CN106744830A - A kind of method that three-dimensional porous/two-dimensional slice Graphene is prepared for carbon source with biology - Google Patents
A kind of method that three-dimensional porous/two-dimensional slice Graphene is prepared for carbon source with biology Download PDFInfo
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Abstract
The invention discloses a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass.The method step is as follows：（1）Biomass carbon source material is immersed in Fe (NO3)3·9H2In O solution；（2）Biomass carbon source material after immersion is calcined into carbonization, Fe is obtained2O3/ C compound precursors；（3）By Fe2O3After/C compound precursor pickling, mixed under aqueous conditions with activator, dried；（4）Desciccate is heat-treated；（5）Heat-treated products are cleaned, is dried, obtain three-dimensional porous/two-dimensional slice Graphene.The inventive method has experimentation simple, with low cost, the advantage of environmental protection and energy saving.The three-dimensional porous Graphene aperture for preparing of the invention is small, specific surface area is high；The two-dimensional slice graphene layer spacing of preparation is big, fault of construction is few, can be widely applied to include energy storage material, sorbing material and Heat Conduction Material field.
Description
Technical field
The invention belongs to the preparing technical field of Graphene, be related to it is a kind of with biomass as carbon source prepare it is three-dimensional porous/bis-
The method for tieing up Sheet Graphite alkene.
Background technology
Graphene is a kind of nano material of the excellent performance with two-dimensional structure, and high with specific surface area, intensity is high, leads
Electrically strong the advantages of.At present, the primary synthetic methods of Graphene have three kinds：Hydro-thermal method, chemical vapour deposition technique and stripping method.Its
Although Graphene pore structure prepared by middle hydro-thermal method, than more uniform, electric conductivity is not high, and preparation time is more long, limits it
Commercial Application.Chemical vapour deposition technique it is relatively costly, and control condition is strict, it is difficult to which large-scale promotion is produced.Peel off legal system
The yield of standby Graphene is not high, and the graphene sheet layer agglomeration for preparing is serious.
The content of the invention
It is an object of the invention to solve the production cost that existing three-dimensional porous/two-dimensional slice Graphene preparation process is present
High, expensive, complex technical process problem, and one kind is provided and prepares three-dimensional porous/two-dimensional slice by carbon source of biomass
The method of Graphene.
A kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass, specifically includes following steps：
（1）Biomass carbon source material is immersed in Fe (NO3)3·9H2In O solution；
（2）Biomass carbon source material after immersion is calcined into carbonization under inert gas atmosphere, Fe is obtained2O3Body before/C compounds
Body, cleans in hydrochloric acid；
（3）Fe after cleaning2O3Activator is added in/C compound precursors, and mixing is dissolved with pure water, dried, in obtaining
Between product；
（4）The intermediate product that will be obtained is heat-treated in inert gas atmosphere；
（5）Product after heat treatment is cleaned with hydrochloric acid, washes away metal and its oxide, then is washed with deionized water and is in cleaning solution
Property, dry, obtain three-dimensional porous/two-dimensional slice Graphene.
Preferably, step（1）In, the biomass carbon source material includes agaric, and dry biomass carbon source material needs
Fe (NO are soaked in again after soaking expansion in deionized water3)3·9H2In O solution.
Preferably, step（1）In, the time of the immersion is 18 ~ 20h.
Preferably, step（1）In, the Fe (NO3)3·9H2The concentration of O solution is 0.5 ~ 3M.
Preferably, step（2）In, the temperature of the calcining is 300 ~ 450 DEG C, and the time is 2 ~ 4h.
Preferably, step（2）In, the biomass carbon source material after immersion is carried out into calcining carbonization again after drying.
Preferably, step（2）In, the concentration of the hydrochloric acid is 0 ~ 6M.
Preferably, step（2）In, the time of the cleaning is 20min ~ 6h, preferably 30 ~ 40min.
Preferably, step（2）In, according to the difference of concentration of hydrochloric acid, obtain three-dimensional porous or two-dimensional slice Graphene；Work as step
Suddenly（2）When middle concentration of hydrochloric acid is 0M, three-dimensional porous Graphene is obtained, work as step（2）When middle concentration of hydrochloric acid is between 0 ~ 6M, obtain
To two-dimensional slice Graphene.
Preferably, step（3）In, the activator is potassium hydroxide, NaOH, calcium hydroxide, phosphoric acid, sulfuric acid and chlorine
Change one or more of zinc.
Preferably, step（3）In, the addition of the activator is：The mass ratio of biomass carbon source material and activator
It is 1:1~5.
Preferably, step（3）In, the drying is that 1 ~ 5h is dried under the conditions of 80 ~ 130 DEG C.
Preferably, step（4）In, the heat treatment is first to be warming up to 300 ~ 400 DEG C with 5 ~ 10 DEG C/min of heating rate, is protected
0 ~ 1h of temperature；600 ~ 800 DEG C are warming up to 10 DEG C/min of heating rate again, 2 ~ 5h is heat-treated.
Preferably, step（5）In, the drying is that 0.5 ~ 5h is dried under conditions of 40 ~ 100 DEG C.
Preferably, step（2）、（4）In, the inert gas is one or more of nitrogen, argon gas and helium.
Compared with prior art, the present invention has advantages below and beneficial effect：
（1）The present invention synthesizes three-dimensional porous/two-dimensional slice Graphene by simple heat treatment method, and preparation process is simple is forged
Burning temperature is low, and energy consumption is low, meets environmental requirement.
（2）The present invention with the biomass class carbon material including agaric be carbon source, compared with the carbon source of other synthesizing graphite alkenes,
There is low toxicity, of low pollution, material is cheap and easy to get, raw material sources are extensive, low-carbon environment-friendly；Using the method and principle, will
Realize the more cheap three-dimensional porous and dilute large-scale production of two-dimensional slice graphite.
Brief description of the drawings
Fig. 1 is the XRD of three-dimensional porous Graphene prepared by embodiment 1；
Fig. 2 is the Raman spectrogram of three-dimensional porous Graphene prepared by embodiment 1；
Fig. 3 is the SEM figures of three-dimensional porous Graphene prepared by embodiment 1；
Fig. 4 is the SEM figures of three-dimensional porous Graphene prepared by embodiment 1；
Fig. 5 is the nitrogen adsorption-desorption figure of three-dimensional porous Graphene prepared by embodiment 1；
Fig. 6 is the graph of pore diameter distribution of three-dimensional porous Graphene prepared by embodiment 1；
Fig. 7 is the Raman spectrogram of two-dimensional slice Graphene prepared by embodiment 3；
Fig. 8 is the SEM figures of two-dimensional slice Graphene prepared by embodiment 3；
Fig. 9 is the SEM figures of two-dimensional slice Graphene prepared by embodiment 3.
Specific embodiment
With reference to instantiation, the present invention will be further described, but the invention is not restricted to following instance.
Embodiment 1
The preparation of three-dimensional porous Graphene：
（1）The dried fungus of 10g are weighed, is soaked in deionized water, agaric water swelling after 20min, removal is soaked behind root
Steep in 3M Fe (NO3)3·9H2In O solution, agaric is placed in graphite crucible after 18h, added a cover, be placed in tube furnace, in nitrogen
300 DEG C of calcining 2h, obtain Fe in atmosphere2O3/ C compound precursors；
（2）By Fe2O3/ C compound precursors stirring and washing 1h in 6M concentrated hydrochloric acids, adds 5 times of KOH solids of quality after cleaning
With the mixing of 3mL deionized water dissolvings, 2h is dried under the conditions of 120 DEG C；Desciccate is placed in tube furnace, in nitrogen atmosphere
Under, 300 DEG C first are risen to the speed of 5 DEG C/min, 0h is incubated, then 700 DEG C are risen to the speed of 10 DEG C/min, it is heat-treated 3h；
To sample cleaned with 2M hydrochloric acid, and be washed with deionized water to cleaning solution in neutrality, finally dry 2h in 60 DEG C of baking ovens,
Obtain three-dimensional porous Graphene.
The X ray diffracting spectrum of the three-dimensional porous Graphene that the present embodiment is obtained is as shown in figure 1, as shown in Figure 1, prepare
Three-dimensional porous Graphene have diffraction maximum respectively at 21.5 °, 26.3 ° and 44.6 °, wherein 21.5 ° and 44.6 ° of diffraction maximum explanation
Material is graphene-structured, and according to 21.5 ° of diffraction maximum, the stacking interlayer of Graphene is can be calculated with reference to Bragg equation
Away from being 0.41nm；And still with the presence of the micro graphite not being fully exfoliated in the weak peak explanation material at 26.3 °.
The Raman spectrogram of the three-dimensional porous Graphene that the present embodiment is obtained is as shown in Figure 2, it can be seen that Raman spectrogram
It is middle to there is obvious characteristic peak at three：D peaks（1350cm-1）, G peaks（1593cm-1）With 2D peaks（2823cm-1）.It is fitted by swarming
And it is 1.36 to calculate Id/Ig, illustrates that the degree of graphitization of resulting materials is higher.
Such as Fig. 3 of the scanning electron microscope analysis under different multiples for the three-dimensional porous Graphene that the present embodiment is obtained and
Shown in Fig. 4, as seen from the figure, the three-dimensional grapheme of preparation is perforated grill structure.
The nitrogen adsorption of the three-dimensional porous Graphene that the present embodiment is obtained-desorption figure is as shown in figure 5, as can be seen from the figure
Prepared three-dimensional porous Graphene has specific surface area higher, about 507cm3/g。
The graph of pore diameter distribution of the three-dimensional porous Graphene that the present embodiment is obtained is as shown in fig. 6, three-dimensional more as can be seen from Figure
It is microcellular structure that hole Graphene is most of, and pore size is in below 3nm.
Embodiment 2
The preparation of three-dimensional porous Graphene：
（1）The dried fungus of 10g are weighed, is soaked in deionized water, agaric water swelling after 20min, removal is soaked behind root
Steep in 0.5M Fe (NO3)3·9H2In O solution, agaric is placed in culture dish after 20h, is placed in and 12h is freezed in refrigerator, be put into true
Freeze-drying 24h in vacuum freecing-dry machine；Agaric after freeze-drying is put into graphite crucible, is added a cover, be placed in tube furnace,
450 DEG C of calcining 4h, obtain Fe in nitrogen atmosphere2O3/ C compound precursors；
（2）By Fe2O3/ C compound precursors stirring and washing 6h in 0.001M watery hydrochloric acid, adds 1 times of KOH of quality after cleaning
Solid and 3mL deionized water dissolvings mix, and 5h is dried under the conditions of 80 DEG C；Drying is placed in tube furnace, under an argon atmosphere,
400 DEG C first are risen to the speed of 10 DEG C/min, 1h is incubated, then 800 DEG C are risen to the speed of 10 DEG C/min, be heat-treated 2h；Obtain
Sample cleaned with 2M hydrochloric acid, and be washed with deionized water to cleaning solution in neutrality, finally dry 5h in 40 DEG C of baking ovens, obtain
To three-dimensional porous Graphene.
The three-dimensional porous graphite for obtaining is similar to three-dimensional porous Graphene prepared by embodiment 1, is perforated grill structure, tool
There is specific surface area high, pore size is in below 3nm.
Embodiment 3
The preparation of two-dimensional slice Graphene：
（1）The dried fungus of 10g are weighed, is soaked in deionized water, agaric water swelling after 20min, removal is soaked behind root
Steep in 2M Fe (NO3)3·9H2In O solution, agaric is placed in graphite crucible after 19h, added a cover, be placed in tube furnace, in nitrogen
425 DEG C of calcining 3h, obtain Fe in atmosphere2O3/ C compound precursors；
（2）By Fe2O3/ C compound precursors clean 20min in pure water, afterwards add 4 times of quality KOH solids and 3mL go from
Sub- water dissolves mixing, 1h is dried under the conditions of 130 DEG C；Desciccate is placed in tube furnace, in a nitrogen atmosphere, first with 7 DEG C/
The speed of min rises to 350 DEG C, is incubated 0.5h, then rises to 600 DEG C with the speed of 10 DEG C/min, is heat-treated 5h；The sample for obtaining is used
2M hydrochloric acid is cleaned, and is washed with deionized water to cleaning solution in neutrality, finally dries 0.5h in 100 DEG C of baking ovens, obtains two
Dimension Sheet Graphite alkene.
The Raman spectrogram of the two-dimensional slice Graphene that the present embodiment is obtained is as shown in Figure 7, it can be seen that Raman spectrogram
It is middle to there is obvious characteristic peak at three：D peaks（1344cm-1）, G peaks（1574cm-1）With 2D peaks（2718cm-1）.It is fitted by swarming
Understand that 2D peaks are single Lorentz fit peak, peak position of the peak position compared with single-layer graphene（2700cm-1）Blue shift, explanation is not individual layer
Graphene；And IG/I2D=0.88, illustrate that the number of plies of Graphene is less than 5.
Such as Fig. 8 of the scanning electron microscope analysis under different multiples for the two-dimensional slice Graphene that the present embodiment is obtained and
Shown in 9, as seen from the figure, the two-dimensional graphene of preparation is lamellar structure, and piece interlamellar spacing is larger, and lamella is very thin.
Claims (10)
1. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass, it is characterised in that including as follows
Step：
（1）Biomass carbon source material is immersed in Fe (NO3)3·9H2In O solution；
（2）Biomass carbon source material after immersion is calcined into carbonization under inert gas atmosphere, Fe is obtained2O3Body before/C compounds
Body, cleans in hydrochloric acid；
（3）Fe after cleaning2O3Activator is added in/C compound precursors, and mixing is dissolved with pure water, dried, in obtaining
Between product；
（4）The intermediate product that will be obtained is heat-treated in inert gas atmosphere；
（5）Product after heat treatment is cleaned with hydrochloric acid, washes away metal and its oxide, then is washed with deionized water and is in cleaning solution
Property, dry, obtain three-dimensional porous/two-dimensional slice Graphene.
2. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（1）In, the biomass carbon source material includes agaric, dry biomass carbon source material need go from
Fe (NO are soaked in again after soaking expansion in sub- water3)3·9H2In O solution；The soak time is 18 ~ 20h；The Fe
(NO3)3·9H2The concentration of O solution is 0.5 ~ 3M.
3. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（2）In, the temperature of the calcining is 300 ~ 450 DEG C, and the time is 2 ~ 4h；The time of the cleaning is
20min~6h。
4. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（2）In, the biomass carbon source material after immersion is carried out into calcining carbonization again after drying.
5. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（2）In, the concentration of the hydrochloric acid is 0 ~ 6M；The time of the cleaning is 30 ~ 40min.
6. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, according to step（2）The difference of middle concentration of hydrochloric acid, obtains three-dimensional porous or two-dimensional slice Graphene；Work as step（2）
When middle concentration of hydrochloric acid is 0M, three-dimensional porous Graphene is obtained, work as step（2）When middle concentration of hydrochloric acid is between 0 ~ 6M, two dimension is obtained
Sheet Graphite alkene.
7. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（3）In, the activator is potassium hydroxide, NaOH, calcium hydroxide, phosphoric acid, sulfuric acid and zinc chloride
One or more of, biomass carbon source material is 1 with the mass ratio of activator:1~5；The drying is under the conditions of 80 ~ 130 DEG C
Dry 1 ~ 5h.
8. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（4）In, the heat treatment is first to be warming up to 300 ~ 400 DEG C with 5 ~ 10 DEG C/min of heating rate, insulation 0 ~
1h；600 ~ 800 DEG C are warming up to 10 DEG C/min of heating rate again, 2 ~ 5h is heat-treated.
9. a kind of method for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1,
Characterized in that, step（5）In, the drying is that 0.5 ~ 5h is dried under conditions of 40 ~ 100 DEG C.
10. a kind of side for preparing three-dimensional porous/two-dimensional slice Graphene as carbon source with biomass according to claim 1
Method, it is characterised in that step（2）、（4）In, the inert gas is one or more of nitrogen, argon gas and helium.
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| CN109939643A (en) * | 2019-04-09 | 2019-06-28 | 西安工业大学 | α-Fe2O3Adulterate the preparation method and applications of charcoal |
| CN110395723A (en) * | 2019-08-26 | 2019-11-01 | 东莞理工学院 | A kind of method of fuse salt strategy preparation High-performance graphene |
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| CN114261955A (en) * | 2021-12-03 | 2022-04-01 | 海南师范大学 | Gelidium derived carbonitrident/porous graphitized carbon and preparation method and application thereof |
| CN115557490A (en) * | 2022-10-18 | 2023-01-03 | 武汉工程大学 | Method for preparing biomass-based vertical graphene in batches |
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| CN109399615A (en) * | 2018-11-27 | 2019-03-01 | 天津科技大学 | A kind of preparation method of the using biomass resource 3D- grapheme material as carbon source |
| CN109399615B (en) * | 2018-11-27 | 2022-06-07 | 天津科技大学 | Preparation method of 3D-graphene material with biomass resource as carbon source |
| CN109939643A (en) * | 2019-04-09 | 2019-06-28 | 西安工业大学 | α-Fe2O3Adulterate the preparation method and applications of charcoal |
| CN110395723A (en) * | 2019-08-26 | 2019-11-01 | 东莞理工学院 | A kind of method of fuse salt strategy preparation High-performance graphene |
| CN110395723B (en) * | 2019-08-26 | 2021-06-01 | 东莞理工学院 | Method for preparing high-performance graphene by molten salt strategy |
| CN113429933A (en) * | 2021-07-30 | 2021-09-24 | 陕西科技大学 | Ferroferric oxide/biomass porous carbon composite wave-absorbing material and preparation method thereof |
| CN114261955A (en) * | 2021-12-03 | 2022-04-01 | 海南师范大学 | Gelidium derived carbonitrident/porous graphitized carbon and preparation method and application thereof |
| CN114261955B (en) * | 2021-12-03 | 2024-01-30 | 海南师范大学 | Gelidium amansii derived tri-carbon tetranitride/porous graphitized carbon as well as preparation method and application thereof |
| CN115557490A (en) * | 2022-10-18 | 2023-01-03 | 武汉工程大学 | Method for preparing biomass-based vertical graphene in batches |
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