CN104310490A - Schwertmannite-graphene oxide composite material and preparation method thereof - Google Patents
Schwertmannite-graphene oxide composite material and preparation method thereof Download PDFInfo
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- CN104310490A CN104310490A CN201410514284.6A CN201410514284A CN104310490A CN 104310490 A CN104310490 A CN 104310490A CN 201410514284 A CN201410514284 A CN 201410514284A CN 104310490 A CN104310490 A CN 104310490A
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Abstract
The invention discloses a Schwertmannite-graphene oxide composite material and a preparation method thereof, belonging to the technical field of novel functional composite materials. The preparation method comprises the following steps: firstly, oxidizing expandable graphite by using concentrated sulfuric acid and potassium permanganate to obtain graphene oxide; then, mixing the graphene oxide with FeCl3.6H2O and Na2SO4 in sequence, and synthesizing the Schwertmannite-graphene oxide composite material by virtue of a chemical synthetic method. The preparation method disclosed by the invention is simple, easy to operate, mild in experiment condition, small in space usage, cheap and easily available in raw material and free of secondary pollution; the prepared composite material is relatively great in specific surface area and capable of blocking the graphene oxide from agglomeration to keep the reaction activity of each component in the composite material, easy to separate and recycle, and has a wide application prospect.
Description
Technical field
The invention belongs to new function technical field of composite materials, be specifically related to a kind of Schwertmannite-graphene oxide composite material and preparation method thereof.
Background technology
Schwertmannite is also known as special graceful stone (Schwertmannite) of showing severity, and its chemical formula is Fe
8o
8(OH)
8-2x(SO
4)
xnH
2o (wherein 1≤x≤1.75) is a kind of low crystalloid sulfovinic acid height iron mineral, is prevalent in the abundant sour environment of sulfate radical content, as acidic mine waste water and Acidic sulphate soils.Owing to having nano level granularity and irregular pore passage structure, large (the 100 – 200m of its specific surface area
2/ g), reactive behavior is strong, and containing the group such as great amount of hydroxy group, sulfate radical, therefore can it can be used as catalyzer or sorbent material, thus reach the object turned waste into wealth.
Graphene is a kind of New Two Dimensional carbon nanomaterial be made up of the two dimensional structure of carbon atom six-ring, the very large (2630m of its theoretical specific surface area
2/ g); There is the oxy radicals such as a large amount of epoxide groups, hydroxyl, carboxyl in its surface, has unique nanostructure and excellent absorption reaction performance.But because the surface energy of graphene oxide is higher, easily reunite, and be scattered in after in water and be difficult to separate from the aqueous solution, be therefore necessary to carry out surface modification to it.Graphene has excellent physical and chemical performance, receives extensive concern in recent years using the matrix material that it obtains as matrix load oxide compound.If can a kind of matrix material be prepared, in conjunction with the advantage of graphene oxide and Schwertmannite, both Separation and Recovery was easy to, the reunion of graphene oxide can be avoided again, and technique is simple, can scale operation, this matrix material will have great application prospect (as fields such as catalyzer, sewage disposal, battery materials).
Summary of the invention
The object of the present invention is to provide a kind of Schwertmannite-graphene oxide composite material and preparation method thereof.
A preparation method for Schwertmannite-graphene oxide composite material, concrete steps are as follows:
Graphene oxide is disperseed in deionized water for ultrasonic; Add FeCl
36H
2o stirs; Then Na is added
2sO
4, be incubated under 60-85 DEG C of water bath condition; Centrifugal after naturally cooling to room temperature, abandoning supernatant; Adopt the dilute hydrochloric acid solution of pH 2.5 as scavenging solution, pelleting centrifugation is washed; Last vacuum-drying i.e. obtained Schwertmannite-graphene oxide composite material.
Wherein, FeCl
36H
2the mass ratio of O and graphene oxide is 5:1-10:1, FeCl
36H
2o and Na
2sO
4mass ratio be 3:1-4:1.
The time of described stirring is 1-3h.
The time of described insulation is 12-60min.
Described centrifugal condition is centrifugal 3-10min under 10000-12000r/min.
Described graphene oxide can be prepared with the following method: first add in reaction vessel by expansible black lead 1 – 2g, add the vitriol oil, and the mass ratio of the vitriol oil and graphite is 70:1 – 200:1, stirs 10 – 30min in ice-water bath; Slowly add potassium permanganate, the mass ratio of potassium permanganate and graphite is 1.5:1 – 6:1, keeps system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 34-36 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, stirs 30 – 60min at 59-61 DEG C, and second time adds 40mL, keeps 30 – 60min at 89-91 DEG C, and third time directly adds 40mL deionized water; Finally add H
2o
2, H used
2o
2for 30wt%, H
2o
2be 4.5:1 – 13.5:1 with the mass ratio of graphite.Centrifugal 30min under 10000 – 12000r/min while hot, abandoning supernatant is hydrochloric acid and the distilled water centrifuge washing of 1:10 by volume ratio, and obtained graphene oxide, lyophilize is for subsequent use.
Schwertmannite-graphene oxide composite material surface prepared by method of the present invention has needle-like burr, is about 50nm, and width is at about 10nm; Its specific surface area is 196.26m
2/ g, aperture is 3.87nm, and pore volume is 0.37cm
3/ g.
Beneficial effect of the present invention is mainly reflected in: the preparation method of Schwertmannite-graphene oxide composite material is simple, and experiment condition is gentle, and envrionment conditions is without particular requirement to external world, takes up room little, raw materials used cheap and easy to get, and there is not secondary pollution; Obtained matrix material specific surface area is comparatively large, can stop the reunion of graphene oxide, keeps the reactive behavior of each component in matrix material, and is easy to Separation and Recovery, have broad application prospects.
Accompanying drawing explanation
The XRD of Fig. 1 Schwertmannite-graphene oxide mixture characterizes spectrogram.
The HRTEM spectrogram of Fig. 2 Schwertmannite-graphene oxide mixture: (a) scale 200nm; (b) scale 50nm; (c) scale 10nm; (d) selected area electron diffraction (SAED) figure.
The EDX spectrogram of Fig. 3 Schwertmannite-graphene oxide mixture and elementary composition table.
The adsorption-desorption isothermal (a) of Fig. 4 Schwertmannite-graphene oxide mixture and graph of pore diameter distribution (b).
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
First prepare graphene oxide (GO), step is as follows: add in reaction vessel by the 106mL vitriol oil and 1.0g expansible black lead, in ice-water bath, stir 30min; Slowly add 5g potassium permanganate, keep system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 35 ± 1 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, at 60 ± 1 DEG C, stir 60min, and second time adds 40mL, at 90 ± 1 DEG C, keep 30min, and third time directly adds 40mL deionized water; Finally add the H of 10mL30wt%
2o
2, centrifugal 30min under 12000r/min while hot, abandoning supernatant, with hydrochloric acid (massfraction 36 – 38%) and the distilled water centrifuge washing several of volume ratio 1:10, lyophilize is for subsequent use.
Then prepare Schwertmannite-graphene oxide composite material, step is as follows: 0.108g graphene oxide is placed in 100mL deionized water, and ultrasonic disperse 3h adds 0.54g FeCl
36H
2o, stirs 1h; Then 0.15g Na is added
2sO
4, under 60 DEG C of water bath condition, be incubated 12min; After naturally cooling to room temperature, centrifugal 3min under 10000 – 12000r/min, abandoning supernatant; Pelleting centrifugation being washed, for controlling dissolving and the conversion of Schwertmannite, adopting the dilute hydrochloric acid solution of pH 2.5 as scavenging solution; Last vacuum-drying i.e. obtained Schwertmannite-graphene oxide composite material.
Carry out X-ray diffraction (XRD) analysis to obtained Schwertmannite-graphene oxide composite material, result as shown in Figure 1a.As can be seen from the figure, based on the characteristic diffraction peak of graphite oxide; Be occur very strong diffraction peak near 12 ° at 2 θ, corresponding to the diffraction peak in graphite oxide (001) face.The degree of crystallinity of Schwertmannite is often very low, does not occur the diffraction peak of good Schwertmannite in the XRD spectra of therefore mixture.
Embodiment 2
First prepare graphene oxide (GO), step is as follows: add in reaction vessel by the 106mL vitriol oil and 1.0g expansible black lead, in ice-water bath, stir 30min; Slowly add 5g potassium permanganate, keep system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 35 ± 1 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, at 60 ± 1 DEG C, stir 60min, and second time adds 40mL, at 90 ± 1 DEG C, keep 30min, and third time directly adds 40mL deionized water; Finally add the H of 10mL30wt%
2o
2, centrifugal 30min under 12000r/min while hot, abandoning supernatant, with hydrochloric acid (massfraction 36 – 38%) and the distilled water centrifuge washing several of volume ratio 1:10, lyophilize is for subsequent use.
Then prepare Schwertmannite-graphene oxide composite material, step is as follows: 0.054g graphene oxide is placed in 100mL deionized water, and ultrasonic disperse 2h adds 0.54g FeCl
36H
2o, stirs 3h; Then 0.15g Na is added
2sO
4, under 85 DEG C of water bath condition, be incubated 30min; After naturally cooling to room temperature, centrifugal 10min under 10000 – 12000r/min, abandoning supernatant; Pelleting centrifugation being washed, for controlling dissolving and the conversion of Schwertmannite, adopting the dilute hydrochloric acid solution of pH 2.5 as scavenging solution; Last vacuum-drying i.e. obtained Schwertmannite-graphene oxide composite material.
Carry out X-ray diffraction (XRD) analysis to obtained Schwertmannite-graphene oxide composite material, result as shown in Figure 1 b.As can be seen from the figure, FeCl
36H
2after the mass ratio of O and graphene oxide is increased to 10:1 from 5:1, the characteristic diffraction peak of graphene oxide is not obvious; Be occur diffraction peak near 35 °, corresponding to the diffraction peak of Schwertmannite at 2 θ.The crystalline form of Schwertmannite is poor, close to metamict.Contrasted from Fig. 1 a and 1b, Schwertmannite-graphene oxide composite material that different reaction conditionss obtains is had any different.
Embodiment 3
First prepare graphene oxide (GO), step is as follows: add in reaction vessel by the 106mL vitriol oil and 1.0g expansible black lead, in ice-water bath, stir 20min; Slowly add 5g potassium permanganate, keep system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 35 ± 1 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, at 60 ± 1 DEG C, stir 60min, and second time adds 40mL, at 90 ± 1 DEG C, keep 30min, and third time directly adds 40mL deionized water; Finally add the H of 10mL30wt%
2o
2, centrifugal 30min under 12000r/min while hot, abandoning supernatant, with hydrochloric acid (massfraction 36 – 38%) and the distilled water centrifuge washing several of volume ratio 1:10, lyophilize is for subsequent use.
Then prepare Schwertmannite-graphene oxide composite material, step is as follows: 0.054g graphene oxide is placed in 100mL deionized water, and ultrasonic disperse 3h adds 0.54g FeCl
36H
2o, stirs 3h; Then 0.15g Na is added
2sO
4, under 60 DEG C of water bath condition, be incubated 12min; After naturally cooling to room temperature, centrifugal 3min under 10000 – 12000r/min, abandoning supernatant; Pelleting centrifugation being washed, for controlling dissolving and the conversion of Schwertmannite, adopting the dilute hydrochloric acid solution of pH 2.5 as scavenging solution; Last vacuum-drying i.e. obtained Schwertmannite-graphene oxide composite material.
Carry out high resolution TEM (HRTEM) scanning analysis to it, result as shown in Figure 2.As seen from the figure, the Schwertmannite-graphene oxide composite surface of synthesis has needle-like burr (Fig. 2 a), is about 50nm (Fig. 2 b), and width is at about 10nm (Fig. 2 c).Selected area electron diffraction (SAED) figure (Fig. 2 d) of Schwertmannite-graphene oxide mixture is in annulus, and what wherein annulus has six specks is graphene oxide, and what two other annulus was corresponding is Schwertmannite.
Carry out high resolution TEM scanning analysis to it and obtain EDX spectrogram and elementary composition table, result as shown in Figure 3.The EDX spectrogram of Schwertmannite-graphene oxide mixture confirms the component of mixture, and wherein the weight percentage of C, O, S and Fe is respectively 29.77%, 15.40%, 4.28% and 49.93%.
Embodiment 4
First prepare graphene oxide (GO), step is as follows: add in reaction vessel by the 106mL vitriol oil and 1.0g expansible black lead, in ice-water bath, stir 30min; Slowly add 5g potassium permanganate, keep system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 35 ± 1 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, at 60 ± 1 DEG C, stir 60min, and second time adds 40mL, at 90 ± 1 DEG C, keep 30min, and third time directly adds 40mL deionized water; Finally add the H of 10mL30wt%
2o
2, centrifugal 30min under 12000r/min while hot, abandoning supernatant, with hydrochloric acid (massfraction 36 – 38%) and the distilled water centrifuge washing several of volume ratio 1:10, lyophilize is for subsequent use.
Then prepare Schwertmannite-graphene oxide composite material, step is as follows: 0.054g graphene oxide is placed in 100mL deionized water, and ultrasonic disperse 3h adds 0.54g FeCl
36H
2o, stirs 3h; Then 0.18g Na is added
2sO
4, under 60 DEG C of water bath condition, be incubated 12min; After naturally cooling to room temperature, centrifugal 5min under 10000 – 12000r/min, abandoning supernatant; Pelleting centrifugation being washed, for controlling dissolving and the conversion of Schwertmannite, adopting the dilute hydrochloric acid solution of pH 2.5 as scavenging solution; Last vacuum-drying i.e. obtained Schwertmannite-graphene oxide composite material.
From Schwertmannite-graphene oxide mixture adsorption-desorption isothermal figure (Fig. 4 a), according to BDDT classification (the Brunauer – Deming – Deming – Teller classification), Schwertmannite-graphene oxide mixture presents V-type H2 type hysteresis loop adsorption desorption isothermal curve, illustrates that this mixture has typical meso pore characteristics.The graph of pore diameter distribution (Fig. 4 b) adopting BJH desorption technology to obtain shows that Schwertmannite-graphene oxide mixture pore size distribution mainly concentrates on about 3.87nm, also illustrate that this mixture is meso-hole structure.The specific surface area of Schwertmannite-graphene oxide mixture, aperture and pore volume are respectively 196.26m
2/ g, 3.87nm and 0.37cm
3/ g.
Claims (7)
1. a preparation method for Schwertmannite-graphene oxide composite material, is characterized in that, concrete steps are as follows:
Graphene oxide is disperseed in deionized water for ultrasonic; Add FeCl
36H
2o stirs; Then Na is added
2sO
4, be incubated under 60-85 DEG C of water bath condition; Centrifugal after naturally cooling to room temperature, abandoning supernatant; Adopt the dilute hydrochloric acid solution of pH2.5 as scavenging solution, pelleting centrifugation is washed; Last vacuum-drying i.e. obtained Schwertmannite-graphene oxide composite material.
2. preparation method according to claim 1, is characterized in that, FeCl
36H
2the mass ratio of O and graphene oxide is 5:1-10:1.
3. preparation method according to claim 1, is characterized in that, FeCl
36H
2o and Na
2sO
4mass ratio be 3:1-4:1.
4. preparation method according to claim 1, is characterized in that, the time of described stirring is 1-3h.
5. preparation method according to claim 1, is characterized in that, the time of described insulation is 12-60min.
6. preparation method according to claim 1, is characterized in that, described centrifugal condition is centrifugal 3-10min under 10000-12000r/min.
7. Schwertmannite-graphene oxide composite material of preparing of preparation method described in any one of claim 1-6.
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| CN111725003A (en) * | 2020-07-10 | 2020-09-29 | 大连理工大学 | Cubic iron-based oxyhydroxide/graphene composite material for supercapacitor and preparation method thereof |
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| CN111725003B (en) * | 2020-07-10 | 2021-07-06 | 大连理工大学 | Cubic iron-based oxyhydroxide/graphene composite material for supercapacitor and preparation method thereof |
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