CN104671234A - Method for preparing graphene by lamellar template carbonization - Google Patents
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- CN104671234A CN104671234A CN201310619894.8A CN201310619894A CN104671234A CN 104671234 A CN104671234 A CN 104671234A CN 201310619894 A CN201310619894 A CN 201310619894A CN 104671234 A CN104671234 A CN 104671234A
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Abstract
The invention discloses a method for preparing graphene by carbonizing carbohydrate with a lamellar phosphate template, which comprises the following steps: synthesizing a lamellar compound phosphate as a lamellar template, adsorbing to interlayers under the static action by using natural molecular carbohydrate as a carbon source, carrying out primary carbonization at low temperature, carbonizing at high temperature to obtain a composite with uniform graphene among the phosphate interlayers, dissolving, carrying out centrifugal separation, and drying to obtain the high-quality graphene. By using the lamellar phosphate as the template, the crystal lattice catalytic element in the lamellar phosphate is used as the active group spot in the high-temperature calcination process to carbonize the carbon source into the high-quality graphene. The method has the advantages of abundant carbon sources, simple and mild preparation technique and lower cost, and can implement large-scale industrial production.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to a kind of method utilizing the carbonization of stratiform template to prepare Graphene.
Background technology
Graphene adopts SP by monolayer carbon atom
2the carbonaceous material of the two-dimentional honeycomb crystal lattice that hydridization is piled up, its special construction makes Graphene show excellent mechanical property, peculiar electrical properties and good thermal property, such as Graphene Young's modulus can reach 11000GPa, breaking tenacity reaches 125GPa, thermal conductivity reaches 5000W/mK, and theoretical specific surface area is up to 2630m
2/ g, and the character such as the specific conductivity with perfect quantum tunneling effect, half integral quantum hall effect and superelevation, have a good application prospect in fields such as aerospace, novel material, electric power, electronics.
The preparation method of Graphene comprises two large classes, i.e. " top-dwon " and " bottom-up " method.The former is interacted by the strong π-π overcoming graphite layers and obtains Graphene (comprise hummer oxidation-reduction method, machinery or electrochemical stripping, ball milling, overcritically to strut) from top to bottom, and this method is not only time-consuming but also require great effort, and output is very low.Atom is generally assembled into two-dimensional sheet Graphene (comprising chemical Vapor deposition process, arc discharge method, polymer cracking method etc.) from bottom to top by High Temperature High Pressure by the latter.Wherein the most frequently used is chemical Vapor deposition process, can prepare high quality, large-area Graphene, but its preparation process preparing substrate material desirable needed for Graphene is complicated, and required equipment is expensive.
The stratiform template grown up recent years is that Graphene preparation provides new approach.After utilizing lamellar compound to adsorb carbon source, at high temperature carbonization can obtain high-quality Graphene, and overcomes the difficulty controlling graphene layer thickness in above-mentioned graphene preparation method.Lamellar compound refer to there is laminate structure, a compounds that interlayer ion has interchangeability, some functional guest species are introduced bedding void and laminate distance are strutted thus form layer-pillared compound by the intercalation utilizing lamellar compound main body to have under strong polar molecule effect and the interchangeability of interlayer ion.
The preparation method of a kind of two-dimensional nano-graphene that Chinese Patent Application No. 201080043559.2 and 201210410900.4 is reported, all utilize hydrotalcite as stratiform template, respectively warm and fine for propylene vinylformic acid is added to interlayer, then be polymerized under initiator effect, after the calcining of the polymeric carbon source of generation, carbonization, obtain Graphene.Aforesaid method carbon source used all needs to obtain after initiated polymerization, preparation process more complicated.Chinese Patent Application No. 201210472499.7 reports a kind of Graphene with high specific capacitance and preparation method thereof, employing MCM-22 has divided the katalysis of sieving as template and nickel, be immersed in the mixed solution of carbon source, nickel salt and the vitriol oil, then by the pre-carbonization of low temperature and high-temperature calcination, high-quality Graphene is obtained.Adopt the vitriol oil as dewatering agent in the preparation process of the method, there is certain danger, and addn of nickel is as catalyzer, need strict control catalyzer amount and temperature of reaction (otherwise formed be carbon granule but not Graphene), whole preparation process cost is higher.Up to now, there is not yet the report adopting phosphoric acid salt as stratiform Template preparation Graphene.
Summary of the invention
Higher for overcoming the complicated process of preparation, the cost that exist in existing Graphene production technique, and the unmanageable difficult problem of Graphene thickness, the object of the invention is to provide a kind of method utilizing the carbonization of stratiform template to prepare Graphene, its preparation technology is simple, cost is lower, favorable reproducibility, can be used for large-scale industrial production.
A kind of method utilizing the carbonization of stratiform template to prepare Graphene of the present invention's report, specifically comprises the steps:
(1) after soluble metallic salt and soluble phosphate being dissolved respectively, mix and blend forms coagulant liquid, is transferred in reactor by this gel, at 60-200 DEG C of reaction 4-150h, is washed with distilled water to neutrality, obtains layered phosphates after separation, drying;
(2) by the aqueous solution of carbohydrate, join the layered phosphates suspension obtained through ultrasonication or mechanical stirring, at 50-100 DEG C, stir 6-48h, make carbohydrate fully enter the interlayer of layered phosphates, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 100-200 DEG C pre-carbonizing treatment 0.5-2h and obtain pressed powder; Then under protection of inert gas, by pressed powder in by pressed powder in vacuum tube furnace, high-temperature calcination, obtains phosphoric acid salt/graphene complex;
(4) phosphoric acid salt/graphene complex obtained is joined in hydrochloric acid soln, stirring at normal temperature 0.5-8h, centrifugation, drying graphene powder.
Described step (1) laminate phosphoric acid salt comprises the one in stratiform titanium phosphate, bedded zirconium phosphate, stratiform phosphoric acid tin, stratiform phosphoric acid hafnium, stratiform niobium phosphate, stratiform phosphoric acid germanium and stratiform lead phosphate.
In described step (1), soluble metallic salt is selected from metal nitrate or oxychlorination thing.
Described metal comprises the one in titanium, zirconium, tin, hafnium, niobium, germanium and lead; Described soluble phosphate is one or both of SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, potassium primary phosphate, dipotassium hydrogen phosphate, phosphoric acid dihydro amine and diammonium hydrogen phosphate; Wherein, the mol ratio 1:2-5 of metal and phosphorus.
In described step (1), the concentration of soluble metallic salt is 0.5-1mol/L, and the concentration of soluble phosphate is 1-2mol/L.
In described step (2), carbohydrate is one or both of glucose, fructose, sucrose, maltose, lactose, Zulkovsky starch, dextrin, glycogen, Walocel MT 20.000PV and Natvosol.
The mass ratio of described step (2) laminate phosphoric acid salt, carbohydrate, water is 1:(0.5-3): (25-50).
During ultrasonication in described step (2), hyperacoustic power is 200-500W, and ultrasonication and churned mechanically time are 1-3h.
In described step (3), the condition of high-temperature calcination is the roasting temperature 1-5 hour of 500-1200 DEG C.
The mass concentration of the hydrochloric acid soln described in described step (4) is 20-37%.The mass volume ratio of described phosphoric acid salt/graphene complex and hydrochloric acid soln is 1g:(5-10) mL.
The present invention utilizes layered phosphates as template, and carbohydrate is carbon source, obtains high-quality Graphene by the pre-carbonization of low temperature, high temperature cabonization.Compared with prior art, the beneficial effect that has of the present invention is as follows:
(1) in high-temperature burning process, the layered phosphates as stratiform template can promote that carbon source is converted into Graphene, and the catalytic elements zirconium, titanium, hafnium etc. in layered phosphates lattice is as active basic point, can improve the quality of gained Graphene.Verified, utilize other lamellar compound (see comparative example) as stratiform template, Graphene product can not be obtained.
(2) shown in, layered phosphates preparation method is simple, and productive rate is high, and does not need surface treatment; Carbohydrate source as carbon source is abundant, cheap, meets requirement that is green, environmental protection.Owing to containing a large amount of hydroxyls in carbohydrate, with the Na of layered phosphates interlayer
+, H
+etc. there is strong electrostatic force, the effective filling between therefore can realizing phosphate layer, gained Graphene productive rate is high, can reach more than 28wt% (relative to carbohydrate).
(3) due to phosphatic special laminate structure, Graphene grows in its interlayer finite space, therefore controlled, the size uniform of the Graphene thickness prepared of the present invention.
(4) whole preparation technology is simple, gentle, cost is lower, can large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the Graphene of preparation in embodiment 1.
Fig. 2 is the high-resolution-ration transmission electric-lens figure of the Graphene of preparation in embodiment 1.
Fig. 3 is the Raman spectrogram of preparation in embodiment 2.
Fig. 4 is the x-ray photoelectron energy spectrogram of the Graphene of preparation in embodiment 6.
Fig. 5 is the scanning electron microscope (SEM) photograph of the Graphene of preparation in comparative example 1.
Fig. 6 is the transmission electron microscope picture of the Graphene of preparation in comparative example 2.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be appreciated that, these embodiments only for illustration of the present invention, and are not intended to limit the scope of the invention.The improvement made according to the present invention of technician and adjustment, still belong to protection scope of the present invention in actual applications.
Embodiment 1
(1) 0.5mol titanium tetrachloride is dissolved in wiring solution-forming in the distilled water of 1000mL, again 1mol potassium primary phosphate is dissolved in 500mL distilled water and is added to above-mentioned solution, stir and form gel, this gel is transferred in reactor, at 150 DEG C of reaction 75h, be washed with distilled water to solution for neutral, dry, obtain stratiform titanium phosphate;
(2) getting stratiform titanium phosphate prepared by 1g above-mentioned steps (1) is added in 15mL distilled water, and ultrasonic (power 300W) also stirs 2h and prepare stable suspension; After the glucose sugar of 1.5g is dissolved in 30mL distilled water, joins in suspension, at 80 DEG C, stir 24h, finally by centrifuge washing, dry, grinding, obtains precursor powder;
(3) presoma is carried out at 150 DEG C pre-carbonizing treatment 1.5h and obtain pressed powder; Then, under protection of inert gas, by pressed powder in vacuum tube furnace, the roasting temperature of 900 DEG C 3 hours, obtains titanium phosphate/graphene complex;
(4) titanium phosphate/graphene complex obtained being joined concentration is in the hydrochloric acid soln of 30%, the hydrochloric acid soln of the corresponding 7.5mL of every gram of powder, stirring at normal temperature 4h, centrifuge washing, drying graphene powder, productive rate can reach 32wt%.
Fig. 1 and Fig. 2 shows transmission electron microscope and the high-resolution-ration transmission electric-lens figure of Graphene obtained in the present embodiment respectively.As can be seen from transmission electron microscope picture, material is mutually piled up by a large amount of transparent sheet to form, and the sidewall at edge is high-visible, is the even size distribution of the characteristic feature of Graphene, Graphene, and thickness is homogeneous, be mainly positioned at 0.4-4nm.The thickness of the Graphene shown in high-resolution electron microscopy figure is only 4 atomic shells, and the crystallization degree of Graphene is high.
Embodiment 2
(1) 0.5mol zirconium oxychloride is dissolved in the distilled water wiring solution-forming of 1000mL, again 1mol SODIUM PHOSPHATE, MONOBASIC is dissolved in 500mL distilled water and is added to above-mentioned solution, stir and form gel, this gel is transferred in reactor, at 150 DEG C of reaction 75h, be washed with distilled water to solution for neutral, dry, obtain bedded zirconium phosphate;
(2) getting stratiform titanium phosphate prepared by 1g above-mentioned steps (1) is added in 15mL distilled water, and ultrasonic (power 300W) also stirs 2h and prepare stable suspension; After the fructose of 1.5g is dissolved in 30mL distilled water, join in suspension, at 80 DEG C, stir 24h, finally by centrifugal, washing, grinding, obtain precursor powder;
(3) presoma is carried out at 150 DEG C pre-carbonizing treatment 1.5h and obtain pressed powder; Then, under protection of inert gas, by pressed powder in vacuum tube furnace, the roasting temperature of 900 DEG C 3 hours, obtains zirconium phosphate/graphene complex;
(4) zirconium phosphate/graphene complex obtained being joined concentration is in the hydrochloric acid soln of 30%, the hydrochloric acid soln of the corresponding 7.5mL of every gram of powder, stirring at normal temperature 4h, centrifuge washing, drying graphene powder, productive rate reaches 30wt%.
Fig. 3 gives the Raman spectrogram of the Graphene obtained in the present embodiment.At 1350cm in figure
-1and 1586cm
-1present two strong Raman peaks, be respectively D band and be with G.The former with the latter ratio (I
d/ I
g) being about 1.2, this shows that obtained Graphene degree of graphitization is relatively high, defect is less.In addition, at 2698cm
-1place is obvious visible 2D band also, testimonial material aligning on C axle, the successful preparation of sufficient proof Graphene.
Embodiment 3
(1) 0.5mol oxychlorination tin is dissolved in wiring solution-forming in the distilled water of 1000mL, again 1mol Sodium phosphate dibasic is dissolved in 500mL distilled water and is added to above-mentioned solution, stir and form gel, this gel is transferred in reactor, at 180 DEG C of reaction 60h, be washed with distilled water to solution for neutral, dry, obtain bedded zirconium phosphate;
(2) getting stratiform titanium phosphate prepared by 1g above-mentioned steps (1) is added in 15mL distilled water, and ultrasonic (power 300W) also stirs 2h and prepare stable suspension; After the lactose of 1g fructose, 0.5g is dissolved in 30mL distilled water, join in suspension, at 80 DEG C, stir 24h, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 150 DEG C pre-carbonizing treatment 1.5h and obtain pressed powder; Then, under protection of inert gas, by pressed powder in by vacuum tube furnace, the roasting temperature of 900 DEG C 3 hours, obtains phosphoric acid tin/graphene complex;
(4) phosphoric acid obtained tin/graphene complex being joined concentration is in the hydrochloric acid soln of 30%, the hydrochloric acid soln of the corresponding 7.5mL of every gram of powder, stirring at normal temperature 4h, centrifuge washing, drying graphene powder, productive rate can reach 28wt%.
Embodiment 4
(1) 0.5mol nitric acid niobium is dissolved in wiring solution-forming in the distilled water of 1000mL, again 1.5mol phosphoric acid dihydro amine is dissolved in 1000mL distilled water and is added to above-mentioned solution, stir and form gel, this gel is transferred in reactor, at 120 DEG C of reaction 100h, be washed with distilled water to solution for neutral, dry, obtain stratiform niobium phosphate;
(2) getting stratiform niobium phosphate prepared by 1g above-mentioned steps (1) is added in 15mL distilled water, and ultrasonic (power 300W) also stirs 2h and prepare stable suspension; After the Zulkovsky starch of 2g is dissolved in 35mL distilled water, join in suspension, at 70 DEG C, stir 36h, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 150 DEG C pre-carbonizing treatment 1.5h and obtain pressed powder; Then under protection of inert gas, by pressed powder in by pressed powder in vacuum tube furnace, the roasting temperature of 800 DEG C 4 hours, obtains niobium phosphate/graphene complex;
(4) niobium phosphate/graphene complex obtained being joined concentration is in the hydrochloric acid soln of 20%, the hydrochloric acid soln of the corresponding 5mL of every gram of powder, stirring at normal temperature 0.5h, centrifuge washing, drying graphene powder, productive rate can reach 32%.
Embodiment 5
(1) 0.5mol lead nitrate is dissolved in wiring solution-forming in the distilled water of 500mL, again 1mol phosphoric acid dihydro amine, 1mol potassium primary phosphate are dissolved in 2000mL distilled water and are added to above-mentioned solution, stir and form gel, this gel is transferred in reactor, at 60 DEG C of reaction 150h, be washed with distilled water to solution for neutral, dry, obtain stratiform lead phosphate;
(2) getting stratiform lead phosphate prepared by 1g above-mentioned steps (1) is added in 15mL distilled water, and ultrasonic (power 200W) also stirs 1h and prepare stable suspension; After the cyclodextrin of 0.5g is dissolved in 10mL distilled water, join in suspension, at 50 DEG C, stir 48h, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 100 DEG C pre-carbonizing treatment 2h and obtain pressed powder; Then, under protection of inert gas, by pressed powder in vacuum tube furnace, the roasting temperature of 500 DEG C 5 hours, obtains phosphoric acid tin/graphene complex;
(4) lead phosphate/graphene complex that step (3) obtains being joined concentration is in the hydrochloric acid soln of 37%, the hydrochloric acid soln of the corresponding 5mL of every gram of powder, stirring at normal temperature 8h, centrifuge washing, drying graphene powder, productive rate can reach 34wt%.
Embodiment 6
(1) 0.5mol oxychlorination germanium is dissolved in wiring solution-forming in the distilled water of 500mL, again 2.5mol potassium primary phosphate is dissolved in 2000mL distilled water and is added to above-mentioned solution, at 200 DEG C of reaction 4h, be washed with distilled water to solution for neutral, drying, obtains stratiform phosphoric acid germanium;
(2) getting stratiform phosphoric acid germanium prepared by 1g above-mentioned steps (1) is added in 15mL distilled water, and ultrasonic (power 500W) also stirs 3h and prepare stable suspension; After the Walocel MT 20.000PV of 3g is dissolved in 35ml distilled water, join in suspension, at 100 DEG C, stir 6h, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 200 DEG C pre-carbonizing treatment 0.5h and obtain pressed powder; Then under protection of inert gas, by pressed powder in by pressed powder in vacuum tube furnace, the roasting temperature of 1200 DEG C 1 hour, obtains phosphoric acid germanium/graphene complex;
(4) phosphoric acid obtained germanium/graphene complex being joined concentration is in the hydrochloric acid soln of 20%, the hydrochloric acid soln of the corresponding 10mL of every gram of powder, stirring at normal temperature 8h, centrifuge washing, drying graphene powder, productive rate can reach 36%.
Fig. 4 shows the x-ray photoelectron energy spectrogram of Graphene obtained in the present embodiment.Carbon content about 85% in gained Graphene, and the content of Sauerstoffatom is about 10%, illustrates that employing carbohydrate is less as heteroatoms defect in carbon source gained Graphene, proves to adopt this patent method to prepare the feasibility of high-quality graphene.
Comparative example 1
(1) 0.5mol aluminum chloride is dissolved in wiring solution-forming in the distilled water of 500mL, then 2.5mol potassium primary phosphate is dissolved in 2000mL distilled water is added to above-mentioned solution, at 250 DEG C of reaction 8h, be washed with distilled water to solution for neutral, dry, obtain Layered aluminophosphate;
(2) getting the above-mentioned Layered aluminophosphate of 1g is added in 15mL distilled water, and ultrasonic (power 300W) also stirs 2h and prepare stable suspension; After the glucose sugar of 1.5g is dissolved in 30mL distilled water, joins in suspension, at 80 DEG C, stir 24h, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 150 DEG C pre-carbonizing treatment 1.5h and obtain pressed powder; Then, under protection of inert gas, by pressed powder in vacuum tube furnace, the roasting temperature of 900 DEG C 3 hours, obtains aluminum phosphate/carbon complex;
(4) aluminum phosphate/carbon complex obtained being joined concentration is in the hydrochloric acid soln of 30%, and the hydrochloric acid soln of every gram of corresponding 7.5mL of powder, stirring at normal temperature 4h, centrifuge washing, drying can obtain target product.
Scanning electron microscope Fig. 5 shows that products therefrom is sheet carbon material, and product thickness, at more than 50nm, presents strong D band and weak G band, I in Raman spectrogram
d/ I
gbe about 2.5, show that this carbon material defect is more, crystallization degree is low.Show that several layered phosphates defined in the application prepare the necessary stratiform template of Graphene.
Comparative example 2
(1) by magnesium nitrate and aluminum nitrate in molar ratio for 3:1 is mixed with the aqueous solution that metal ion total concn is 2mol/l; Under room temperature, stirring, dropwise add the alkaline solution that volumetric molar concentration is 1mol/L, regulate pH to 12, be then warmed up to 70 DEG C, after reaction 6h, throw out is centrifugal, distilled water is washed till solution to neutral, and drying, obtains stratiform magnesium aluminum double hydroxide.
(2) getting the above-mentioned stratiform magnesium aluminum double hydroxide of 1g is added in 15mL distilled water, and ultrasonic (power 300W) also stirs 2h and prepare stable suspension; After the glucose sugar of 1.5g is dissolved in 30mL distilled water, joins in suspension, at 80 DEG C, stir 24h, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 150 DEG C pre-carbonizing treatment 1.5h and obtain pressed powder; Then, under protection of inert gas, by pressed powder in vacuum tube furnace, the roasting temperature of 900 DEG C 3 hours, obtains magnesium aluminum oxide/carbon complex;
(4) magnesium aluminum oxide/carbon complex obtained being joined concentration is in the hydrochloric acid soln of 30%, the hydrochloric acid soln of the corresponding 7.5mL of every gram of powder, stirring at normal temperature 4h, centrifuge washing, drying product.
Transmission electron microscope Fig. 6 shows that products therefrom is decolorizing carbon (in figure, lower left corner ratio scale is 170nm), presents strong D band and weak G band, I in Raman spectrogram
d/ I
gbe about 2.8, show that this product defect is more, crystallization degree is low.Explanation utilizes other lamellar compound can not obtain Graphene product as template, and several lamellar compounds limited in the application are the prerequisite of synthesizing graphite alkene.
Claims (10)
1. utilize the carbonization of stratiform template to prepare a method for Graphene, it is characterized in that concrete steps are as follows:
(1) after soluble metallic salt and soluble phosphate being dissolved respectively, mix and blend forms coagulant liquid, is transferred in reactor by this gel, at 60-200 DEG C of reaction 4-150h, is washed with distilled water to neutrality, obtains layered phosphates after separation, drying;
(2) by the aqueous solution of carbohydrate, join the layered phosphates suspension obtained through ultrasonication or mechanical stirring, at 50-100 DEG C, stir 6-48h, make carbohydrate fully enter the interlayer of layered phosphates, finally by centrifuge washing, drying, grinding, obtain precursor powder;
(3) presoma is carried out at 100-200 DEG C pre-carbonizing treatment 0.5-2h and obtain pressed powder; Then under protection of inert gas, by pressed powder in by pressed powder in vacuum tube furnace, high-temperature calcination, obtains phosphoric acid salt/graphene complex;
(4) phosphoric acid salt/graphene complex obtained is joined in hydrochloric acid soln, stirring at normal temperature 0.5-8h, centrifugation, drying graphene powder.
2. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, it is characterized in that, described step (1) laminate phosphoric acid salt comprises the one in stratiform titanium phosphate, bedded zirconium phosphate, stratiform phosphoric acid tin, stratiform phosphoric acid hafnium, stratiform niobium phosphate, stratiform phosphoric acid germanium and stratiform lead phosphate.
3. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, is characterized in that, in described step (1), soluble metallic salt is selected from metal nitrate or oxychlorination thing.
4. a kind of method utilizing the carbonization of stratiform template to prepare Graphene according to claim 3, it is characterized in that, described metal comprises the one in titanium, zirconium, tin, hafnium, niobium, germanium and lead; Described soluble phosphate is one or both of SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, potassium primary phosphate, dipotassium hydrogen phosphate, phosphoric acid dihydro amine and diammonium hydrogen phosphate; Wherein, the mol ratio 1:2-5 of metal and phosphorus.
5. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, is characterized in that, in described step (1), the concentration of soluble metallic salt is 0.5-1mol/L, and the concentration of soluble phosphate is 1-2mol/L.
6. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, it is characterized in that, in described step (2), carbohydrate is one or both of glucose, fructose, sucrose, maltose, lactose, Zulkovsky starch, dextrin, glycogen, Walocel MT 20.000PV and Natvosol.
7. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, it is characterized in that, the mass ratio of described step (2) laminate phosphoric acid salt, carbohydrate, water is 1:(0.5-3): (25-50).
8. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, is characterized in that, during ultrasonication in described step (2), hyperacoustic power is 200-500W, and ultrasonication and churned mechanically time are 1-3h.
9. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, is characterized in that, in described step (3), the condition of high-temperature calcination is the roasting temperature 1-5 hour of 500-1200 DEG C.
10. a kind of method utilizing the carbonization of stratiform template to prepare Graphene as claimed in claim 1, it is characterized in that, the mass concentration of the hydrochloric acid soln described in described step (4) is 20-37%; The mass volume ratio of described phosphoric acid salt/graphene complex and hydrochloric acid soln is 1g:(5-10) mL.
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| CN105694107B (en) * | 2016-01-26 | 2018-12-18 | 同济大学 | A kind of preparation method of nanometer of alpha zirconium phosphate load graphene oxide fire retardant |
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| CN108428894A (en) * | 2018-02-09 | 2018-08-21 | 武汉科技大学 | A kind of sulfur doping two dimension carbon material, preparation method and application |
| CN108428894B (en) * | 2018-02-09 | 2020-08-11 | 武汉科技大学 | Sulfur-doped two-dimensional carbon material, and preparation method and application thereof |
| CN109054015A (en) * | 2018-08-01 | 2018-12-21 | 安徽省绩溪县华宇防火滤料有限公司 | A kind of light heat-resisting fire proofing material and preparation method thereof |
| CN113314695A (en) * | 2021-04-30 | 2021-08-27 | 天津大学 | Method for improving performance of carbon fluoride battery material by salt template method |
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