CN105967175A - Preparation method of water-soluble fluorinated graphene - Google Patents
Preparation method of water-soluble fluorinated graphene Download PDFInfo
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- CN105967175A CN105967175A CN201610320893.7A CN201610320893A CN105967175A CN 105967175 A CN105967175 A CN 105967175A CN 201610320893 A CN201610320893 A CN 201610320893A CN 105967175 A CN105967175 A CN 105967175A
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- soluble fluorine
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
Abstract
The invention provides a preparation method of water-soluble fluorinated graphene. The method comprises the steps of providing graphene oxide; dispersing the graphene oxide into deionized water to form a graphene oxide solution, then adding hydrofluoric acid and concentrated nitric acid into the graphene oxide solution, carrying out a reaction for 5-30 hours, and controlling the temperature of the reaction solution to be 150-200 DEG C; after the reaction, evaporating the product to dry to obtain the water-soluble fluorinated graphene. The preparation method is simple in technology and low in cost; the obtained water-soluble fluorinated graphene product has better dispersity.
Description
Technical field
The present invention relates to Material Field, be specifically related to the preparation method of a kind of water-soluble fluorine functionalized graphene.
Background technology
Graphene (Graphene) is a kind of monolayer carbon atom through the tightly packed bi-dimensional cellular shape carbon back novel nano-material of sp2 hydridization, has superior physics, chemical property, such as the theoretical specific surface area (2630 of super large
m2/ g), high heat conductance (5000
W/m K) and high conductivity (64 mS/cm) etc., in fields such as energy storage and conversion, electronic device, bio-sensings, there is huge using value.By carrying out addition or the replacement of fluorine on graphene carbon atomic layer, the band gap of Graphene can be regulated, change the Chemical response characteristic of Graphene so that it is there is in fields such as semiconductor device, field-effect transistor, bio-sensings the character being more suitable for.Additionally, due to fluorine is distributed seldom in human body, and NMR (Nuclear Magnetic Resonance)-imaging can be carried out, so also there is extremely attractive application prospect in fields such as biological standardization, medicine tracking.
At present, the synthesis of fluorinated graphene relies primarily on strong fluorination reagent such as fluorine gas, xenon difluoride and Graphene direct reaction.Although this kind of method is quickly effective, but compared with high, consersion unit, cost of material requires that harshness, operational danger are big.Additionally, fluorinated graphene can also be obtained by the mechanically or chemically stripping of fluorographite, because raw material the most directly uses Graphene, so reducing reaction cost, but owing to being difficult to control to the stripping of monolayer carbon atom, the products therefrom often number of plies is bigger, and the fluorographite mechanically or chemically peeling off preparation is to utilize fluorine gas to produce with the reaction of graphite, still suffer from consersion unit requirement big shortcoming high, dangerous, and the fluorinated graphene prepared of above two method there is also the defect of bad dispersibility, greatly limit its using value.
In order to solve with present on problem, people are seeking a kind of preferably technical solution always.
Summary of the invention
It is an object of the invention to for the deficiencies in the prior art, thus provide that a kind of technique is simple, with low cost, the preparation method of the water-soluble fluorine functionalized graphene of products obtained therefrom favorable dispersibility.
To achieve these goals, the technical solution adopted in the present invention is: the preparation method of a kind of water-soluble fluorine functionalized graphene, and concrete steps include:
A kind of graphene oxide is provided；
Described graphene oxide is scattered in deionized water formation graphene oxide solution, then in described graphene oxide solution, add Fluohydric acid. and concentrated nitric acid carries out reacting 5 hours～30 hours, controlling solution temperature is 150 DEG C～200 DEG C, and reaction obtains water-soluble fluorine functionalized graphene through being evaporated to dryness after terminating.Wherein, for preventing solution from splashing during being evaporated to dryness, temperature should control below 100 DEG C, and because Fluohydric acid. can react with glass drying oven, the container of course of reaction should select the container of hydrofluoric acid resistant material, such as polytetrafluoroethylcontainer container etc..
Based on above-mentioned, the step providing a kind of described graphene oxide includes: graphite raw material, oxidant is carried out hybrid reaction with solvent and obtains yellow suspension, wherein, before controlling reaction solution, the temperature of two hours is less than 20 DEG C, and the temperature controlling described reaction solution after reacting 2 hours is 30 DEG C～40 DEG C；
Deionized water is added in described yellow suspension, carry out mixing 1～3 hour under the conditions of temperature is 90 DEG C～100 DEG C, entering hydrogenperoxide steam generator after being cooled to room temperature wherein and carry out centrifuging treatment and obtain supernatant and lower sediment, described supernatant prepares described graphene oxide after being evaporated to dryness process.
Based on above-mentioned, the step providing a kind of described graphene oxide also includes, it is respectively adopted hydrochloric acid and deionization described lower sediment is washed, then the described lower sediment after washing is scattered in deionized water and is centrifuged separating treatment, then the supernatant of centrifugation gained is evaporated to dry-cure step by step.
Based on above-mentioned, described oxidant is sodium nitrate and potassium permanganate, and described solvent is concentrated sulphuric acid.
Based on above-mentioned, in the step preparing described water-soluble fluorine functionalized graphene, the concentration of described graphene oxide solution is 0.5～2 mg/mL.
Based on above-mentioned, preparing the mass fraction of nitric acid in the reaction solution system of described water-soluble fluorine functionalized graphene is 10%～20%.
Based on above-mentioned, preparing the mass fraction of Fluohydric acid. in the reaction solution system of described water-soluble fluorine functionalized graphene is 1%～10%.
Hinge structure of the present invention has prominent substantive distinguishing features and significantly progress, specifically, the present invention uses graphene oxide to be raw material, with the mixed solution of Fluohydric acid. and nitric acid as reaction medium, carry out the fluorination process of described graphene oxide thus prepare described water-soluble fluorine functionalized graphene, nitric acid composition in reaction medium, it is possible not only to avoid graphene oxide and Fluohydric acid. to react generation Precipitation under hydrothermal conditions, improve fluorinated graphene dispersibility in aqueous, more active group can also be manufactured on described graphene oxide by the Oxidation of nitric acid self, fluorination process for graphene oxide provides more reaction site, improve the productivity of fluorinated graphene.
Further, the present invention uses graphite and sodium nitrate and potassium permanganate and concentrated sulphuric acid to react, prepare described graphene oxide, described graphite is the raw material that conventional method prepares Graphene, its price is cheaper than Graphene, and in the fluorination process to described graphene oxide, fluorization agent is the mixed solution of Fluohydric acid. and nitric acid, do not use severe corrosive, the high risk fluorination reagents such as the fluorine gas used by conventional fluorinated graphene production or xenon difluoride, therefore, the method technique is simple, with low cost.
Test proves: the described water-soluble fluorine functionalized graphene that the preparation method having the present invention to provide prepares shows through infrared detection, at 1000cm-1～1250 cm-1In the range of occur in that the peak representing C-F structure, therefore illustrate to be successfully realized by preparation method of the present invention the fluorination process of graphene oxide, thus prepared water-soluble fluorine functionalized graphene.And, described water-soluble fluorine functionalized graphene material weight-loss ratio when temperature is less than 500 DEG C is bigger, steady statue is reached when temperature is 500 DEG C, described water-soluble fluorine functionalized graphene can be with stable dispersion in the case of the neutral aqueous solution without any surfactant, within 6 months, have no layering, there is good dispersibility.
Accompanying drawing explanation
Fig. 1 is graphene oxide pictorial diagram prepared by the present invention.
Fig. 2 is the pictorial diagram of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 3 is the full spectrogram of x-ray photoelectron power spectrum of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 4 is the x-ray photoelectron power spectrum fluorine spectrogram of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 5 is the infrared spectrum of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 6 is the thermogravimetric curve of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 7 is the pictorial diagram of 300 DEG C of thermal decomposition products of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 8 is the pictorial diagram of 400 DEG C of thermal decomposition products of water-soluble fluorine functionalized graphene prepared by the present invention.
Fig. 9 is the pictorial diagram of 600 DEG C of thermal decomposition products of water-soluble fluorine functionalized graphene prepared by the present invention.
Detailed description of the invention
Below by detailed description of the invention, technical scheme is described in further detail.
Embodiment
1
The present embodiment provides the preparation method of a kind of water-soluble fluorine functionalized graphene, and concrete steps include:
The synthesis of graphene oxide: weigh 2.0 g crystalline flake graphites and 1.0 g sodium nitrates, join in 46 mL concentrated sulphuric acids, is slowly added to the potassium permanganate of 6 g under frozen water water-bath wherein, and the temperature controlling reaction solution is 15DEG C it is stirred reacting 2 hours, then described reaction solution temperature is risen to 40DEG C carrying out reacting to solution is that yellow obtains yellow suspension, adds 92 mL deionized waters and be warming up to 90 in described yellow suspensionDEG C being stirred reacting 2 hours, after reaction end is cooled to room temperature, then adds 15 mL hydrogenperoxide steam generators in described reaction solution and be centrifuged separating treatment, controlling centrifugal speed is 5000
R/min, thus obtain first separation supernatant and lower sediment；
Described lower sediment is respectively washed three times through deionized water and the hydrochloric acid that mass fraction is 5%, then by the described lower sediment ultrasonic disperse after washing in deionized water, is 8000 in centrifugal speed
Under the conditions of r/min, it is centrifuged isolated secondary separation supernatant, the described secondary separation supernatant of gained is placed in air blast be evaporated to dryness in case be evaporated to dryness at 50 DEG C i.e. obtain good dispersion, graphene oxide that impurity content is low, as it is shown in figure 1, the graphene oxide pictorial diagram prepared for the present invention.
The preparation of water-soluble fluorine functionalized graphene: the described graphene oxide ultrasonic disperse of 200 mg is formed graphene oxide solution in the deionized water of 100 ml, Fluohydric acid. and the concentrated nitric acid of 42.9 mg of 85.8 mg is added in described graphene oxide solution, control the mass fraction of nitric acid in reaction solution system be 20%, the mass fraction of Fluohydric acid. be 10%, transfer in pyroreaction still after stirring, 180React 30 hours at DEG C, after cooling, obtain water-soluble fluorine functionalized graphene through being evaporated to dryness, as in figure 2 it is shown, the water-soluble fluorine functionalized graphene pictorial diagram prepared for the present invention.
Described water-soluble fluorine functionalized graphene detects through X-ray, result is as shown in Figure 3 and Figure 4, its x-ray photoelectron power spectrum showing, the content that this material contains C, O, F element and F element is higher, do not contain other elements, thus confirm in reaction solution and can manufacture more active group on described graphene oxide by the Oxidation of nitric acid self, the fluorination process for graphene oxide provides more reaction site.
Described water-soluble fluorine functionalized graphene is through infrared detection, and result is as it is shown in figure 5, at 1000cm-1～1250 cm-1In the range of occur in that the peak representing C-F structure, therefore explanation the method is successfully realized the fluorination process of graphene oxide, thus has prepared described water-soluble fluorine functionalized graphene.
Described water-soluble fluorine functionalized graphene through thermogravimetric test and 300 DEG C, 400 DEG C, carry out thermal decomposition test at a temperature of 600 DEG C, result is respectively as shown in Fig. 6, Fig. 7, Fig. 8 and Fig. 9, as can be seen from the figure when temperature is less than 500 DEG C, material weight-loss ratio is relatively big, reaches steady statue when temperature is 500 DEG C.
The dispersion experiment test result of described water-soluble fluorine functionalized graphene shows: concentration is that the described water-soluble fluorine functionalized graphene of 2 mg/mL can have no layering in 6 months with stable dispersion in the case of the neutral aqueous solution without any surfactant.
Embodiment
2
The present embodiment provides the preparation method of a kind of water-soluble fluorine functionalized graphene, and concrete steps are roughly the same with the step in embodiment 1, and the proportioning raw materials that difference is in each step is different with parameter:
In the synthesis step of described graphene oxide, control the temperature of reaction solution after reaction 2 hours be 30 DEG C of reaction to solution be yellow；
In the preparation process of described water-soluble fluorine functionalized graphene, the concentration of described graphene oxide solution is 0.5 mg/mL, and the mass fraction of nitric acid described in reaction solution system is 10%, the mass fraction of described Fluohydric acid. is 1%.
The described water-soluble fluorine functionalized graphene that the present embodiment provides is through infrared detection, at 1000cm-1～1250 cm-1In the range of occur in that the peak representing C-F structure, therefore explanation is successfully realized the fluorination process of graphene oxide, thus has prepared water-soluble fluorine functionalized graphene.And, described water-soluble fluorine functionalized graphene material weight-loss ratio when temperature is less than 500 DEG C is relatively big, reaches steady statue when temperature is 500 DEG C.The dispersion experiment test result of described water-soluble fluorine functionalized graphene shows: concentration is that the described water-soluble fluorine functionalized graphene of 1 mg/mL can have no layering in 6 months with stable dispersion in the case of the neutral aqueous solution without any surfactant.
Embodiment
3
The present embodiment provides the preparation method of a kind of water-soluble fluorine functionalized graphene, and concrete steps are roughly the same with the step in embodiment 1, and the proportioning raw materials that difference is in each step is different with parameter:
In the synthesis step of described graphene oxide, dried crystalline flake graphite 1.0 g is joined in the four-hole boiling flask equipped with sodium nitrate 1.0 g and concentrated sulphuric acid 30 mL mixture, ultrasonic mix homogeneously, stirs and is slowly added to potassium permanganate 6.0 g in ice-water bath, and the temperature controlling reaction solution is 10DEG C it is stirred reacting 2 hours, then described reaction solution temperature is risen to 35DEG C carrying out reacting to solution is that yellow obtains yellow suspension, adds 100 mL deionized waters and be warming up to 90 in described yellow suspensionDEG C being stirred reacting 2 hours, after reaction end is cooled to room temperature, then adds 15 mL hydrogenperoxide steam generators in described reaction solution and be centrifuged separating treatment, controlling centrifugal speed is 5000
R/min, thus obtain first separation supernatant and lower sediment；
In the preparation process of described water-soluble fluorine functionalized graphene, the concentration of described graphene oxide solution is 2 mg/mL, and the mass fraction of nitric acid described in reaction solution system is 15%, the mass fraction of described Fluohydric acid. is 5%.
The described water-soluble fluorine functionalized graphene that the present embodiment provides is through infrared detection, at 1000cm-1～1250 cm-1In the range of occur in that the peak representing C-F structure, therefore explanation is successfully realized the fluorination process of graphene oxide, thus has prepared water-soluble fluorine functionalized graphene.And, described water-soluble fluorine functionalized graphene material weight-loss ratio when temperature is less than 500 DEG C is relatively big, reaches steady statue when temperature is 500 DEG C.The dispersion experiment test result of described water-soluble fluorine functionalized graphene shows: concentration is 0.5
The described water-soluble fluorine functionalized graphene of mg/mL can have no layering in 6 months with stable dispersion in the case of the neutral aqueous solution without any surfactant.
Finally should be noted that: above example is only in order to illustrate that technical scheme is not intended to limit；Although being described in detail the present invention with reference to preferred embodiment, those of ordinary skill in the field are it is understood that still can modify to the detailed description of the invention of the present invention or portion of techniques feature is carried out equivalent；Without deviating from the spirit of technical solution of the present invention, it all should be contained in the middle of the technical scheme scope that the present invention is claimed.
Claims (7)
1. a preparation method for water-soluble fluorine functionalized graphene, concrete steps include:
A kind of graphene oxide is provided；
Described graphene oxide is scattered in deionized water formation graphene oxide solution, then in described graphene oxide solution, add Fluohydric acid. and concentrated nitric acid, carry out reacting 5～30 hours under the conditions of temperature is 150 DEG C～200 DEG C, react after terminating through being evaporated to dryness prepared water-soluble fluorine functionalized graphene.
The preparation method of water-soluble fluorine functionalized graphene the most according to claim 1, it is characterized in that, the step providing a kind of described graphene oxide includes: graphite raw material, oxidant is carried out hybrid reaction with solvent and obtains yellow suspension, before wherein controlling reaction solution, the temperature of two hours is less than 20 DEG C, and the temperature controlling described reaction solution after reacting 2 hours is 30 DEG C～40 DEG C；
Deionized water is added in described yellow suspension, carry out mixing 1～3 hour under the conditions of temperature is 90 DEG C～100 DEG C, enter hydrogenperoxide steam generator after being cooled to room temperature wherein and carry out centrifuging treatment, obtaining supernatant and lower sediment, described supernatant prepares described graphene oxide after being evaporated to dryness process.
The preparation method of water-soluble fluorine functionalized graphene the most according to claim 2, it is characterized in that, the step providing a kind of described graphene oxide also includes, it is respectively adopted hydrochloric acid and deionization described lower sediment is washed, then the described lower sediment after washing is scattered in deionized water and is centrifuged separating treatment, then the supernatant of centrifugation gained is evaporated to dry-cure step by step.
The preparation method of water-soluble fluorine functionalized graphene the most according to claim 2, it is characterised in that described oxidant is sodium nitrate and potassium permanganate, described solvent is concentrated sulphuric acid.
5., according to the preparation method of the water-soluble fluorine functionalized graphene described in any one of Claims 1 to 4, it is characterised in that prepare in the step of described water-soluble fluorine functionalized graphene, the concentration of described graphene oxide solution is 0.5～2 mg/mL.
The preparation method of water-soluble fluorine functionalized graphene the most according to claim 5, it is characterised in that preparing the mass fraction of nitric acid in the reaction solution system of described water-soluble fluorine functionalized graphene is 10%～20%.
The preparation method of water-soluble fluorine functionalized graphene the most according to claim 6, it is characterised in that preparing the mass fraction of Fluohydric acid. in the reaction solution system of described water-soluble fluorine functionalized graphene is 1%～10%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117599A (en) * | 2017-04-19 | 2017-09-01 | 东华大学 | A kind of preparation method of the miscellaneous graphene of chlorine |
| CN107879328A (en) * | 2017-11-29 | 2018-04-06 | 科凯精细化工（上海）有限公司 | A kind of preparation method of water dispersible fluorinated graphene |
| CN108245433A (en) * | 2017-12-21 | 2018-07-06 | 中国科学院兰州化学物理研究所 | A kind of novel mouth section glass ionomer/fluorinated graphene composite material |
| CN108264036A (en) * | 2018-03-29 | 2018-07-10 | 中国科学院福建物质结构研究所 | A kind of preparation method of fluorine graphene oxide |
| CN108484909A (en) * | 2018-03-29 | 2018-09-04 | 中国科学院福建物质结构研究所 | A kind of fluorine graphene oxide/composite polyimide material and its preparation method and application |
| CN112473065A (en) * | 2020-12-07 | 2021-03-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof |
| CN114350114A (en) * | 2022-01-21 | 2022-04-15 | 中国科学院山西煤炭化学研究所 | Fluorine-doped graphene oxide modified epoxy resin and preparation method of carbon fiber composite material thereof |
| CN115028163A (en) * | 2022-06-23 | 2022-09-09 | 湖南科技大学 | Preparation method of highly fluorinated graphene |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107117599A (en) * | 2017-04-19 | 2017-09-01 | 东华大学 | A kind of preparation method of the miscellaneous graphene of chlorine |
| CN107117599B (en) * | 2017-04-19 | 2020-11-13 | 东华大学 | Preparation method of chloro-hybrid graphene |
| CN107879328A (en) * | 2017-11-29 | 2018-04-06 | 科凯精细化工（上海）有限公司 | A kind of preparation method of water dispersible fluorinated graphene |
| CN108245433A (en) * | 2017-12-21 | 2018-07-06 | 中国科学院兰州化学物理研究所 | A kind of novel mouth section glass ionomer/fluorinated graphene composite material |
| CN108264036A (en) * | 2018-03-29 | 2018-07-10 | 中国科学院福建物质结构研究所 | A kind of preparation method of fluorine graphene oxide |
| CN108484909A (en) * | 2018-03-29 | 2018-09-04 | 中国科学院福建物质结构研究所 | A kind of fluorine graphene oxide/composite polyimide material and its preparation method and application |
| CN108484909B (en) * | 2018-03-29 | 2020-07-31 | 中国科学院福建物质结构研究所 | Fluorine oxidized graphene/polyimide composite material and preparation method and application thereof |
| CN112473065A (en) * | 2020-12-07 | 2021-03-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof |
| CN112473065B (en) * | 2020-12-07 | 2022-04-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof |
| CN114350114A (en) * | 2022-01-21 | 2022-04-15 | 中国科学院山西煤炭化学研究所 | Fluorine-doped graphene oxide modified epoxy resin and preparation method of carbon fiber composite material thereof |
| CN114350114B (en) * | 2022-01-21 | 2023-03-14 | 中国科学院山西煤炭化学研究所 | Fluorine-doped graphene oxide modified epoxy resin and preparation method of carbon fiber composite material thereof |
| CN115028163A (en) * | 2022-06-23 | 2022-09-09 | 湖南科技大学 | Preparation method of highly fluorinated graphene |
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Application publication date: 20160928 |