CN103274384B - Graphene oxide reinforced carbon aerogel material, and preparation method and application thereof - Google Patents
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Abstract
The invention belongs to the field of material preparation, and discloses a graphene oxide reinforced carbon aerogel material, and a preparation method and an application thereof. The preparation method of the material comprises the following steps of, by weight, dissolving 40-20 parts of resorcinol in 80-95 parts of purified water, adding 0.008-0.07 part of a catalyst, mixing the above materials, adding 10-40 parts of a graphene oxide aqueous solution with a mass percentage of 1%; finally adding 6-29 parts of a formaldehyde solution, sealing a gel, drying the gel to obtain a xerogel, and carbonizing the xerogel, so that the graphene oxide reinforced carbon aerogel material is obtained. The preparation method is in no need of solvent exchange, thereby reducing energy consumption. Besides, the time needed by the whole preparation process is shorter than that of a common preparation method; and the process is simpler. Moreover, the carbon aerogel material with low density (the lowest density can reach 0.02g/cm<-3>) and high specific surface area (the highest specific surface area can reach 1,100 m<2>)/g) can be obtained with no need of carbon dioxide supercritical drying.
Description
Technical field
The invention belongs to field of material preparation, particularly a kind of graphene oxide strengthens carbon aerogels material and preparation method thereof and application.
Background technology
Carbon aerogels material refers to a kind of low density, the high porosity carbon material that are obtained by carbonization organogel.It is widely used in the fields such as absorption, catalysis, battery electrode material and super capacitor.Carbon gel based on resorcinol-formaldehyde (RF) is used widely owing to having high porosity, low-resistivity, high-specific surface area, excellent electric conductivity and thermostability and physical strength.Preparing the common method of carbon aerogels by RF gel is with 1:2 mixed in molar ratio by Resorcinol and formaldehyde, add catalyzer as salt of wormwood, acetic acid etc., configure certain density solution and be obtained by reacting wet gel under certain temperature, after wet gel falls the water in wet gel by exchange of solvent after, supercritical co drying or lyophilize obtain xerogel, carbonization obtains carbon aerogels.But this preparation method's required time is long, from gel to exchange of solvent, need 5-8 days time to drying process.In addition, if need the carbon gel obtaining low density, high-specific surface area, prepare RF concentration in wet gel process can not be too high, thus cause the frame strength of RF gel lower.The words of convection drying cause subsiding of duct in gel compared with conference due to the surface tension of water, and the carbon gel shrinks obtained is comparatively large, and after therefore needing exchange of solvent, supercritical co is dry, and this makes energy consumption and cost significantly increase.
Summary of the invention
In order to overcome the shortcoming of prior art with not enough, primary and foremost purpose of the present invention is to provide graphene oxide and strengthens carbon aerogels material.
Another object of the present invention is to provide described graphene oxide to strengthen the preparation method of carbon aerogels.
Another object of the present invention is to provide described graphene oxide to strengthen the application of carbon aerogels material.
Object of the present invention is achieved through the following technical solutions:
Graphene oxide strengthens a preparation method for carbon aerogels material, comprises the following steps:
By weight, the Resorcinol of 4 ~ 20 parts is dissolved in 80 ~ 95 parts of pure water, after adding the catalyst mix of 0.008 ~ 0.07 part, adding 10 ~ 40 parts of massfractions is the graphene oxide water solution of 1%, finally add 6 ~ 29 parts of formaldehyde solutions, sealing gel, drying obtains xerogel, strengthens carbon aerogels by obtaining graphene oxide after xerogel carbonization.
Described catalyzer is basic catalyst or an acidic catalyst.
Described an acidic catalyst is oxalic acid, acetic acid, hydrochloric acid or phosphoric acid; Described basic catalyst is salt of wormwood, sodium carbonate, potassium hydroxide or sodium hydroxide;
Preferred an acidic catalyst is hydrochloric acid; Preferred basic catalyst is sodium carbonate or salt of wormwood.
The massfraction of described formaldehyde solution is 37%; The temperature of described sealing gel is 50 DEG C ~ 85 DEG C, and the time is 1 ~ 3 day; Described drying is lyophilize.
Described carbonization is at 500 ~ 1000 DEG C, carbonization 2 ~ 5h under protection of inert gas, and wherein said rare gas element is nitrogen or argon gas.
The preparation process of described graphene oxide is: by weight, by Powdered natural graphite 1 part, and SODIUMNITRATE 0.3 ~ 0.7 part of combination cooling to 0 DEG C, then stir 0.3 ~ 0.7h after dripping 35 ~ 45 parts of vitriol oils, and keep the temperature 0 ~ 5 DEG C of reaction system; Then, add 0.2 ~ 0.5 part of potassium permanganate and fully stir 0.3 ~ 0.7h, keep temperature of reaction system 5 ~ 10 DEG C simultaneously; In 1h, add 3 ~ 4 parts of potassium permanganate again, keep temperature of reaction system 15 ~ 20 DEG C, withdraw cryostat, Heating temperature to 30 ~ 40 DEG C, and fully stir 2h ~ 3h, obtain brown suspension, drip 40 ~ 50 parts of water in reacting 10 ~ 20min at 85 ~ 95 DEG C of temperature, having reacted in backward suspension the massfraction adding 2 ~ 4 parts is the H of 30%
2o
2, obtain glassy yellow graphite oxide dispersion after the pure water of 20 ~ 30 parts, dispersion liquid filter, centrifugal, removing supernatant liquor, the water of 100 parts used successively by solid, 100 parts of massfractions are the cleaning of 30%HCl solution, after 100 parts of ethanol purge twice, after centrifuge washing with 100 parts of petroleum ether precipitations filter after drying oxide yellow Graphene solid.
The graphene oxide prepared by preparation method described above strengthens a carbon aerogels material, and the density of this gelatinous material is 0.02 ~ 0.07g/cm
-2, specific surface area is 700 ~ 1100m
2/ g, oil number is 21 ~ 70 times of own wt.
Graphene oxide described above strengthens the application of carbon aerogels material in absorption and catalysis technical field.
The present invention has following advantage and effect relative to prior art:
(1) the present invention by adding graphene oxide in RF gel, the intensity of RF wet gel is enhanced, and graphene oxide is reduced into Graphene through Resorcinol, add the hydrophobicity of gel, thus gel its pore passage structure under lyophilize is maintained and gel more easily drying.
(2) the present invention does not need through exchange of solvent, thus reduces energy consumption, and the more common preparation method of whole preparation process required time is shorter, and technique is more simple.In addition do not need CO 2 supercritical drying can obtain low density and (be low to moderate 0.02g/cm most
-3), high-specific surface area (is up to 1100m
2/ g) carbon aerogels.
(3) graphene oxide that prepared by the present invention strengthens carbon aerogels material and has excellent absorption property, and oil number can reach 21 ~ 70 times of sole mass.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of graphene oxide prepared by Graphene and embodiment 1.
Fig. 2 is the Scanning Electron microscope figure that the Graphene prepared of embodiment 1-4 strengthens carbon aerogels (GCA-1 ~ GCA5) and carbon aerogels (CA).
Fig. 3 is the transmission electron microscope picture of Graphene enhancing carbon aerogels (GCA-1) prepared by embodiment 1.
Embodiment
Below in conjunction with embodiment and Figure of description, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) by weight, by Powdered natural graphite 1 part, SODIUMNITRATE 0.5 part adds in reactor and is cooled to 0 DEG C; Again 40 parts of vitriol oils are slowly added in reactor and fully stir 0.5h, and keep the temperature 0 ~ 5 DEG C of reaction system; Then, 0.3 part of potassium permanganate is added in reactor and also fully stir 0.5h, keep temperature of reaction system 5 ~ 10 DEG C simultaneously; In 1h, then 3.5 parts of potassium permanganate are slowly added in reactor, keep temperature of reaction system 15 ~ 20 DEG C, withdraw cryostat, with water-bath, reaction system is heated to 35 DEG C, and fully stirs 2h, obtain brown suspension.Slowly be added dropwise in brown suspension by 45 parts of pure water, and react 15min at 90 DEG C of temperature, having reacted in backward suspension the massfraction adding 3 parts is the H of 30%
2o
2pure water with 20 parts obtains glassy yellow graphite oxide dispersion.Centrifugation after dispersion liquid filtration, removing supernatant liquor, the water of 100 parts used successively by solid, and 100 parts of massfractions are after the cleaning of 30%HCl solution, and 100 parts of ethanol purge twice, filter with 100 parts of petroleum ether precipitations and obtain oxide yellow Graphene solid after drying.
(2) by weight, be added in 99 parts of pure water by graphene oxide 1 part made for step (1), after 2000rpm centrifugation 8min, removing insolubles after ultrasonic 2h, namely to obtain massfraction be 1% graphene oxide water solution.
(3) by weight, the Resorcinol of 4 parts is dissolved in after in 95 parts of pure water and adds 0.008 part, sodium carbonate, add obtained 1% graphene oxide water solution 10 parts of step (2) after mixing, finally adding massfraction is that at being sealed in 60 DEG C after 37% formaldehyde solution 6 parts mixes, gel 2 days postlyophilizations obtain xerogel GOR-1.The same GOR-1 of preparation method of OR, difference is not add 1% graphene oxide water solution inside OR.
(4) xerogel OR and GOR-1 step (3) obtained is in 750 DEG C, and the lower carbonization 3h of argon gas protection can obtain graphene oxide and strengthen carbon aerogels material GCA-1 and carbon aerogels material C A.Its density is respectively 0.45 and 0.02g/cm
-2, specific surface area is respectively 125 and 1100m
2/ g.
Specific surface area is obtained by BET method, and density obtains according to the quality of the carbon gel of measurement rules shape and volume computing: density=mass/volume.
Embodiment 2
(1) by weight, by Powdered natural graphite 1 part, SODIUMNITRATE 0.3 part adds in reactor and is cooled to 0 DEG C; Again 45 parts of vitriol oils are slowly added in reactor and fully stir 0.7h, and keep the temperature 0 ~ 5 DEG C of reaction system; Then, 0.5 part of potassium permanganate is added in reactor and also fully stir 0.3h, keep temperature of reaction system 5 ~ 10 DEG C simultaneously; In 1h, then 4 parts of potassium permanganate are slowly added in reactor, keep temperature of reaction system 15 ~ 20 DEG C, withdraw cryostat, with water-bath, reaction system is heated to 40 DEG C, and fully stirs 2h, obtain brown suspension.50 parts of pure water are slowly added dropwise in brown suspension, and in reacting 10min at 95 DEG C of temperature, having reacted in backward suspension the massfraction adding 2 parts is the H of 30%
2o
2pure water with 30 parts obtains glassy yellow graphite oxide dispersion.Centrifugation after dispersion liquid filters, removing supernatant liquor, 100 parts of water used successively by solid, and 100 parts of massfractions are the HCl solution cleaning of 30%, after 100 parts of ethanol purge twice, filter to obtain oxide yellow Graphene solid with 100 parts of petroleum ether precipitations.
(2) by weight, be added in 99 parts of pure water by graphene oxide 1 part made for step (1), after 2500rpm centrifugation 5min, removing insolubles after ultrasonic 1h, to obtain massfraction be 1% graphene oxide water solution.
(3) by weight, the Resorcinol of 6 parts is dissolved in after in 90 parts of pure water and adds oxalic acid 0.012 part, add 1% graphene oxide water solution 24 parts that step (2) is made after mixing, finally adding massfraction is that at being sealed in 50 DEG C after 37% formaldehyde solution 9 parts mixes, gel 3 days postlyophilizations obtain xerogel GOR-2.
(4) xerogel step (3) obtained is in 500 DEG C, and the lower carbonization 5h of argon gas protection can obtain graphene oxide and strengthen carbon aerogels material GCA-2.Its density is 0.035/cm
-2, specific surface area is 755m
2/ g.
Embodiment 3
(1) by weight, by Powdered natural graphite 1 part, SODIUMNITRATE 0.7 part adds in reactor and is cooled to 0 DEG C; Again 35 parts of vitriol oils are slowly added in reactor and fully stir 0.3h, and keep the temperature 0 ~ 5 DEG C of reaction system; Then, 0.2 part of potassium permanganate is added in reactor and also fully stir 0.7h, keep temperature of reaction system 5 ~ 10 DEG C simultaneously; In 1h, then 3 parts of potassium permanganate are slowly added in reactor, keep temperature of reaction system 15 ~ 20 DEG C, withdraw cryostat, with water-bath, reaction system is heated to 30 DEG C, and fully stirs 3h, obtain brown suspension.40 parts of pure water are slowly added dropwise in brown suspension, and in reacting 20min at 85 DEG C of temperature, have reacted in backward suspension the 30%H adding 4 parts
2o
2pure water with 20 parts obtains glassy yellow graphite oxide dispersion.Centrifugation after dispersion liquid filters, removing supernatant liquor, solid 100 parts of water successively, 100 parts of massfractions are that after the HCl solution cleaning of 30%, with 100 parts of ethanol purge twice, rear use 100 parts of petroleum ether precipitations filter to obtain oxide yellow Graphene solid.
(2) by weight, be added in 99 parts of pure water by graphene oxide 1 weight part made for step (1), after 3000rpm centrifugation 4min, removing insolubles after ultrasonic 3h, to obtain massfraction be 1% graphene oxide water solution.
(3) by weight, the Resorcinol of 20 parts is dissolved in after in 80 parts of pure water and adds 0.07 part, sodium carbonate, add 1% graphene oxide water solution 40 parts that step (2) is made after mixing, finally adding massfraction is that at being sealed in 85 DEG C after 37% formaldehyde solution 29 parts mixes, gel 1 day postlyophilization obtains xerogel GOR-3.
(4) xerogel step (3) obtained is in 1000 DEG C, and the lower carbonization 2h of nitrogen gas protection can obtain graphene oxide and strengthen carbon aerogels material GCA-3.Its density is 0.07g/cm
-2, specific surface area is 700m
2/ g.
Embodiment 4
(1) by weight, by Powdered natural graphite 1 part, SODIUMNITRATE 0.6 part adds in reactor and is cooled to 0 DEG C; Again 37 parts of vitriol oils are slowly added in reactor and fully stir 0.5h, and keep the temperature 0 ~ 5 DEG C of reaction system; Then, 0.5 part of potassium permanganate is added in reactor and also fully stir 0.5h, keep temperature of reaction system 5 ~ 10 DEG C simultaneously; In 1h, then 3.2 parts of potassium permanganate are slowly added in reactor, keep temperature of reaction system 15 ~ 20 DEG C, withdraw cryostat, with water-bath, reaction system is heated to 35 DEG C, and fully stirs 2h, obtain brown suspension.46 parts of pure water are slowly added dropwise in brown suspension, and in reacting 12min at 90 DEG C of temperature, having reacted in backward suspension the massfraction adding 3.2 parts is 30%H
2o
2pure water with 25 parts obtains glassy yellow graphite oxide dispersion.Centrifugation after dispersion liquid filters, removing supernatant liquor, 100 parts of pure water used successively by solid, and 100 parts of massfractions are that after the HCl solution cleaning of 30%, 100 parts of ethanol purge twice, filter to obtain oxide yellow Graphene solid with 100 parts of petroleum ether precipitations.
(2) by weight, be added in 99 parts of pure water by graphene oxide 1 part made for step (1), after 2500rpm centrifugation 6min, removing insolubles after ultrasonic 3h, to obtain massfraction be 1% graphene oxide water solution.
(3) by weight, the Resorcinol of 10 parts is dissolved in after in 90 parts of pure water and adds 0.02 part, salt of wormwood, add 1% graphene oxide water solution 20 parts that step (2) is made after mixing, finally adding massfraction is that at being sealed in 85 DEG C after 37% formaldehyde solution 15 parts mixes, gel 1 day postlyophilization obtains xerogel GOR-4.Prepare xerogel GOR-5 as stated above, the difference of itself and GOR-4 is: the made 1% graphene oxide water solution add-on of step (2) is 10 parts, other materials and the same GOR-4 of step.
(4) xerogel step (3) obtained is in 750 DEG C, and the lower carbonization 5h of nitrogen gas protection can obtain graphene oxide and strengthen carbon aerogels material GCA-4 and graphene oxide enhancing carbon aerogels material GCA-5.Its density is respectively 0.05 and 0.03g/cm
-2, specific surface area is respectively 700 and 760m
2/ g.
Wherein, the natural graphite that embodiment 1-4 is used is bought in Qingdao Heng Li get graphite company limited.
Effect example
(1) graphene oxide that step (1) in embodiment 1 obtains is carried out examination of infrared spectrum, obtain the infrared signature absorption peak of typical oxidation Graphene, its result as shown in Figure 1.
Wherein: wherein 3650cm
-1the strong absorption peak at place is the stretching vibration peak of hydroxyl, 3100cm
-1the absorption peak at place is graphene oxide carbon skeleton C-H absorption peak, 1732cm
-1for the absorption peak of carbonyl, 1573 is the absorption peak of graphene carbon skeleton, and 1216 is the absorption peak of C-O.Can observe from Fig. 1, after Graphene oxidation, occur 3650,3100,1732,1216cm
-1the absorption peak that a few place is new, this several places absorption peak is the typical absorption peak of graphene oxide, all on Graphene skeleton, introduces Sauerstoffatom and caused.
(2) the carbon gelatinous material obtained in embodiment 1-4 is carried out scanning electron microscope test, its result as shown in Figure 2.Graphene oxide has obvious enhancement to carbon gel as can be seen from Figure 2.The carbon gel strengthened through Graphene is as good in GCA-1 ~ GCA-5 duct pattern, and tunnel collapse degree is low, its vesicular structure is maintained, shrinks little; And the carbon gel that not oxidised Graphene strengthens as CA because the structural strength of gel is low, in dry and carbonization process gel shrinks large, there is the phenomenon of luming.
(3) the carbon aerogels GCA-1 obtained in enforcement 1 is carried out transmission electron microscope observation, its result as shown in Figure 3.The vesicular structure of graphene film Rotating fields and carbon aerogels clearly can be found out from Fig. 3.
(4) the carbon gelatinous material obtained by 1-4 in embodiment carries out the test of the performance of adsorbed oil type organic, its concrete steps are, 6 kinds of carbon gels (CA, GCA-1, GCA-2, GCA-3, GCA-4, GCA-5) are placed in chloroform, perhydronaphthalene, toluene, Virahol oils organism respectively, adsorb the quality of carbon gel before and after saturated rear record absorption, the quality before its absorption multiple=(quality before the quality-absorption after absorption)/absorption.It the results are shown in Table 1.
The Graphene of table 1 embodiment 1 ~ 4 strengthens the density of what is said or talked about gelatinous material and adsorbs organic performance
Graphene strengthens the adsorbed oil type organic performance that carbon aerogels material has excellence as can be seen from Table 1, and its highest adsorbed oil reaches 70 times of own wt.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. graphene oxide strengthens a preparation method for carbon aerogels material, it is characterized in that: comprise the following steps:
By weight, the Resorcinol of 4 ~ 20 parts is dissolved in 80 ~ 95 parts of pure water, after adding the catalyst mix of 0.008 ~ 0.07 part, adding 10 ~ 40 parts of massfractions is the graphene oxide water solution of 1%, finally add 6 ~ 29 parts of formaldehyde solutions, sealing gel, drying obtains xerogel, strengthens carbon aerogels by obtaining graphene oxide after xerogel carbonization;
The massfraction of described formaldehyde solution is 37%; The temperature of described sealing gel is 50 DEG C ~ 85 DEG C, and the time is 1 ~ 3 day; Described drying is lyophilize;
Described carbonization is at 500 ~ 1000 DEG C, carbonization 2 ~ 5h under protection of inert gas;
The density that this graphene oxide strengthens carbon aerogels is 0.02 ~ 0.07g/cm
3, specific surface area is 700 ~ 1100m
2/ g, oil number is 21 ~ 70 times of own wt.
2. preparation method according to claim 1, is characterized in that: described catalyzer is basic catalyst or an acidic catalyst.
3. preparation method according to claim 2, is characterized in that: described an acidic catalyst is oxalic acid, acetic acid, hydrochloric acid or phosphoric acid; Described basic catalyst is salt of wormwood, sodium carbonate, potassium hydroxide or sodium hydroxide.
4. preparation method according to claim 3, is characterized in that: described an acidic catalyst is hydrochloric acid; Described basic catalyst is sodium carbonate or salt of wormwood.
5. preparation method according to claim 1, is characterized in that: described rare gas element is nitrogen or argon gas.
6. preparation method according to claim 1, it is characterized in that: the preparation process of described graphene oxide is: by weight, by Powdered natural graphite 1 part, SODIUMNITRATE 0.3 ~ 0.7 part of combination cooling to 0 DEG C, stir 0.3 ~ 0.7h after dripping 35 ~ 45 parts of vitriol oils again, and keep the temperature 0 ~ 5 DEG C of reaction system; Then, add 0.2 ~ 0.5 part of potassium permanganate and fully stir 0.3 ~ 0.7h, keep temperature of reaction system 5 ~ 10 DEG C simultaneously; In 1 h, add 3 ~ 4 parts of potassium permanganate again, keep temperature of reaction system 15 ~ 20 DEG C, Heating temperature to 30 ~ 40 DEG C, and fully stir 2 h ~ 3h, obtain brown suspension, drip 40 ~ 50 parts of water in reacting 10 ~ 20 min at 85 ~ 95 DEG C of temperature, having reacted in backward suspension the massfraction adding 2 ~ 4 parts is the H of 30%
2o
2, obtain glassy yellow graphite oxide dispersion after the pure water of 20 ~ 30 parts, dispersion liquid filter, centrifugal, removing supernatant liquor, the water of 100 parts used successively by solid, 100 parts of massfractions are 30% HCl solution cleaning, after 100 parts of ethanol purge twice, after centrifuge washing with 100 parts of petroleum ether precipitations filter after drying oxide yellow Graphene solid.
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