CN109368634A - A kind of preparation method and applications of graphene-based material precursor - Google Patents
A kind of preparation method and applications of graphene-based material precursor Download PDFInfo
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- CN109368634A CN109368634A CN201811351941.4A CN201811351941A CN109368634A CN 109368634 A CN109368634 A CN 109368634A CN 201811351941 A CN201811351941 A CN 201811351941A CN 109368634 A CN109368634 A CN 109368634A
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/23—Oxidation
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- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C01B2204/00—Structure or properties of graphene
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Abstract
The invention discloses a kind of preparation method and applications of graphene-based material precursor.Include following steps: (1) pre-oxidation being carried out to graphite by the concentrated sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide, obtains pre-oxidation product A product；(2) after carrying out oxidation processes to the pre-oxidation product A product concentrated sulfuric acid and potassium permanganate, deionized water is added dropwise into reaction system, obtain suspension B product: after hydrogen peroxide is added into suspension B product in (3), gained mixture is cleaned with dilute hydrochloric acid, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.Solid-state graphite containing acid oxidase obtained by the present invention may replace pure oxygen graphite as the presoma for preparing graphene-based material, eliminate the deacidification step in pure oxygen graphite preparation process, it can be applied to prepare graphene hydrogel/aeroge, graphene film, graphene fiber etc., so that the characteristics of graphene-based material preparation cost reduces, is high-efficient, pollution is lowered, easy extension.
Description
Technical field
The present invention relates to graphene presoma technical fields, more particularly to a kind of inexpensive, efficient graphene-based
The preparation method of material precursor, and its preparing graphene-based material, including graphene hydrogel/aeroge, graphene are thin
The application of film, graphene fiber etc..
Background technique
Graphene have high electron mobility, excellent heating conduction, huge specific surface area, superpower mechanical strength,
The excellent physical characteristic such as high transparency, therefore graphene-based material all has huge application prospect in many fields.But stone
Black alkene has strong hydrophobicity, its liquid phase operability is low, is difficult through graphene direct construction macroscopic material.It is so far
Only, the preparation majority of graphene-based material is using graphite oxide as presoma.Graphite oxide is peelable at two wieners through ultrasound
Rice sheet layer material, that is, graphene oxide.Graphene oxide contains graphene skeleton and oxygen-containing functional group abundant simultaneously, by also
It manages to obtain graphene-based material in original place.
The preparation of graphite oxide can be traced to 19th century mid-term, and graphite is added to potassium chloride in a heated condition by Brodie
Graphite oxide is prepared in the mixture of fuming nitric aicd.Later, many scientific research personnel constantly explore the preparation process of graphite oxide,
But it is not significantly modified compared with Brodie method.Finally, Hummers in 1985 et al. invented it is a kind of relatively safe and effective
Then there is a series of improved Hummers method in graphite oxide synthetic method.However, preparing pure oxygen using these methods
Graphite still needs several days time.All consumed in final step it is worth noting that preparing the graphite oxide most of the time ---
Deacidification.This step plus dilute hydrochloric acid washing rather than use pure water, be because graphite oxide and water will form gel.To obtain pure oxygen fossil
Ink need to be deacidified using suitable cleaning technique (such as: dialysis and centrifugal process), but these cleaning techniques consume a large amount of water and when
Between, production efficiency is low.In recent years, Huang seminar has found a kind of method for removing demineralizing acid.It is filtered and is deacidified with acetone, then
Pure oxygen graphite is obtained as acetone volatilizees naturally.Although this method significantly shortens graphite oxide preparation time, remove
Sour process needs a large amount of acetone, and acetone is inflammable and explosive chemicals, and not only increasing synthesis cost, there is also security risks.
In conclusion there are the deacidification difficulties in pure oxygen graphite preparation process for the prior art, so that graphene-based material
Preparation cost drop it is high, efficiency is lower, pollute greatly, be not easy the technical issues of magnifying.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and applications of graphene-based material precursor.The present invention
Obtained solid-state graphite containing acid oxidase may replace pure oxygen graphite as the presoma for preparing graphene-based material, eliminate pure
It is fine to can be applied to graphene hydrogel/aeroge, graphene film, graphene for deacidification step in graphite oxide preparation process
Dimension etc., so that the preparation cost of graphene-based material reduces, efficiency is got higher, pollution is lowered, is easier to the characteristics of extension.
Technical solution of the present invention: a kind of preparation method and applications of graphene-based material precursor, include following
Step:
(1) by weight, taking 250-340 parts of mass fractions respectively is the concentrated sulfuric acid, the 12-18 parts of persulfuric acid of 90-98%
Potassium, 10-20 part phosphorus pentoxide and 15-25 parts of graphite mixing carry out pre-oxidation, and natural cooling must mix after pre-oxidation
Object is closed, is cleaned mixture with deionized water after being 6.5-7 to pH value, mixture is dry at 20-30 DEG C, it is pre-oxidized
Product A product；
(2) by weight, 1100-1500 parts are added into 20-30 parts of pre-oxidation product A product in a low temperature of 0-5 DEG C
Mass fraction is the oxidation processes 3-6h at 30-50 DEG C, at oxidation after the concentrated sulfuric acid and 80-120 parts of potassium permanganate of 90-98%
Reaction system after reason carries out ice bath, while deionized water being added drop-wise in reaction system, makes the temperature 20-50 of reaction system
DEG C, obtain suspension B product；
(3) hydrogen peroxide that mass fraction is 30-40% is added into suspension B product and obtains mixture, then mixes gained
Object is cleaned with dilute hydrochloric acid, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
In the preparation method of graphene-based material precursor above-mentioned, in step (1), it is described by weight, take respectively
The concentrated sulfuric acid, 15 parts of potassium peroxydisulfates, 15 parts of phosphorus pentoxides and the 20 parts of graphite mixing that 280 parts of mass fractions are 90-98% carry out
Pre-oxidation.
In the preparation method of graphene-based material precursor above-mentioned, in step (1), the pre-oxidation temperature is
60-90 DEG C, the pre-oxidation time is 3-5h.
In the preparation method of graphene-based material precursor above-mentioned, in step (1), the pre-oxidation temperature is 80
DEG C, the pre-oxidation time is 4h.
In the preparation method of graphene-based material precursor above-mentioned, in step (2), it is described by weight, be in 0-5
The concentrated sulfuric acid and 100 parts for being added that 1400 parts of mass fractions are 90-98% in product A product are pre-oxidized in a low temperature of DEG C to 20-30 parts
Potassium permanganate.
In the preparation method of graphene-based material precursor above-mentioned, in step (3), described is to 1-2L suspension B product
The hydrogen peroxide that middle addition 30-60mL mass fraction is 30-40% obtains mixture, then by the dilute hydrochloric acid of gained mixture 2-5L
Cleaning, the concentration of the dilute hydrochloric acid are 2-5mol/L.
The application of graphene-based material precursor above-mentioned, the graphene-based material precursor are applied to prepare graphene
Hydrogel.
The application of graphene-based material precursor above-mentioned, the graphene-based material precursor are applied to prepare graphene
Aeroge.
The application of graphene-based material precursor above-mentioned, the graphene-based material precursor are applied to prepare graphene
Film.
The application of graphene-based material precursor above-mentioned, the graphene-based material precursor are applied to prepare graphene
Fiber.
Compared with prior art, the features of the present invention and the utility model has the advantages that
It (1) is as compared with preparing graphene-based material precursor with using pure oxygen graphite, the present invention prepares solid-state containing acid
Graphite oxide is presoma, eliminates the deacidification step in pure oxygen graphite preparation process, so that preparing graphene-based material
Process cost reduce, efficiency is got higher, pollution is lowered, is easier to magnify.
(2) solid-state graphite containing acid oxidase obtained by the present invention can be used as the presoma for preparing graphene-based material, can apply
In preparing graphene hydrogel/aeroge, graphene film, graphene fiber etc..
In conclusion there is the present invention solid-state graphite containing acid oxidase obtained by the present invention may replace pure oxygen graphite conduct
The presoma for preparing graphene-based material eliminates the deacidification step in pure oxygen graphite preparation process, can be applied to prepare stone
Black alkene hydrogel/aeroge, graphene film, graphene fiber etc. so that the preparation cost of graphene-based material reduce,
Efficiency is got higher, pollution is lowered, is easier to the beneficial effect of extension.
Experiments have shown that:
Fig. 1 is solid-state graphite containing acid oxidase prepared by the present invention and existing pure oxygen graphite (a) XRD and (b) FTIR
Comparison diagram is obtained: solid-state graphite containing acid oxidase prepared by the present invention and existing pure zirconia by (a) XRD and (b) FTIR comparison
The performance of graphite is similar.
Graphene hydrogel/aeroge, stone that applicant respectively prepares the graphene oxide prepared by the present invention containing acid
Black alkene film, graphene fiber and existing pure zirconia graphene are graphene hydrogel/aeroge, graphene of precursor preparation
Film, graphene fiber carry out performance comparison, and the results are shown in Table 1:
1 performance comparison table of table
Obtained by the electrochemical data in table 1: graphene hydrogel/aeroge prepared by the present invention, graphene film,
Graphene fiber and using pure oxygen graphite preparation graphene hydrogel/aeroge, graphene film, graphene fiber ratio
Capacitor is all close respectively, so graphene prepared by the present invention hydrogel/aeroge, graphene film, graphene fiber are distinguished
It is similar to using the graphene hydrogel/aeroge, graphene film, graphene fiber performance of pure oxygen graphite preparation.
Detailed description of the invention
Fig. 1 is solid-state graphite containing acid oxidase and pure oxygen graphite result characterization comparison diagram of the present invention.
Fig. 2 is the digital photograph for the graphene hydrogel that solid-state graphite containing acid oxidase of the present invention is precursor preparation；
Fig. 3 is the digital photograph for the graphene aerogel that solid-state graphite containing acid oxidase of the present invention is precursor preparation；
Fig. 4 is the digital photograph for the graphene film that solid-state graphite containing acid oxidase of the present invention is precursor preparation；
Fig. 5 is the digital photograph for the graphene film that solid-state graphite containing acid oxidase of the present invention is precursor preparation；
Fig. 6 is that digital in coagulating bath of graphene fiber that solid-state graphite containing acid oxidase of the present invention is precursor preparation is shone
Piece；
Fig. 7 is that solid-state graphite containing acid oxidase of the present invention is that the digital of graphene fiber after the drying of precursor preparation is shone
Piece；
Fig. 8 is the digital photograph for the graphene fiber braided fabric that solid-state graphite containing acid oxidase of the present invention is precursor preparation.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiment 1:
(1) take the concentrated sulfuric acid, 12g potassium peroxydisulfate, 10g phosphorus pentoxide and 15g graphite that 250g mass fraction is 90% mixed
It closes and carries out pre-oxidation, pre-oxidation temperature is 60 DEG C, and the pre-oxidation time is 5h, natural cooling after pre-oxidation
Mixture, with deionized water by mixture clean be 6.5 to pH value after, mixture is dry at 20 DEG C, pre-oxidized
Product A product；
(2) in a low temperature of 0 DEG C to 20g pre-oxidation product A product in be added 1100g mass fraction be 90% the concentrated sulfuric acid and
After 80g potassium permanganate, the oxidation processes 6h at 30 DEG C, the reaction system after oxidation processes carries out ice bath, while by deionized water
It is added drop-wise in reaction system, makes 20 DEG C of temperature of reaction system, obtain suspension B product；
(3) hydrogen peroxide that 30mL mass fraction is 30% is added into 1L suspension B product and obtains mixture, then mixes gained
It closes object to be cleaned with the 4mol/L dilute hydrochloric acid of 2L, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
Embodiment 2:
(1) take the concentrated sulfuric acid, 15g potassium peroxydisulfate, 13g phosphorus pentoxide and 18g graphite that 270g mass fraction is 94% mixed
It closes and carries out pre-oxidation, pre-oxidation temperature is 70 DEG C, and the pre-oxidation time is 4h, natural cooling after pre-oxidation
Mixture, with deionized water by mixture clean be 6.8 to pH value after, mixture is dry at 25 DEG C, pre-oxidized
Product A product；
(2) in a low temperature of 2 DEG C to 22g pre-oxidation product A product in be added 1200g mass fraction be 94% the concentrated sulfuric acid and
After 90g potassium permanganate, the oxidation processes 4h at 40 DEG C, the reaction system after oxidation processes carries out ice bath, while by deionized water
It is added drop-wise in reaction system, makes 30 DEG C of temperature of reaction system, obtain suspension B product；
(3) hydrogen peroxide that 40mL mass fraction is 40% is added into 1.2L suspension B product and obtains mixture, then by gained
Mixture is cleaned with the 4mol/L dilute hydrochloric acid of 3L, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
Embodiment 3:
(1) take the concentrated sulfuric acid, 16g potassium peroxydisulfate, 18g phosphorus pentoxide and 22g graphite that 300g mass fraction is 96% mixed
It closes and carries out pre-oxidation, pre-oxidation temperature is 80 DEG C, and the pre-oxidation time is 3h, natural cooling after pre-oxidation
Mixture, with deionized water by mixture clean be 6.8 to pH value after, mixture is dry at 28 DEG C, pre-oxidized
Product A product；
(2) in a low temperature of 3 DEG C to 24g pre-oxidation product A product in be added 1300g mass fraction be 96% the concentrated sulfuric acid and
After 110g potassium permanganate, the oxidation processes 4h at 50 DEG C, the reaction system after oxidation processes carries out ice bath, while by deionized water
It is added drop-wise in reaction system, makes 20-50 DEG C of temperature of reaction system, obtain suspension B product；
(3) hydrogen peroxide that 50mL mass fraction is 30% is added into 1.4L suspension B product and obtains mixture, then by gained
Mixture is cleaned with the 3mol/L dilute hydrochloric acid of 4L, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
Embodiment 4:
(1) take the concentrated sulfuric acid, 15g potassium peroxydisulfate, 20g phosphorus pentoxide and 23g graphite that 320g mass fraction is 98% mixed
It closes and carries out pre-oxidation, pre-oxidation temperature is 90 DEG C, and the pre-oxidation time is 4h, natural cooling after pre-oxidation
Mixture, with deionized water by mixture clean be 6.6 to pH value after, mixture is dry at 30 DEG C, pre-oxidized
Product A product；
(2) concentrated sulfuric acid that 1400g mass fraction is 98% is added into 26g pre-oxidation product A product in a low temperature of 0-5 DEG C
After 115g potassium permanganate, the oxidation processes 4h at 50 DEG C, the reaction system after oxidation processes carries out ice bath, while by deionization
Water droplet is added in reaction system, is made 40 DEG C of temperature of reaction system, is obtained suspension B product；
(3) hydrogen peroxide that 50mL mass fraction is 30% is added into 1.6L suspension B product and obtains mixture, then by gained
Mixture is cleaned with the 2mol/L dilute hydrochloric acid of 5L, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
Embodiment 5:
(1) take the concentrated sulfuric acid, 15g potassium peroxydisulfate, 15g phosphorus pentoxide and 20g graphite that 280g mass fraction is 94% mixed
It closes and carries out pre-oxidation, pre-oxidation temperature is 60 DEG C, and the pre-oxidation time is 5h, natural cooling after pre-oxidation
Mixture, with deionized water by mixture clean be 7 to pH value after, mixture is dry at 25 DEG C, obtain pre-oxidation and produce
Object A product；
(2) concentrated sulfuric acid that 1400g mass fraction is 94% is added into 28g pre-oxidation product A product in a low temperature of 0-5 DEG C
After 100g potassium permanganate, the oxidation processes 5h at 40 DEG C, the reaction system after oxidation processes carries out ice bath, while by deionization
Water droplet is added in reaction system, is made 40 DEG C of temperature of reaction system, is obtained suspension B product；
(3) hydrogen peroxide that 50mL mass fraction is 40% is added into 1.8L suspension B product and obtains mixture, then by gained
Mixture is cleaned with the 4mol/L dilute hydrochloric acid of 3L, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
Embodiment 6:
(1) take the concentrated sulfuric acid, 18g potassium peroxydisulfate, 20g phosphorus pentoxide and 25g graphite that 340g mass fraction is 98% mixed
It closes and carries out pre-oxidation, pre-oxidation temperature is 80 DEG C, and the pre-oxidation time is 4h, natural cooling after pre-oxidation
Mixture, with deionized water by mixture clean be 7 to pH value after, mixture is dry at 30 DEG C, obtain pre-oxidation and produce
Object A product；
(2) concentrated sulfuric acid that 1500g mass fraction is 98% is added into 30g pre-oxidation product A product in a low temperature of 0-5 DEG C
After 120g potassium permanganate, the oxidation processes 6h at 50 DEG C, the reaction system after oxidation processes carries out ice bath, while by deionization
Water droplet is added in reaction system, is made 50 DEG C of temperature of reaction system, is obtained suspension B product；
(3) hydrogen peroxide that 60mL mass fraction is 40% is added into 2L suspension B product and obtains mixture, then mixes gained
It closes object to be cleaned with the 5mol/L dilute hydrochloric acid of 5L, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
The graphene-based material precursor prepared in the embodiment 1-6 -- solid-state graphite containing acid oxidase is made into appropriate dense
The graphite oxide aqueous solution of degree not deacidified can be with synthesizing graphite alkene hydrogel by hydro-thermal or solvent heat treatment.
The graphene-based material precursor prepared in the embodiment 1-6 -- solid-state graphite containing acid oxidase is made into appropriate dense
The graphite oxide aqueous solution of degree not deacidified can be with synthesizing graphite alkene aeroge by hydro-thermal or solvent heat treatment.
The graphene-based material precursor prepared in the embodiment 1-6 -- solid-state graphite containing acid oxidase is made into appropriate dense
The graphite oxide aqueous solution of degree not deacidified passes through vacuum filtration, available graphene film.
The graphene-based material precursor prepared in the embodiment 1-6 -- solid-state graphite containing acid oxidase is made into appropriate dense
The graphite oxide hydrogel of degree not deacidified, by wet spinning, available graphene fiber.
Claims (10)
1. a kind of preparation method of graphene-based material precursor, it is characterised in that: include following steps:
(1) by weight, take respectively 250-340 parts of mass fractions be the concentrated sulfuric acid of 90-98%, 12-18 parts of potassium peroxydisulfates,
10-20 parts of phosphorus pentoxides and 15-25 parts of graphite mixing carry out pre-oxidation, and natural cooling must mix after pre-oxidation
Object is cleaned mixture with deionized water after being 6.5-7 to pH value, and mixture is dry at 20-30 DEG C, is obtained pre-oxidation and is produced
Object A product；
(2) by weight, 1100-1500 parts of quality are added into 20-30 parts of pre-oxidation product A product in a low temperature of 0-5 DEG C
Score is the oxidation processes 3-6h at 30-50 DEG C, after oxidation processes after the concentrated sulfuric acid and 80-120 parts of potassium permanganate of 90-98%
Reaction system carry out ice bath, while deionized water being added drop-wise in reaction system, makes 20-50 DEG C of temperature of reaction system,
Obtain suspension B product；
(3) hydrogen peroxide that mass fraction is 30-40% is added into suspension B product and obtains mixture, then uses gained mixture
Dilute hydrochloric acid cleaning, obtains graphene-based material precursor-solid-state graphite containing acid oxidase after dry.
2. the preparation method of graphene-based material precursor as described in claim 1, it is characterised in that: described in step (1)
By weight, take respectively 280 parts of mass fractions be the concentrated sulfuric acid of 90-98%, 15 parts of potassium peroxydisulfates, 15 parts of phosphorus pentoxides and
20 parts of graphite mixing carry out pre-oxidation.
3. the preparation method of graphene-based material precursor as described in claim 1, it is characterised in that: described in step (1)
Pre-oxidation temperature is 60-90 DEG C, and the pre-oxidation time is 3-5h.
4. the preparation method of graphene-based material precursor as claimed in claim 3, it is characterised in that: described in step (1)
Pre-oxidation temperature is 80 DEG C, and the pre-oxidation time is 4h.
5. the preparation method of graphene-based material precursor as described in claim 1, it is characterised in that: described in step (2)
It by weight, is 1400 parts of mass fractions to be added into 20-30 parts of pre-oxidation product A product in a low temperature of 0-5 DEG C as 90-
98% concentrated sulfuric acid and 100 parts of potassium permanganate.
6. the preparation method of graphene-based material precursor as described in claim 1, it is characterised in that: described in step (3)
It is that the hydrogen peroxide that 30-60mL mass fraction is 30-40% is added into 1-2L suspension B product to obtain mixture, then mixes gained
It closes object to be cleaned with the dilute hydrochloric acid of 2-5L, the concentration of the dilute hydrochloric acid is 2-5mol/L.
7. a kind of application of the graphene-based material precursor as described in claim 1-6, it is characterised in that: described graphene-based
Material precursor is applied to prepare graphene hydrogel.
8. a kind of application of the graphene-based material precursor as described in claim 1-6, it is characterised in that: described graphene-based
Material precursor is applied to prepare graphene aerogel.
9. a kind of application of the graphene-based material precursor as described in claim 1-6, it is characterised in that: described graphene-based
Material precursor is applied to prepare graphene film.
10. a kind of application of the graphene-based material precursor as described in claim 1-6, it is characterised in that: the graphene
Substrate material precursor is applied to prepare graphene fiber.
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| CN102145887A (en) * | 2011-05-18 | 2011-08-10 | 中国科学院长春应用化学研究所 | Method for preparing and purifying graphene oxide |
| WO2014134663A1 (en) * | 2013-03-08 | 2014-09-12 | Monash University | Graphene-based films |
| CN104445168A (en) * | 2014-11-28 | 2015-03-25 | 张明 | Preparation method of graphene oxide |
| CN105826083A (en) * | 2016-04-21 | 2016-08-03 | 贵州大学 | Preparation method of graphene-based electrode material and construction method of capacitor |
| CN108178146A (en) * | 2018-02-02 | 2018-06-19 | 贵州大学 | A kind of method for efficiently preparing high-energy density graphene aerogel |
| CN108455573A (en) * | 2018-02-02 | 2018-08-28 | 贵州大学 | A kind of preparation method of the loose stratiform graphene aerogel of tearing bread-like |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102145887A (en) * | 2011-05-18 | 2011-08-10 | 中国科学院长春应用化学研究所 | Method for preparing and purifying graphene oxide |
| WO2014134663A1 (en) * | 2013-03-08 | 2014-09-12 | Monash University | Graphene-based films |
| CN104445168A (en) * | 2014-11-28 | 2015-03-25 | 张明 | Preparation method of graphene oxide |
| CN105826083A (en) * | 2016-04-21 | 2016-08-03 | 贵州大学 | Preparation method of graphene-based electrode material and construction method of capacitor |
| CN108178146A (en) * | 2018-02-02 | 2018-06-19 | 贵州大学 | A kind of method for efficiently preparing high-energy density graphene aerogel |
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Application publication date: 20190222 |