CN108840333A - A kind of preparation method of cellular graphite oxide - Google Patents
A kind of preparation method of cellular graphite oxide Download PDFInfo
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- CN108840333A CN108840333A CN201810021555.2A CN201810021555A CN108840333A CN 108840333 A CN108840333 A CN 108840333A CN 201810021555 A CN201810021555 A CN 201810021555A CN 108840333 A CN108840333 A CN 108840333A
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Abstract
It the present invention provides a kind of preparation method of cellular graphite oxide, is dispersed graphite oxide in the mixed solution of the concentrated sulfuric acid and concentrated nitric acid, potassium chlorate is added, room temperature temperature is stirred to react 72 ~ 75h, obtains uniform graphite oxide reaction solution；It again disperses reaction solution in ultrapure water, adjusts pH value of solution to 6.5 ~ 7.5 with sodium hydroxide solution；Then products therefrom is centrifuged, collects sediment, ethyl alcohol and milli-Q water, freeze-drying obtains the graphite oxide of vesicular texture.Sem test is shown, graphite oxide porous structure prepared by the present invention is clear, lamella is larger, with enriching unique pore structure and hole abundant, both with the advantage of graphite oxide, the characteristics of having both porous material again, as a kind of application prospect that excellent composite material filler has been shown.
Description
Technical field
The present invention relates to a kind of preparation method of graphite oxide, especially a kind of preparation method of cellular graphite oxide belongs to
In technical field of nano material.
Background technique
Graphite oxide is the product after graphite oxidation, it is oxidation-treated after graphite oxide, surface is with abundant oxygen-containing
Group, such as-OH ,-C-O-C- and-COOH, these functional groups make graphite oxide have polarity, can be well dispersed in pole
In property solvent；This property of graphite oxide has greatly widened the purposes of graphite oxide, as a kind of composite material filler quilt
It is widely used in the various composite materials of synthesis；In addition, gained composite material not only increases the conduction of material after reduction
Property, simultaneously with the big specific surface area of graphite oxide, these all embody the advantage of graphite oxide well.
Porous material, be it is a kind of have be mutually communicated or closed hole constitute network structure material.Porous material one
As have relative density low, the advantages that specific surface area is high, good penetrability；Its application range is also considerably beyond the material of simple function
Material has important application in the various aspects such as organizational project, catalyst carrier, absorption carrier, separating and filtering material, electrode material,
It has been to be concerned by more and more people.Cavernous graphite oxide is a kind of novel nano material, combine graphite oxide and
The advantage of porous material will play preferably application in graphite oxide and the respective application field of porous material.
Summary of the invention
Mesh of the invention is to provide a kind of preparation method with vesicular texture graphite oxide.
A kind of preparation method of vesicular texture graphite oxide of the present invention, is to disperse graphite oxide in the concentrated sulfuric acid and dense nitre
In the mixed solution of acid, potassium chlorate is added, room temperature temperature is stirred to react 72 ~ 75h, and graphite oxide is more thoroughly removed and aoxidized and cut
It cuts, obtains uniform graphite oxide reaction solution；It again disperses reaction solution in 15 ~ 20mL ultrapure water, with 8 ~ 10mol/L's of concentration
Sodium hydroxide solution adjusts pH value of solution to 6.5 ~ 7.5, and potassium hydroxide present in solution can slowly carve graphite oxide
Erosion, oxidized graphite flake layer have certain expansion, while it is smaller scale abundant occur, equally distributed duct；Then will
Products therefrom centrifugation, collects sediment, ethyl alcohol and milli-Q water, freeze-drying, and surface coats liquid sublimation removal, obtains
The graphite oxide of vesicular texture.
The mass percent concentration of the concentrated sulfuric acid is 95 ~ 98%, and the mass fraction of concentrated nitric acid is 63 ~ 68%, and the concentrated sulfuric acid
Volume ratio with concentrated nitric acid is 2:1~2.5:1.
The dosage of the potassium chlorate is the 90 ~ 92% of graphite oxide quality.
Below by scanning electron microscope, infrared spectrogram, nitrogen adsorption desorption curve to a kind of cellular prepared by the present invention
The structure of structure graphite oxide carries out analytic explanation.
1, scanning electron microscope analysis
Fig. 1 is the scanning electron microscope (SEM) photograph of the graphite oxide of vesicular texture prepared by the present invention.Scanning electron microscope (SEM) photograph shows that gained aoxidizes
Graphite surface shows vesicular texture, so that graphite oxide has great specific surface area.Fig. 2,3 are the corresponding amplification of Fig. 1
Figure, can the clearer porous nano channel design indicated inside graphite oxide.It is by scanning electron microscope analysis as it can be seen that prepared
This cellular graphite oxide there is duct abundant, this cavernous graphite oxide can be used as a kind of excellent composite wood
Filler is expected to apply.
2, infrared analysis
Fig. 4 is the infrared spectrogram of prepared cellular graphite oxide.Infrared spectroscopy is shown, in 1103cm-1There is C-O- in place
The strong vibration absorption peak of C functional group, belongs to the absorption peak of epoxy group on graphite oxide；1620cm−1Locate the absorption peak occurred
Belong to the stretching vibration of C=C key；1730cm−1The absorption peak at place belongs to the absorption peak of C=O key on carbonyl；3400cm−1Place
It is that the stretching vibration of the O-H key of the hydrone absorbed by sample is generated.It is corresponding to occur graphite oxide in infrared spectroscopy
Characteristic peak, illustrate to be successfully prepared graphite oxide by this method.
3, nitrogen adsorption desorption curve
Nitrogen adsorption desorption curve further demonstrates some advantageous features of cellular graphite oxide, and Fig. 5 is to prepare cellular
Isothermal curve figure is desorbed in the nitrogen adsorption of graphite oxide.Illustrate the I type that gained thermoisopleth belongs in IUPAC classification, H4 lag
Ring has preferable platform, belongs to oxidized graphite flake layer and accumulates the slit pore that the layer structure to be formed generates.It can from Fig. 5
Out, sample is slowly increased in periods of low pressure adsorbance, and does not adsorb limitation in higher pressure region, and specific surface area is about 945
m2·g-1；In reported document, pure graphene specific surface area is about 358 m2˙g-1, the specific surface area of porous graphene is about
For 850m2·g-1, comparatively, the specific surface area of gained sample is bigger, illustrates graphite oxide due to the intercalation in reaction
So that the slit pore of its layer structure is more abundant.
In conclusion the cavernous graphite oxide that the present invention obtains, has and enriches this sample of unique porous structure
Not only the characteristics of having had the advantage of graphite oxide, but also having had both porous material, shows as a kind of excellent composite material filler
Good application prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that the present invention prepares cellular graphite oxide.
Fig. 2 is the enlarged drawing of Fig. 1.
Fig. 3 is the enlarged drawing of Fig. 2.
Fig. 4 is the infrared spectrogram that the present invention prepares cellular graphite oxide.
Fig. 5 is the nitrogen adsorption desorption isotherm that the present invention prepares cellular graphite oxide.
Specific embodiment
The preparation of cellular graphite oxide of the present invention is described in detail below by specific embodiment.
Embodiment 1
It disperses 1g graphite oxide in the mixed solution of the 18mL concentrated sulfuric acid and 9mL concentrated nitric acid, 11g potassium chlorate, room temperature temperature is added
It is stirred to react 72h, obtains uniform graphite oxide reaction solution；It disperses reaction solution in 20ml ultrapure water, with 4mol/L hydrogen-oxygen
Change sodium solution and adjusts pH value of solution to 7；Then products therefrom is centrifuged, sediment, ethyl alcohol and milli-Q water is collected, at -55 DEG C
Lower vacuum freeze drying for 24 hours, obtains the graphite oxide of vesicular texture.
Embodiment 2
It disperses 1g graphite oxide in the mixed solution of the 20mL concentrated sulfuric acid and 10mL concentrated nitric acid, 11g potassium chlorate, room temperature temperature is added
It is stirred to react 72h, obtains uniform graphite oxide reaction solution；It disperses gained reaction solution in 20ml ultrapure water, uses 4mol/L
Sodium hydroxide solution adjusts pH value of solution to 7；Then sediment, ethyl alcohol and milli-Q water is collected by centrifugation in products therefrom, -55
Vacuum freeze drying for 24 hours, obtains the graphite oxide of vesicular texture at DEG C.
Embodiment 3
It disperses 1g graphite oxide in the mixed solution of the 18mL concentrated sulfuric acid and 9mL concentrated nitric acid, 12g potassium chlorate, room temperature temperature is added
It is stirred to react 75h, obtains uniform graphite oxide reaction solution；It disperses gained reaction solution in 20ml ultrapure water, uses 5mol/L
Sodium hydroxide solution adjusts pH value of solution to 7；Then sediment, ethyl alcohol and milli-Q water is collected by centrifugation in products therefrom, -55
Vacuum freeze drying for 24 hours, obtains the graphite oxide of vesicular texture at DEG C.
Embodiment 4
It disperses 1g graphite oxide in the mixed solution of the 20mL concentrated sulfuric acid and 10mL concentrated nitric acid, 12g potassium chlorate, room temperature temperature is added
It is stirred to react 75h, obtains uniform graphite oxide reaction solution；It disperses gained reaction solution in 20ml ultrapure water, uses 5mol/L
Sodium hydroxide solution adjusts pH value of solution to 7；Then sediment, ethyl alcohol and milli-Q water is collected by centrifugation in products therefrom, -55
Vacuum freeze drying for 24 hours, obtains the graphite oxide of vesicular texture at DEG C.
Claims (5)
1. a kind of preparation method of cellular graphite oxide, is the mixed solution for dispersing graphite oxide in the concentrated sulfuric acid and concentrated nitric acid
In, potassium chlorate is added, room temperature temperature is stirred to react 72 ~ 75h, obtains uniform graphite oxide reaction solution；Again disperse reaction solution in
In ultrapure water, pH value of solution is adjusted to 6.5 ~ 7.5 with sodium hydroxide solution；Then products therefrom is centrifuged, collects sediment, ethyl alcohol
And milli-Q water, it is dry, obtain the graphite oxide of vesicular texture.
2. a kind of preparation method of cellular graphite oxide as described in claim 1, it is characterised in that：The concentrated sulfuric acid quality hundred
Dividing specific concentration is 95 ~ 98%, and the mass fraction of concentrated nitric acid is 63 ~ 68%, and the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 2:1~2.5:
1。
3. a kind of preparation method of cellular graphite oxide as described in claim 1, it is characterised in that：The dosage of the potassium chlorate
It is the 90 ~ 92% of graphite oxide quality.
4. a kind of preparation method of cellular graphite oxide as described in claim 1, it is characterised in that：The NaOH solution concentration
For 8 ~ 10mol/L.
5. a kind of preparation method of cellular graphite oxide as described in claim 1, it is characterised in that：The drying is -50
Vacuum freeze drying 20 at ~ -60 DEG C ~ for 24 hours.
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Application publication date: 20181120 |