CN105195067A - Graphene aerogel microspheres and preparation method and application thereof - Google Patents
Graphene aerogel microspheres and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses graphene aerogel microspheres and a preparation method and application thereof. The preparation method is characterized in that 1, graphite oxide is prepared; 2, graphene oxide aqueous dispersion is prepared; 3, the graphene oxide aqueous dispersion is atomized through a spraying method into graphene oxide liquid drop microspheres, and meanwhile the microspheres are collected through receiving liquid in a cooling bath; 4, the receiving liquid is filtered to obtain graphene oxide ice microspheres, and then freeze drying is performed on the microspheres to obtain graphene oxide aerogel microspheres; 5, the graphene oxide aerogel microspheres are subjected to thermal reduction to obtain the graphene aerogel microspheres. The preparation method is simple and convenient to implement, no environmental pollution is generated, and the obtained graphene aerogel microspheres are uniform in size and large in specific area, are of a stable center-divergence multi-porous-channel network structure and are used for adsorbing environmental pollutants.
Description
Technical field
The present invention relates to a kind of graphene aerogel microballoon and its production and use, belong to field of functional materials.
Background technology
Graphene is a kind of New Two Dimensional material that carbon atom is formed with the regular arrangement of cellular mode.There is superior mechanical property, electric property, optical property, thermal property, therefore receive the extensive concern of each field personage.The Graphene of two dimension is configured to three-dimensional Graphene macroscopic material, is ensureing, under the condition that the excellent properties of Graphene is not destroyed, Graphene to be really applied in industrial production, there is an important method and the approach of practical use.Wherein, graphene aerogel as the representative of three-dimensional grapheme macroscopic material can not only retain the huge specific area of Graphene and excellent properties; the porous of aeroge uniqueness can also be had simultaneously; ultralow density, the performances such as low-k, therefore; graphene aerogel causes the very big attention of researcher and starts to be widely applied to power conversion and storage; High-performance catalyst carrier, environmental protection and purification, biomaterial and biotechnology field.
Aerogel microball has a series of more excellent character compared to aerogel block body, such as: have larger specific area as catalyst carrier, can provide more active reaction center; As packing material, there is good fluidity and be easy to dispersed, not easily cause stress to concentrate.Therefore can improve the service efficiency of aeroge to a great extent and widen the application of aeroge.Aerogel microball common at present has SiO
2aerogel microball, carbon aerogels microballoon and macromolecule aerogel-like microballoon, but also not about the report of graphene aerogel microballoon.Graphene aerogel being prepared as graphene aerogel microballoon, can not only be that graphene aerogel increases actual application value, for the development exploration in Graphene future and can also open up a new approach.
The porous of aeroge causes it to have the lower easily cracked characteristic of mechanical strength, makes the good uniform aerogel microball of preparation shape can not use simple such as ball milling, the mechanical processes such as shearing.Therefore at present the preparation process great majority of aerogel microball are that under rapid stirring, sol gel original position is prepared hydrogel microsphere and obtained aerogel microball after drying again.But this preparation method operation is comparatively complicated, and production efficiency is lower, and is not applicable to the sol gel reagent preparing Graphene hydrogel microsphere, therefore and be not suitable for the preparation of graphene aerogel microballoon.Therefore, at present also not about the patent document of graphene aerogel microballoon or the report of non-patent literature.
Summary of the invention
The object of the invention is a kind of graphene aerogel microballoon developed for the deficiencies in the prior art and its production and use.Be characterized in that this graphene aerogel microballoon size is comparatively homogeneous, there is abundant oxygen-containing functional group, be convenient to modification and load, have the multi-pore channel network structure of stable center divergent shape, the light density of quality is little and preparation method is simple and convenient, non-environmental-pollution, cost of material is low, and production efficiency is high.This graphene aerogel microballoon is applicable to environmental contaminants absorption.
Object of the present invention is realized by following technical measures, and wherein said raw material number, except specified otherwise, is parts by weight.
The initiation material of graphene aerogel microballoon is made up of following component:
Deionized water 100 parts
Graphite oxide 0.05-2 part
The preparation method of graphene aerogel microballoon comprises the steps:
(1) preparation of graphite oxide
Native graphite is prepared into graphite oxide through chemical oxidization method, and wherein chemical oxidization method is Brodie oxidizing process, Staudemaier oxidizing process, any one in the Hummer method of Hummer method or improvement;
(2) preparation of graphene oxide aqueous dispersions
By deionized water 100 parts, be prepared into dispersion liquid through 200-400W ultrasonic stripping 20-50min after graphite oxide 0.05-2 part Homogeneous phase mixing, concentration is 0.5-20mg/ml;
(3) by spray-on process, graphene oxide aqueous dispersions is atomized into graphene oxide drop microballoon, and is collected by the receiving liquid being placed in cooling bath, wherein, spray-on process is press atomization, any one in ullrasonic spraying or electrostatic spray;
(4) filter above-mentioned receiving liquid and obtain graphene oxide ice microballoon, after freeze drying, obtain graphite oxide aerogel microballoon;
(5) above-mentioned graphite oxide aerogel microballoon is obtained graphene aerogel microballoon by thermal reduction.
The pressure of described press atomization is 10-200Mpa, and the ultrasonic power of ullrasonic spraying is 10-150kHz, and the voltage of electrostatic spray is 5-20kv.
Described cooling bath is the bath of ice/sodium chloride, any one in dry ice/acetone batch or liquid nitrogen/ethyl acetate bath.
Described receiving liquid is ethyl acetate, toluene, at least one in n-hexane and normal heptane;
Described thermal reduction is the intensification thermal reduction of Muffle furnace Program or microwave irradiation thermal reduction under inert gas shielding.
Described temperature programming thermal reduction is that 5-10 DEG C/min is warming up to 800 DEG C and keeps 2-5h, and microwave irradiation thermal reduction is that power is 600-800W and keeps 1-10min.
Graphene aerogel microballoon is used for environmental contaminants absorption.
Structural characterization and performance test:
1, adopt the pattern of JSM-5900LV type SEM to graphene aerogel microballoon to observe, SEM figure is the results detailed in shown in Fig. 3.
Result shows: graphene aerogel microballoon good sphericity, has the cross-linked structure of porous.
2, adopt gravimetry test Graphene aerogel microball to the adsorption capacity of organic solvent, shown in Fig. 4.
Result shows: graphene aerogel microballoon has excellent adsorption capacity to organic solvent, and most high adsorption capacity reaches 178g chloroform/g graphene aerogel microballoon.
The present invention has the following advantages:
1. the present invention has prepared a kind of graphene aerogel microballoon
2. the graphene aerogel microspherulite diameter for preparing of preparation method of the present invention is controlled, and domain size distribution controls in 10-1000 μm of any range by the adjustment of atomization method and parameter, and specific area is high (is greater than 200m
2/ g), porosity, more than 95%, has abundant oxygen-containing functional group, is convenient to modification and load, and have the multi-pore channel network structure of stable center divergent shape, the light density of quality is little.
3. after the snap frozen atomized drop microballoon that the present invention uses, the dry technology obtaining aerogel microball is convenient and swift, easy and simple to handle, and can realize continuous seepage, efficiency is high.
4. the graphene aerogel microballoon that prepared by the present invention adsorbs for environmental contaminants.This graphene aerogel microballoon can adsorb multiple organic solvent and oils, and its adsorption capacity is high, is obviously better than the bulk graphene aerogel reported.And due to the characteristic that graphene aerogel microballoon lightweight is easily scattered, make can better collect absorption environmental contaminants in the environmental accidents such as its leakage of oil at sea.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that the present invention prepares graphene aerogel microballoon;
1. prepare graphite oxide; 2. prepare graphene oxide dispersion; 3. spraying and snap frozen; 4. filter; 5. freeze drying; 6. thermal reduction.
Fig. 2 is preparation technology's schematic diagram of the embodiment of the present invention 1 graphite oxide aerogel microballoon
Fig. 3 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 graphene aerogel microballoon;
Fig. 4 is that the embodiment of the present invention 2 graphene aerogel is to the schematic diagram of the adsorbance of organic solvent.
Detailed description of the invention
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only further described for the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through Brodie oxidizing process.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, the graphite oxide that 0.75gBrodie oxidizing process is prepared and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, 200W ultrasonic disperse stirs after 20 minutes and spends the night, and obtains the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 7.5mg/ml.
(3) trash ice is placed in the good uncovered Dewar bottle of insulation, adds sodium chloride powder, the formation trash ice that stirs/sodium chloride cools down bath.The beaker that ethyl acetate is housed is put into trash ice/sodium chloride cools down bath as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 7.5mg/ml prepared is loaded in the syringe on electrostatic atomizer, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, regulation voltage is 15Kv, start spraying and in receiving liquid cooling drop microballoon fast.As shown in Figure 2.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering ethyl acetate receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon obtained is placed in Muffle furnace under inert gas shielding, be warming up to 800 degrees Celsius by the programming rate of 5 DEG C/min and keep within 5 hours, namely obtaining black light graphite alkene aerogel microball, as shown in Figure 3.Average grain diameter is 247 μm, and density is 5.0kg/m
3.
Embodiment 2
(1) graphite oxide is prepared: the HUMMER method of native graphite through improving is prepared as graphite oxide.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, the graphite oxide that the HUMMER legal system improved by 1.5g is standby and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 400W ultrasonic disperse 35min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 15mg/ml.
(3) ethyl acetate is placed in the good uncovered Dewar bottle of insulation, adds a large amount of liquid nitrogen while stirring, until form the liquid nitrogen/ethyl acetate cooling bath of slush shape.The beaker that toluene and n-hexane are housed is put into liquid nitrogen/ethyl acetate cooling bath to cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 15mg/ml prepared is loaded in the syringe on ultrasonic spray apparatus, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, adjustments supersonic frequency is 150kHz, starts spraying and cool drop microballoon fast in receiving liquid.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon obtained is placed in Muffle furnace under inert gas shielding, be warming up to 800 DEG C by the programming rate of 10 DEG C/min and keep within 5 hours, namely obtaining black light graphite alkene aerogel microball.Average grain diameter is 15 μm, and density is 6.8kg/m
3.
Embodiment 3
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through HUMMER method.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, by graphite oxide standby for 0.5mgHUMMER legal system and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 300W ultrasonic disperse 30min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 5mg/ml.
(3) acetone is placed in the good uncovered Dewar bottle of insulation, adds dry ice fragment while stirring, until substantially cannot stir, namely define the dry ice/acetone cooling bath of thickness.The beaker that ethyl acetate and normal heptane are housed is put into dry ice/acetone cooling bath cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 5mg/ml prepared is loaded in the pressure chamber on press atomization device, regulate sprinkler height to make it to be separated by with receiving liquid after suitable distance, open compression pump and be adjusted to 40Mpa, start spraying and in receiving liquid cooling drop microballoon fast.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon 600W microwave power irradiation heat reduction 10min under inert gas shielding will obtained, namely obtains black light graphite alkene aerogel microball.Average grain diameter is 87 μm, and density is 3.9kg/m
3.
Embodiment 4
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through HUMMER method.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, by graphite oxide standby for 0.6mgHUMMER legal system and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, 200W ultrasonic disperse stirs after 35 minutes and spends the night, and obtains the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 6mg/ml.
(3) ethyl acetate is placed in the good uncovered Dewar bottle of insulation, adds a large amount of liquid nitrogen while stirring, until form the liquid nitrogen/ethyl acetate cooling bath of slush shape.N-hexane will be housed, ethyl acetate, and put into liquid nitrogen/ethyl acetate cooling bath in the beaker of normal heptane and cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 6mg/ml prepared is loaded in the syringe on electrostatic atomizer, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, regulation voltage is 8Kv, start spraying and in receiving liquid cooling drop microballoon fast.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon obtained is placed in Muffle furnace under inert gas shielding, be warming up to 800 DEG C by the programming rate of 6 DEG C/min and keep within 4 hours, namely obtaining black light graphite alkene aerogel microball.Average grain diameter is 180 μm, and density is 4.5kg/m
3.
Embodiment 5
(1) graphite oxide is prepared: the HUMMER method of native graphite through improving is prepared as graphite oxide.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, the graphite oxide that the HUMMER legal system improved by 0.2mg is standby and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 200W ultrasonic disperse 20min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 2mg/ml.
(3) trash ice is placed in the good uncovered Dewar bottle of insulation, adds sodium chloride powder, the formation trash ice that stirs/sodium chloride cools down bath.The beaker that n-hexane and toluene are housed is put into trash ice/sodium chloride cools down bath as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 2mg/ml prepared is loaded in the syringe on ultrasonic spray apparatus, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, adjustments supersonic frequency is 20kHz, starts spraying and cool drop microballoon fast in receiving liquid.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon 800W microwave power irradiation heat reduction 1min under inert gas shielding will obtained, namely obtains black light graphite alkene aerogel microball.Average grain diameter is 118 μm, and density is 1.2kg/m
3.
Embodiment 6
(1) graphite oxide is prepared: the HUMMER method of native graphite through improving is prepared as graphite oxide.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, the graphite oxide that the HUMMER legal system improved by 0.15mg is standby and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 200W ultrasonic disperse 20min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 1.5mg/ml.
(3) acetone is placed in the good uncovered Dewar bottle of insulation, adds dry ice fragment while stirring, until substantially cannot stir, namely define the dry ice/acetone cooling bath of thickness.The beaker that first benzene and heptane is housed is put into dry ice/acetone cooling bath cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 1.5mg/ml prepared is loaded in the pressure chamber on press atomization device, regulate sprinkler height to make it to be separated by with receiving liquid after suitable distance, open compression pump and be adjusted to 10Mpa, start spraying and in receiving liquid cooling drop microballoon fast.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon 700W microwave power irradiation heat reduction 5min under inert gas shielding will obtained, namely obtains black light graphite alkene aerogel microball.Average grain diameter is 340 μm, and density is 1.4kg/m
3.
Embodiment 7
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through Brodie oxidizing process.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, by graphite oxide standby for 0.85gBrodie legal system and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 400W ultrasonic disperse 40min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 8.5mg/ml.
(3) trash ice is placed in the good uncovered Dewar bottle of insulation, adds sodium chloride powder, the formation trash ice that stirs/sodium chloride cools down bath.The beaker that n-hexane and ethyl acetate are housed is put into trash ice/sodium chloride cools down bath to cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 8.5mg/ml prepared is loaded in the syringe on ultrasonic spray apparatus, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, adjustments supersonic frequency is 60kHz, starts spraying and cool drop microballoon fast in receiving liquid.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon 700W microwave power irradiation heat reduction 3min under inert gas shielding will obtained, namely obtains black light graphite alkene aerogel microball.Average grain diameter is 47 μm, and density is 7.1kg/m
3.
Embodiment 8
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through Brodie oxidizing process.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, by graphite oxide standby for 0.05gBrodie legal system and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 200W ultrasonic disperse 20min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 0.5mg/ml.
(3) acetone is placed in the good uncovered Dewar bottle of insulation, adds dry ice fragment while stirring, until substantially cannot stir, namely define the dry ice/acetone cooling bath of thickness.The beaker that ethyl acetate and toluene are housed is put into dry ice/acetone cooling bath cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 0.5mg/ml prepared is loaded in the syringe on electrostatic atomizer, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, regulation voltage is 5Kv, start spraying and in receiving liquid cooling drop microballoon fast.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon 800W microwave power irradiation heat reduction 7min under inert gas shielding will obtained, namely obtains black light graphite alkene aerogel microball.Average grain diameter is 220 μm, and density is 0.35kg/m
3.
Embodiment 9
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through Staudemaier oxidizing process.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, by graphite oxide standby for 0.35gStaudemaier legal system and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 400W ultrasonic disperse 25min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 3.5mg/ml.
(3) ethyl acetate is placed in the good uncovered Dewar bottle of insulation, adds a large amount of liquid nitrogen while stirring, until form the liquid nitrogen/ethyl acetate cooling bath of slush shape.The beaker that n-hexane and normal heptane are housed is put into liquid nitrogen/ethyl acetate cooling bath to cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 3.5mg/ml prepared is loaded in the pressure chamber on press atomization device, regulate sprinkler height to make it to be separated by with receiving liquid after suitable distance, open compression pump and be adjusted to 200Mpa, start spraying and in receiving liquid cooling drop microballoon fast.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon obtained is placed in Muffle furnace under inert gas shielding, be warming up to 800 DEG C by the programming rate of 10 DEG C/min and keep within 2 hours, namely obtaining black light graphite alkene aerogel microball.Average grain diameter is 45 μm, and density is 2.3kg/m
3.
Embodiment 10
(1) graphite oxide is prepared: native graphite is prepared as graphite oxide through Staudemaier oxidizing process.
(2) graphene oxide aqueous dispersions is prepared: under room temperature, by graphite oxide standby for 2gStaudemaier legal system and the mixing of 100ml deionized water, be placed in ultrasonic washing instrument, stir after 400W ultrasonic disperse 50min and spend the night, obtain the graphene oxide aqueous dispersions be uniformly dispersed in dark-brown 20mg/ml.
(3) trash ice is placed in the good uncovered Dewar bottle of insulation, adds sodium chloride powder, the formation trash ice that stirs/sodium chloride cools down bath.The beaker that n-hexane and normal heptane are housed is put into trash ice/sodium chloride cools down bath to cool as receiving liquid.Simultaneously, the graphene oxide aqueous dispersions of the 20mg/ml prepared is loaded in the syringe on electrostatic atomizer, regulate syringe nozzle height to make it to be separated by with receiving liquid after suitable distance, regulation voltage is 20Kv, start spraying and in receiving liquid cooling drop microballoon fast.
(4) obtain brownish black graphene oxide ice microballoon by sieve fast filtering receiving liquid, proceed in freeze drier, at vacuum 20Pa, under temperature-50 DEG C of conditions, dry 24h obtains brown oxidation graphene aerogel microballoon.
(5) the graphite oxide aerogel microballoon obtained is placed in Muffle furnace under inert gas shielding, be warming up to 800 DEG C by the programming rate of 8 DEG C/min and keep within 4 hours, namely obtaining black light graphite alkene aerogel microball.Average grain diameter is 176 μm, and density is 16.7kg/m
3.
Application example 1
Take graphene aerogel microballoon 100mg prepared by embodiment 3, putting into laboratory, to common are machine solvent be acetone, toluene, oxolane, adsorbs 10min to after saturated in Isosorbide-5-Nitrae dioxane and chloroform, take the quality of having adsorbed microballoon after organic solvent, be respectively 6.2g, 8.7g, 9.1g, 15.2g and 17.9g, therefore adsorbance is respectively 6.1g, 8.6g, 9.0g, 15.1g and 17.8g.61g/g is respectively, 86g/g, 90g/g, 151g/g and 178g/g by the adsorption capacity Q calculating microballoon.Shown in Fig. 4.Result shows, graphene aerogel microballoon has excellent adsorption capacity to organic solvent.
Application example 2
Take graphene aerogel microballoon 100mg prepared by embodiment 4, putting into the common oils of environmental pollution that easily causes is diesel oil, gasoline, adsorbs 10-15min to after saturated in waste vegetable oil and pump oil, take the quality of having adsorbed microballoon after oil product, be respectively 8.8g, 8.0g, 10.0g and 10.6g, therefore adsorbance is respectively 8.7g, 7.9g, 9.9g and 10.5g.87g/g is respectively, 79g/g, 99g/g and 105g/g by the adsorption capacity Q calculating microballoon.Result shows, graphene aerogel microballoon has excellent adsorption capacity to oils.
Claims (8)
1. a graphene aerogel microballoon, is characterized in that the initiation material of this graphene aerogel microballoon is made up of following component, counts by weight:
Deionized water 100 parts
Graphite oxide 0.05-2 part.
2. the preparation method of graphene aerogel microballoon according to claim 1, is characterized in that the method comprises the steps:
(1) preparation of graphite oxide
Native graphite is prepared into graphite oxide through chemical oxidization method, and wherein chemical oxidization method is Brodie oxidizing process, Staudemaier oxidizing process, any one in the Hummer method of Hummer method or improvement;
(2) preparation of graphene oxide aqueous dispersions
By deionized water 100 parts, be prepared into dispersion liquid through 200-400W ultrasonic stripping 20-50min after graphite oxide 0.05-2 part Homogeneous phase mixing, concentration is 0.5-20mg/mL;
(3) by spray-on process, graphene oxide aqueous dispersions is atomized into graphene oxide drop microballoon, and the receiving liquid being placed in cooling bath is collected, wherein, spray-on process is press atomization, any one in ullrasonic spraying or electrostatic spray;
(4) filter above-mentioned receiving liquid and obtain graphene oxide ice microballoon, after freeze drying, obtain graphite oxide aerogel microballoon;
(5) above-mentioned graphite oxide aerogel microballoon is obtained graphene aerogel microballoon by thermal reduction.
3. the preparation method of graphene aerogel microballoon according to claim 2, it is characterized in that the pressure of press atomization is 10-200Mpa, the ultrasonic power of ullrasonic spraying is 10-150kHz, and the voltage of electrostatic spray is 5-20kv.
4. the preparation method of graphene aerogel microballoon according to claim 2, is characterized in that cooling bath is ice/sodium chloride bath, any one in dry ice/acetone batch or liquid nitrogen/ethyl acetate bath.
5. the preparation method of graphene aerogel microballoon according to claim 2, is characterized in that receiving liquid is ethyl acetate, toluene, at least one in n-hexane and normal heptane.
6. the preparation method of graphene aerogel microballoon according to claim 2, is characterized in that thermal reduction is the intensification thermal reduction of Muffle furnace Program or microwave irradiation thermal reduction under inert gas shielding.
7. the preparation method of graphene aerogel microballoon according to claim 6, is characterized in that temperature programming thermal reduction is that 5-10 DEG C/min is warming up to 800 DEG C, and keeps 2-5h; Microwave irradiation thermal reduction is that power is 600-800W and keeps 1-10min.
8. the purposes of graphene aerogel microballoon according to claim 1, is characterized in that this graphene aerogel microballoon adsorbs for environmental contaminants.
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