
(2) be scattered in deionized water tri-iron tetroxide is ultrasonic, being mixed with concentration is the tri-iron tetroxide aqueous solution of 0.02g/L～100 g/L; In temperature, be, under the stirring condition of 10～30 ℃, to be 1:100～100:1 in mass ratio, the tri-iron tetroxide aqueous solution is slowly splashed in graphite oxide aqueous 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; In temperature, it is 20～50 ℃, under 100r/min～1000r/min stirs, calcium saline solution is dropwise splashed in the binary complex liquid of graphene oxide/tri-iron tetroxide, the mass ratio of controlling calcium salt and graphene oxide/ferroferric oxide compound is 1:10～1:200, stir again after 1～60min, obtain the binary complex of the graphene oxide/tri-iron tetroxide of thickness;
(4) binary complex of graphene oxide/tri-iron tetroxide step (3) being obtained stirs after 1～10 min, through freeze drying, obtains a kind of graphene oxide magnetic aeroge, 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 a kind of in calcium carbonate and diluted acid mixture, calcium chloride, or multiple; Described diluted acid is a kind of in watery hydrochloric acid, rare nitric acid, acetic acid, or multiple.
5. the preparation method of a kind of magnetic aeroge according to claim 1, it is characterized in that, the graphene oxide magnetic aeroge that step (5) is 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 a kind of 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 to react after 1～24h under the condition of 10 ℃～90 ℃ in temperature, through freeze drying, obtains a kind of Graphene magnetic aeroge, the density>=0.1mg/cm of described Graphene magnetic aeroge
3.
6. a kind of graphene oxide magnetic aeroge obtaining by claim 1 preparation method.
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