CN104310490B - A kind of Schwertmannite-graphene oxide composite material and preparation method thereof - Google Patents
A kind of Schwertmannite-graphene oxide composite material and preparation method thereof Download PDFInfo
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- CN104310490B CN104310490B CN201410514284.6A CN201410514284A CN104310490B CN 104310490 B CN104310490 B CN 104310490B CN 201410514284 A CN201410514284 A CN 201410514284A CN 104310490 B CN104310490 B CN 104310490B
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000002000 scavenging effect Effects 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 8
- 239000012286 potassium permanganate Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001311 chemical methods and process Methods 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 15
- 239000005457 ice water Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 4
- 238000004098 selected area electron diffraction Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- KIWBPDUYBMNFTB-UHFFFAOYSA-N Ethyl hydrogen sulfate Chemical compound CCOS(O)(=O)=O KIWBPDUYBMNFTB-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001608 iron mineral Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a kind of Schwertmannite-graphene oxide composite material belonging to new function technical field of composite materials and preparation method thereof.First the method obtains graphene oxide with the vitriol oil and potassium permanganate oxidation expansible black lead, then by graphene oxide priority and FeCl
36H
2o and Na
2sO
4mixing, synthesizes Schwertmannite-graphene oxide composite material by chemical process.This preparation method is simple, easy handling, and experiment condition is gentle, 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.
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 pH2.5 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 naturally cool to room temperature after centrifugal, 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 0.54gFeCl
36H
2o, stirs 1h; Then 0.15gNa 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 pH2.5 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 0.54gFeCl
36H
2o, stirs 3h; Then 0.15gNa 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 pH2.5 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 0.54gFeCl
36H
2o, stirs 3h; Then 0.15gNa 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 pH2.5 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 0.54gFeCl
36H
2o, stirs 3h; Then 0.18gNa 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 pH2.5 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 (theBrunauer – Deming – Deming – Tellerclassification), 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. Schwertmannite-graphene oxide composite material, is characterized in that, its chemical formula is GOFe
8o
8(OH)
8-2x(SO
4)
xnH
2o, wherein 1≤x≤1.75; This composite material surface has needle-like burr.
2. 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.
3. preparation method according to claim 2, is characterized in that, FeCl
36H
2the mass ratio of O and graphene oxide is 5:1-10:1.
4. preparation method according to claim 2, is characterized in that, FeCl
36H
2o and Na
2sO
4mass ratio be 3:1-4:1.
5. preparation method according to claim 2, is characterized in that, the time of described stirring is 1-3h.
6. preparation method according to claim 2, is characterized in that, the time of described insulation is 12-60min.
7. preparation method according to claim 2, is characterized in that, described in naturally cool to room temperature after centrifugal, centrifugal condition is centrifugal 3-10min under 10000-12000r/min.
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| CN109999844B (en) * | 2019-05-07 | 2020-06-12 | 南京农业大学 | MoS2Composite Fenton catalyst of/Schweitermann stone, preparation method and application |
| CN111186933A (en) * | 2020-01-08 | 2020-05-22 | 南京农业大学 | Chemical method for quickly forming sea urchin-shaped schneiderian minerals from acid mine wastewater |
| 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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