CN103274384A - Graphene oxide reinforced carbon aerogel material, and preparation method and application thereof - Google Patents
Graphene oxide reinforced carbon aerogel material, and preparation method and application thereof Download PDFInfo
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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
The carbon aerogels material refers to a kind of low density, the high porosity carbon material that obtain by the carbonization organogel.It is widely used in fields such as absorption, catalysis, battery electrode material and super capacitor.Be used widely owing to having high porosity, low-resistivity, high-specific surface area, excellent electric conductivity and thermostability and physical strength based on the carbon gel of Resorcinol-formaldehyde (RF).Be with the 1:2 mixed in molar ratio with Resorcinol and formaldehyde by the common method of RF preparing gel carbon aerogels, add catalyzer such as salt of wormwood, acetic acid etc., dispose certain density solution and react under certain temperature and obtain wet gel, carbonization obtained carbon aerogels after wet gel fell behind the water in the wet gel supercritical co drying or lyophilize and obtains xerogel by exchange of solvent.But this preparation method's required time is long, needs 5-8 days time to drying process from the gel to the exchange of solvent.In addition, obtain the carbon gel of low density, high-specific surface area if desired, RF concentration can not be too high in preparation wet gel process, thereby cause the frame strength of RF gel lower.The words of convection drying are because the surface tension of water causes subsiding of duct in the gel than conference, and the carbon gel that obtains shrinks bigger, therefore need supercritical co drying after the exchange of solvent, and this makes energy consumption and cost significantly increase.
Summary of the invention
For the shortcoming and deficiency that overcome prior art, primary and foremost purpose of the present invention provides graphene oxide and strengthens the carbon aerogels material.
Another object of the present invention is to provide described graphene oxide to strengthen the preparation method of carbon aerogels.
A further object of the present invention is to provide described graphene oxide to strengthen the application of carbon aerogels material.
Purpose of the present invention is achieved through the following technical solutions:
A kind of graphene oxide strengthens the carbon aerogels preparation methods, may further comprise the steps:
By weight, 4～20 parts Resorcinols are dissolved in 80～95 parts of pure water, after adding 0.008～0.07 part catalyst mix, add 10～40 parts of massfractions and be 1% graphite oxide aqueous solution, add 6～29 parts of formaldehyde solutions at last, the sealing gel, drying obtains xerogel, strengthens carbon aerogels with obtaining graphene oxide after the 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, yellow soda ash, potassium hydroxide or sodium hydroxide;
Preferred an acidic catalyst is hydrochloric acid; Preferred basic catalyst is yellow soda ash or salt of wormwood.
The massfraction of described formaldehyde solution is 37%; The temperature of described sealing gel is 50 ℃～85 ℃, and the time is 1～3 day; Described drying is lyophilize.
Described carbonization is at 500～1000 ℃, and carbonization 2～5h under the protection of inert gas, wherein said rare gas element are nitrogen or argon gas.
The preparation process of described graphene oxide is: by weight, with 1 part of Powdered natural graphite, 0.3～0.7 part of mixing of SODIUMNITRATE is cooled to 0 ℃, stirs 0.3～0.7h behind part vitriol oil of Dropwise 35～45 again, and keeps 0～5 ℃ of the temperature of reaction system; Then, add 0.2～0.5 part of potassium permanganate and fully stir 0.3～0.7h, keep 5～10 ℃ of temperature of reaction system simultaneously; In 1h, add 3～4 parts of potassium permanganate again, keep 15～20 ℃ of temperature of reaction system, withdraw cryostat, Heating temperature to 30～40 ℃, and fully stir 2h～3h, obtain brown suspension, drip 40～50 parts of water in react 10～20min under 85～95 ℃ of temperature, having reacted the back, to add 2～4 parts massfraction in the suspension be 30% H
2O
2, obtain glassy yellow graphite oxide dispersion liquid behind 20～30 parts the pure water, dispersion liquid filtration, centrifugal, remove supernatant liquor, solid is used 100 parts water successively, 100 parts of massfractions clean for 30%HCl solution, after 100 parts of ethanol clean twice, get oxide yellow Graphene solid after drying with 100 parts of petroleum ether precipitations filtrations behind the centrifuge washing.
A kind of graphene oxide that is prepared by preparation method described above strengthens the 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 with respect to prior art:
(1) the present invention is by adding graphene oxide in the RF gel, the intensity of RF wet gel is enhanced, and graphene oxide is reduced into Graphene through Resorcinol, has increased the hydrophobicity of gel, thereby gel its pore passage structure under lyophilize is maintained and the easier drying of gel.
(2) the present invention does not need through exchange of solvent, thereby cuts down the consumption of energy, and the more common preparation method of whole process of preparation required time is shorter, and technology is more simple.Do not need the CO 2 supercritical drying can obtain low density in addition 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 of the present invention's preparation strengthens the absorption property that the carbon aerogels material has excellence, and oil number can reach 21～70 times of sole mass.
Description of drawings
Fig. 1 is the infrared spectrogram of the graphene oxide of Graphene and embodiment 1 preparation.
Fig. 2 strengthens carbon aerogels (the surface sweeping electron microscope picture of GCA-1～GCA5) and carbon aerogels (CA) for the Graphene of embodiment 1-4 preparation.
Fig. 3 is the transmission electron microscope picture that the Graphene of embodiment 1 preparation strengthens carbon aerogels (GCA-1).
Embodiment
The present invention is described in further detail below in conjunction with embodiment and Figure of description, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) by weight, with 1 part of Powdered natural graphite, be cooled to 0 ℃ in 0.5 part of adding of SODIUMNITRATE reactor; Again 40 parts of vitriol oils are slowly added in the reactor and fully to stir 0.5h, and keep 0～5 ℃ of the temperature of reaction system; Then, add in the reactor 0.3 part of potassium permanganate and the abundant 0.5h of stirring, keep 5～10 ℃ of temperature of reaction system simultaneously; In 1h, again 3.5 parts of potassium permanganate are slowly added in the reactor, keep 15～20 ℃ of temperature of reaction system, withdraw cryostat, with water-bath reaction system is heated to 35 ℃, and fully stirs 2h, obtain brown suspension.45 parts of pure water slowly are added dropwise in the brown suspension, and react 15min under 90 ℃ of temperature, having reacted the back, to add 3 parts massfraction in the suspension be 30% H
2O
2Obtain glassy yellow graphite oxide dispersion liquid with 20 parts pure water.Dispersion liquid filters the back centrifugation, removes supernatant liquor, and solid is used 100 parts water successively, and 100 parts of massfractions are for after 30%HCl solution cleans, and 100 parts of ethanol clean twice, filter with 100 parts of petroleum ether precipitations and get oxide yellow Graphene solid after drying.
(2) by weight, the graphene oxide that step (1) is made is added in 99 parts of pure water for 1 part, and ultrasonic 2h removes insolubles after by 2000rpm centrifugation 8min, and namely to get massfraction be 1% graphite oxide aqueous solution.
(3) by weight, add 0.008 part in yellow soda ash after being dissolved in 4 parts Resorcinols in 95 parts of pure water, mix the back and add 10 parts of the obtained 1% graphite oxide aqueous solutions of step (2), adding massfraction at last is to be sealed in 2 days postlyophilizations of 60 ℃ of following gels after 6 parts of 37% formaldehyde solutions mix to obtain xerogel GOR-1.The same GOR-1 of the preparation method of OR, difference is that the OR the inside does not add 1% graphite oxide aqueous solution.
(4) the xerogel OR that step (3) is obtained and GOR-1 are in 750 ℃, and argon gas protection carbonization 3h down can obtain graphene oxide enhancing 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 obtains by the BET method, density according to measuring gage then quality and the volume calculation of the carbon gel of shape obtain: density=mass/volume.
Embodiment 2
(1) by weight,, with 1 part of Powdered natural graphite, be cooled to 0 ℃ in 0.3 part of adding of SODIUMNITRATE reactor; Again 45 parts of vitriol oils are slowly added in the reactor and fully to stir 0.7h, and keep 0～5 ℃ of the temperature of reaction system; Then, add in the reactor 0.5 part of potassium permanganate and the abundant 0.3h of stirring, keep 5～10 ℃ of temperature of reaction system simultaneously; In 1h, again 4 parts of potassium permanganate are slowly added in the reactor, keep 15～20 ℃ of temperature of reaction system, withdraw cryostat, with water-bath reaction system is heated to 40 ℃, and fully stirs 2h, obtain brown suspension.50 parts of pure water slowly are added dropwise in the brown suspension, and in react 10min under 95 ℃ of temperature, having reacted the back, to add 2 parts massfraction in the suspension be 30% H
2O
2Obtain glassy yellow graphite oxide dispersion liquid with 30 parts pure water.Dispersion liquid filters the back centrifugation, removes supernatant liquor, and solid is used 100 parts of water successively, and 100 parts of massfractions are that 30% HCl solution cleans, after 100 parts of ethanol clean twice, with 100 parts of petroleum ether precipitations filter oxide yellow Graphene solid.
(2) by weight, the graphene oxide that step (1) is made is added in 99 parts of pure water for 1 part, and ultrasonic 1h removes insolubles after by 2500rpm centrifugation 5min, and to get massfraction be 1% graphite oxide aqueous solution.
(3) by weight, add 0.012 part of oxalic acid after being dissolved in 6 parts Resorcinols in 90 parts of pure water, mix the back and add 24 parts of 1% made graphite oxide aqueous solutions of step (2), adding massfraction at last is to be sealed in 3 days postlyophilizations of 50 ℃ of following gels after 9 parts of 37% formaldehyde solutions mix to obtain xerogel GOR-2.
(4) xerogel that step (3) is obtained is in 500 ℃, and argon gas protection carbonization 5h down can obtain graphene oxide enhancing carbon aerogels material GCA-2.Its density is 0.035/cm
-2, specific surface area is 755m
2/ g.
Embodiment 3
(1) by weight, with 1 part of Powdered natural graphite, be cooled to 0 ℃ in 0.7 part of adding of SODIUMNITRATE reactor; Again 35 parts of vitriol oils are slowly added in the reactor and fully to stir 0.3h, and keep 0～5 ℃ of the temperature of reaction system; Then, add in the reactor 0.2 part of potassium permanganate and the abundant 0.7h of stirring, keep 5～10 ℃ of temperature of reaction system simultaneously; In 1h, again 3 parts of potassium permanganate are slowly added in the reactor, keep 15～20 ℃ of temperature of reaction system, withdraw cryostat, with water-bath reaction system is heated to 30 ℃, and fully stirs 3h, obtain brown suspension.40 parts of pure water slowly are added dropwise in the brown suspension, and under 85 ℃ of temperature, reacting 20min, have reacted the back and added 4 parts 30%H in the suspension
2O
2Obtain glassy yellow graphite oxide dispersion liquid with 20 parts pure water.Dispersion liquid filters the back centrifugation, removes supernatant liquor, and solid is with 100 parts of water successively, and 100 parts of massfractions are after 30% HCl solution cleans, to clean twice with 100 parts of ethanol, after with 100 parts of petroleum ether precipitations filter oxide yellow Graphene solid.
(2) by weight, graphene oxide 1 weight part that step (1) is made is added in 99 parts of pure water, and ultrasonic 3h removes insolubles after by 3000rpm centrifugation 4min, and to get massfraction be 1% graphite oxide aqueous solution.
(3) by weight, add 0.07 part in yellow soda ash after being dissolved in 20 parts Resorcinols in 80 parts of pure water, mix the back and add 40 parts of 1% made graphite oxide aqueous solutions of step (2), adding massfraction at last is to be sealed in 1 day postlyophilization of 85 ℃ of following gels after 29 parts of 37% formaldehyde solutions mix to obtain xerogel GOR-3.
(4) xerogel that step (3) is obtained is in 1000 ℃, and nitrogen gas protection carbonization 2h down can obtain graphene oxide enhancing carbon aerogels material GCA-3.Its density is 0.07g/cm
-2, specific surface area is 700m
2/ g.
Embodiment 4
(1) by weight, with 1 part of Powdered natural graphite, be cooled to 0 ℃ in 0.6 part of adding of SODIUMNITRATE reactor; Again 37 parts of vitriol oils are slowly added in the reactor and fully to stir 0.5h, and keep 0～5 ℃ of the temperature of reaction system; Then, add in the reactor 0.5 part of potassium permanganate and the abundant 0.5h of stirring, keep 5～10 ℃ of temperature of reaction system simultaneously; In 1h, again 3.2 parts of potassium permanganate are slowly added in the reactor, keep 15～20 ℃ of temperature of reaction system, withdraw cryostat, with water-bath reaction system is heated to 35 ℃, and fully stirs 2h, obtain brown suspension.46 parts of pure water slowly are added dropwise in the brown suspension, and in react 12min under 90 ℃ of temperature, having reacted the back, to add 3.2 parts massfraction in the suspension be 30%H
2O
2Obtain glassy yellow graphite oxide dispersion liquid with 25 parts pure water.Dispersion liquid filters the back centrifugation, removes supernatant liquor, and solid is used 100 parts of pure water successively, and 100 parts of massfractions are that 100 parts of ethanol cleaned twice after 30% HCl solution cleaned, with 100 parts of petroleum ether precipitations filter oxide yellow Graphene solid.
(2) by weight, the graphene oxide that step (1) is made is added in 99 parts of pure water for 1 part, and ultrasonic 3h removes insolubles after by 2500rpm centrifugation 6min, and to get massfraction be 1% graphite oxide aqueous solution.
(3) by weight, add 0.02 part in salt of wormwood after being dissolved in 10 parts Resorcinols in 90 parts of pure water, mix the back and add 20 parts of 1% made graphite oxide aqueous solutions of step (2), adding massfraction at last is to be sealed in 1 day postlyophilization of 85 ℃ of following gels after 15 parts of 37% formaldehyde solutions mix to obtain xerogel GOR-4.Prepare xerogel GOR-5 as stated above, the difference of itself and GOR-4 is: 1% made graphite oxide aqueous solution add-on of step (2) is 10 parts, the same GOR-4 of other materials and step.
(4) xerogel that step (3) is obtained is in 750 ℃, and nitrogen gas protection carbonization 5h down can obtain graphene oxide enhancing 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 used natural graphite of embodiment 1-4 is bought the permanent sharp graphite company limited that gets in Qingdao.
Effect embodiment
(1) the resulting graphene oxide of step (1) among the embodiment 1 is carried out examination of infrared spectrum, obtain the infrared signature absorption peak of typical graphene oxide, its result as shown in Figure 1.
Wherein: 3650cm wherein
-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
-1Be 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, occur 3650,3100,1732 after the Graphene oxidation, 1216cm
-1The absorption peak that several places are new, this several places absorption peak is the typical absorption peak of graphene oxide, all is to introduce Sauerstoffatom at the Graphene skeleton to cause.
(2) resulting carbon gelatinous material among the embodiment 1-4 is carried out scanning electron microscope test, its result as shown in Figure 2.Graphene oxide has tangible enhancement to the carbon gel as can be seen from Figure 2.The carbon gel such as the GCA-1～GCA-5 duct pattern that strengthen through Graphene are good, and duct degree of subsiding is low, and its vesicular structure is maintained, and shrinks little; And the carbon gel of not oxidised Graphene enhancing such as CA are low owing to the structural strength of gel, and gel shrinks phenomenon big, that appearance is lumpd in dry and carbonization process.
(3) will implement that resulting carbon aerogels GCA-1 carries out transmission electron microscope observation in 1, its result as shown in Figure 3.Can clearly find out the vesicular structure of Graphene lamella structure and carbon aerogels from Fig. 3.
(4) the resulting carbon gelatinous material of 1-4 among the embodiment is carried 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 chloroform, perhydronaphthalene, toluene, Virahol oils organism respectively, the quality of adsorbing record absorption front and back, saturated back carbon gel, the quality before its absorption multiple=(quality before the quality-absorption after the absorption)/absorption.It the results are shown in Table 1.
The Graphene of table 1 embodiment 1～4 strengthens the density of talking gelatinous material and adsorbs organic performance
Graphene strengthens the adsorbed oil type organic performance that the 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 preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a graphene oxide strengthens the carbon aerogels preparation methods, it is characterized in that: may further comprise the steps:
By weight, 4～20 parts Resorcinols are dissolved in 80～95 parts of pure water, after adding 0.008～0.07 part catalyst mix, add 10～40 parts of massfractions and be 1% graphite oxide aqueous solution, add 6～29 parts of formaldehyde solutions at last, the sealing gel, drying obtains xerogel, strengthens carbon aerogels with obtaining graphene oxide after the xerogel carbonization.
2. preparation method according to claim 1, it is characterized in that: described catalyzer is basic catalyst or an acidic catalyst.
3. preparation method according to claim 2, it 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, yellow soda ash, potassium hydroxide or sodium hydroxide.
4. preparation method according to claim 3, it is characterized in that: described an acidic catalyst is hydrochloric acid; Described basic catalyst is yellow soda ash or salt of wormwood.
5. preparation method according to claim 1, it is characterized in that: the massfraction of described formaldehyde solution is 37%; The temperature of described sealing gel is 50 ℃～85 ℃, and the time is 1～3 day; Described drying is lyophilize.
6. preparation method according to claim 1, it is characterized in that: described carbonization is at 500～1000 ℃, carbonization 2～5h under the protection of inert gas.
7. preparation method according to claim 6, it is characterized in that: described rare gas element is nitrogen or argon gas.
8. preparation method according to claim 1, it is characterized in that: the preparation process of described graphene oxide is: by weight, with 1 part of Powdered natural graphite, 0.3～0.7 part of mixing of SODIUMNITRATE is cooled to 0 ℃, stir 0.3～0.7h behind part vitriol oil of Dropwise 35～45 again, and keep 0～5 ℃ of the temperature of reaction system; Then, add 0.2～0.5 part of potassium permanganate and fully stir 0.3～0.7h, keep 5～10 ℃ of temperature of reaction system simultaneously; In 1h, add 3～4 parts of potassium permanganate again, keep 15～20 ℃ of temperature of reaction system, Heating temperature to 30～40 ℃, and fully stir 2h～3h, obtain brown suspension, drip 40～50 parts of water in react 10～20min under 85～95 ℃ of temperature, having reacted the back, to add 2～4 parts massfraction in the suspension be 30% H
2O
2, obtain glassy yellow graphite oxide dispersion liquid behind 20～30 parts the pure water, dispersion liquid filtration, centrifugal, remove supernatant liquor, solid is used 100 parts water successively, 100 parts of massfractions clean for 30%HCl solution, after 100 parts of ethanol clean twice, get oxide yellow Graphene solid after drying with 100 parts of petroleum ether precipitations filtrations behind the centrifuge washing.
9. a graphene oxide that is prepared by each described preparation method of claim 1～8 strengthens the carbon aerogels material, and it is characterized in that: 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.
10. graphene oxide according to claim 9 strengthens the application of carbon aerogels material in absorption and catalysis technical field.
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