CN104064375B - Method for compounding ternary composite membrane of cellulose, graphene oxide and carbon nano tube in ionic liquid - Google Patents
Method for compounding ternary composite membrane of cellulose, graphene oxide and carbon nano tube in ionic liquid Download PDFInfo
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- CN104064375B CN104064375B CN201410323347.XA CN201410323347A CN104064375B CN 104064375 B CN104064375 B CN 104064375B CN 201410323347 A CN201410323347 A CN 201410323347A CN 104064375 B CN104064375 B CN 104064375B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a preparing method of cellulose composite materials, and discloses a method for compounding a ternary composite membrane of cellulose, graphene oxide and a carbon nano tube in ionic liquid to solve the technical problem that cellulose composite aerogel prepared based on an existing method is low in strength and prone to collapsing and deforming. The method comprises the steps that the carbon nano tube and graphene oxide dispersion liquid dispersed into organic solvent are added into the ionic liquid solution of cellulose, temperature is increased, stirring is carried out, repeated washing and suction filtration forming are carried out, and after vacuum drying at the normal temperature, the cellulose/carbon nano tube/graphene oxide ternary composite membrane is obtained. The ternary composite membrane of the cellulose, the graphene oxide and the carbon nano tube can be used in a supercapacitor.
Description
Technical field
The invention belongs to material science, more particularly to one kind synthetic cellulose and graphite oxide under ionic liquid
The method of alkene and carbon nanometer pipe ternary composite membrane.
Background technology
Natural plant cellulose is one of natural organic matter most abundant on the earth, it account for the 50% of plant kingdom's carbon content with
On, can synthesize about 1.5 × 10 by photosynthesis every year12t.In recent years, with the rapidly soaring of oil equal energy source price and
Sustainable development in the urgent need to natural plant cellulose is increasingly taken seriously as eco-friendly Renewable resource.It is fine
Dimension have fine network structure, by the use of cellulose as matrix, so as to replace relatively expensive synthesis macromolecule, same to recurrence of disease at the same time next year
With the performance of wherein every material, the cellulose base Graphene/carbon nanotube composite material prepared has excellent condensation material
Good mechanical property and capacitive property, can make EMI shield, chemically modified electrode, ultracapacitor etc..Patent
Number a kind of method for preparing cellulose composite aerogel is disclosed for 201110274091.4 Chinese patent, it is first that cellulose is molten
Solution in alkaline solution, subsequently dispersing Nano carbon tubes, graphene oxide or redox graphene in this solution system, then lead to
Cross gelation, solvent exchange, dry run and obtain cellulose composite aerogel.The method gel in solvent exchange procedure because
Structure collapses, deformation are easily caused for gel strength is low.
The content of the invention
The present invention is to solve the cellulose composite aerogel low intensity of existing method preparation, the skill easily caved in, deform
Art problem, and a kind of synthetic cellulose under ionic liquid is provided with graphene oxide and the side of carbon nanometer pipe ternary composite membrane
Method.
A kind of synthetic cellulose under ionic liquid and the graphene oxide of the present invention and carbon nanometer pipe ternary composite membrane
Method is carried out according to the following steps:
First, the cellulose for weighing 1~15 part of parts by weight is added in the ionic liquid of 100 parts of parts by weight, 60~100
4~12h of stirring and dissolving obtains cellulose solution to being completely dissolved at DEG C;
2nd, graphene oxide and CNT are separately added in solvent, are uniformly dispersed, obtain graphene oxide dispersion
And carbon nano tube dispersion liquid;
3rd, the graphene oxide dispersion and carbon nano tube dispersion liquid for obtaining step 2 is added to the fibre that step one is obtained
In the plain solution of dimension, 8~24h of stirring reaction, obtains mixed solution at 70~100 DEG C;
4th, the mixed solution obtained by step 3 is added to into cyclic washing in distilled water, then carries out filtration under diminished pressure, obtained
Wet film, then wet film is put in vacuum drying oven, under vacuum drying at room temperature is to constant weight, obtain cellulose/graphene oxide/
Carbon nanometer pipe ternary composite membrane.
The present invention is a kind of in ionic liquid system synthetic cellulose and graphene oxide and the method for carbon nano-tube compound film.
First graphene oxide and CNT are dispersed in organic solvent, after CNT is added to graphene oxide dispersion
In cellulose ionic liquid solution, heating is made between graphene oxide, CNT and cellulosic molecule mutually using mechanical agitation
Effect, forms the membrane material of composite construction, under the preparation condition of the present invention, the active bond and graphite oxide of cellulose surface
Alkene, CNT combination are strong, so as to get composite membrane mechanical strength improve, structural stability improve.This method has
Process conditions are simple, and stability is high, and reaction production safety degree is high, and raw material is easy to get, and reaction condition is gentle, and preparation cost is low, gained
Product does not contain objectionable impurities, environmentally safe and the features such as ionic liquid can be recycled.
Cellulose/graphene oxide/carbon nanometer pipe ternary composite membrane can obtain different shapes by different processing modes
State.The composite membrane has many excellent performances, the such as good toughness of cellulose, the good machine of graphene oxide and CNT
Tool performance and electric conductivity, in can be used for ultracapacitor.
Description of the drawings
Fig. 1 is the X-ray diffraction spectra figure of the cellulose for testing 1;
Fig. 2 is the X-ray diffraction spectra figure of the CNT for testing 1.
Fig. 3 is the X-ray diffraction spectra figure of the graphene oxide for testing 1.
Fig. 4 is to test 1 cellulose for preparing with CNT and the X-ray diffraction spectra figure of graphene oxide composite membrane.
Fig. 5 is to test 1 cellulose for preparing with CNT and the cyclic voltammogram of graphene oxide composite membrane.
Fig. 6 is Fu for testing cellulose, graphene oxide, cellulose and CNT and graphene oxide composite membrane in 1
Vertical leaf transformation infrared spectrogram.
Fig. 7 is the scanning electron microscope (SEM) of cellulose and CNT and the graphene oxide composite membrane for testing 1
Sectional view.
Fig. 8 is Fu for testing cellulose, graphene oxide, cellulose and CNT and graphene oxide composite membrane in 2
Vertical leaf transformation infrared spectrogram.
Fig. 9 is the scanning electron microscope (SEM) of cellulose and CNT and the graphene oxide composite membrane for testing 3
Plane graph.
Figure 10 is the scanning electron microscope (SEM) of cellulose and CNT and the graphene oxide composite membrane for testing 3
Sectional view.
Specific embodiment
Specific embodiment one:One kind of present embodiment synthetic cellulose and graphene oxide and carbon under ionic liquid
The method of nanotube tri compound film is carried out according to the following steps:
First, the cellulose for weighing 1~15 part of parts by weight is added in the ionic liquid of 100 parts of parts by weight, 60~100
4~12h is stirred at DEG C, cellulose solution is obtained;
2nd, graphene oxide and CNT are separately added in solvent, are uniformly dispersed, obtain graphene oxide dispersion
And carbon nano tube dispersion liquid;
3rd, the graphene oxide dispersion and carbon nano tube dispersion liquid for obtaining step 2 is added to the fibre that step one is obtained
In the plain solution of dimension, 8~24h of stirring reaction, obtains mixed solution at 70~100 DEG C;
4th, the mixed solution obtained by step 3 is added to into cyclic washing in distilled water, then carries out filtration under diminished pressure, obtained
Wet film, then wet film is put in vacuum drying oven, under vacuum drying at room temperature is to constant weight, obtain cellulose/graphene oxide/
Carbon nanometer pipe ternary composite membrane.
Specific embodiment two:Present embodiment and the cellulose unlike specific embodiment one described in step one
For chemical cellulose.Other are identical with specific embodiment one.
Specific embodiment three:Present embodiment and step one intermediate ion liquid unlike specific embodiment one or two
For 1- butyl -3- methylimidazole villaumites.Other are identical with specific embodiment one or two.
Specific embodiment four:Fiber in step one unlike one of present embodiment and specific embodiment one to three
Element is (1~15) with the mass ratio of ionic liquid:100.Other are identical with one of specific embodiment one to three.
Has full embodiment five;80 in step one unlike one of present embodiment and specific embodiment one to four
8h is stirred at DEG C.Other are identical with one of specific embodiment one to four.
Specific embodiment six:Unlike one of present embodiment and specific embodiment one to five described in step 2
CNT be surface treated CNT, the process of surface treatment is:By the concentrated nitric acid that mass concentration is 70%
It is 1 with the volume ratio of the concentrated sulphuric acid that mass concentration is 98%:3, concentrated nitric acid is mixed homogeneously with concentrated sulphuric acid, nitration mixture is obtained, by carbon
Nanotube is dispersed in nitration mixture, and flow back 2h under conditions of temperature is for 70 DEG C, then clean with deionized water with dilute hydrochloric acid successively,
It is vacuum dried again, completes the surface treatment of CNT.Other are identical with one of specific embodiment one to five.
Specific embodiment seven:Unlike one of present embodiment and specific embodiment one to six described in step 2
Solvent be N,N-dimethylformamide (DMF), DMAC N,N' dimethyl acetamide (DMAc) or dimethyl sulfoxide (DMSO).Other with
One of specific embodiment one to six is identical.
Specific embodiment eight:Aoxidize in step 3 unlike one of present embodiment and specific embodiment one to seven
The gross mass of Graphene and CNT is (0.5~10) with the ratio of the quality of cellulose:100, graphene oxide and carbon nanometer
The mass ratio of pipe is (0.1~10):1.Other are identical with one of specific embodiment one to seven.
With following verification experimental verification beneficial effects of the present invention:
Test 1:One kind of this test synthetic cellulose under ionic liquid is multiple with graphene oxide and carbon nanometer pipe ternary
Closing the method for film is carried out according to the following steps:
First, 0.4g celluloses are added in the 1- butyl -3- methylimidazole villaumites of 15g, and stirring and dissolving 10h is extremely at 80 DEG C
It is completely dissolved, obtains cellulose solution;
2nd, graphene oxide, surface-treated CNT are added separately in N,N-dimethylformamide (DMF)
It is configured to suspension that concentration is 20mg/ml and ultrasound makes it be uniformly dispersed, obtains graphene oxide dispersion and CNT point
Dispersion liquid;The surface treatment process of wherein CNT is specially:It is by the concentrated nitric acid and mass concentration that mass concentration is 70%
The volume ratio of 98% concentrated sulphuric acid is 1:3, concentrated nitric acid is mixed homogeneously with concentrated sulphuric acid, nitration mixture is obtained, CNT is dispersed in
In nitration mixture, flow back 2h under conditions of temperature is for 70 DEG C, then clean with deionized water with dilute hydrochloric acid successively, then is vacuum dried,
Complete the surface treatment of CNT;
3rd, the graphene oxide dispersion and carbon nano tube dispersion liquid for obtaining step 2 is added to the fibre that step one is obtained
In the plain solution of dimension, stirring reaction 12h at 80 DEG C obtains mixed solution;Wherein, the mass ratio of graphene oxide and CNT
For 1:1, the ratio of the quality sum and cellulose quality of graphene oxide and CNT is 1:25;
4th, the mixed solution obtained by step 3 is added to into cyclic washing 3 times in distilled water, then carries out filtration under diminished pressure,
Wet film is obtained, then wet film is put in vacuum drying oven, under vacuum drying at room temperature obtains cellulose/oxidation stone to constant weight
Black alkene/carbon nanometer pipe ternary composite membrane.
The X-ray diffraction spectra figure of the cellulose described in step one is as shown in figure 1, the CNT described in step 2
X-ray diffraction spectra figure as shown in Fig. 2 the graphene oxide described in step 2 X-ray diffraction spectra figure as shown in figure 3,
The X-ray diffraction spectra figure of cellulose/graphene oxide/carbon nanometer pipe ternary composite membrane that this test one is obtained as shown in figure 4,
Relatively Fig. 1~4 understand that X-ray diffraction peak can find correspondence peak on Fig. 4 on Fig. 1,2,3, illustrate that pluralgel is by fibre
Dimension element, CNT, graphene oxide tri compound is formed, wherein containing only these three compositions.
Cellulose/graphene oxide/carbon nanometer pipe ternary composite membrane that this test is obtained is put in Muffle furnace 700
DEG C, N2Calcination 6 hours is carried out under protection, powder is obtained, with the powder capacity measurement is carried out, (carried out by electrochemical workstation
Cyclic voltammetry, used as reference electrode, used as to electrode, sample is working electrode to platinum electrode to calomel electrode, electronegative potential for-
0.2V, high potential is 0.6V, scan 6 sections of hop count, sensitivity is 1.e-002), the cyclic voltammetry curve for obtaining as shown in figure 5, its
Middle a is that scanning speed is the cyclic voltammetry curve under the conditions of 100mv/s, and b is that scanning speed is the circulation volt under the conditions of 20mv/s
Peace curve, c is that scanning speed is the cyclic voltammetry curve under the conditions of 5mv/s, from fig. 5, it can be seen that the powder that this test is obtained
Electrical property it is preferable.
Fig. 6 is the Fourier transform infrared spectroscopy of material in this test, and wherein a is cellulose fourier-transform infrared light
Spectrum, the Fourier transform infrared spectroscopy of b graphene oxides, c is cellulose and CNT and graphite oxide prepared by this test
The Fourier transform infrared spectroscopy figure of alkene composite membrane.Knowable in infrared figure, with the addition of graphene oxide and CNT,
The absorption peak strength of cellulose is greatly reduced.
Fig. 7 is the scanning electron microscope (SEM) photograph (SEM) of composite membrane section, as we can see from the figure the lamella knot of obvious Graphene
Structure, and the linear structure of CNT, its CNT plays longitudinal phase support, and Graphene plays a part of to improve mechanical strength.
By one-dimensional material with carbon element CNT and Two-dimensional Carbon material oxidation Graphene, formed in the presence of cellulose 3-D solid structure from
And improve mechanical property.Cellulose is transformed into by material with carbon element by calcining, is made overall with more empty, the big carbon materials of specific surface area
Material, it is extremely suitable to make capacitor.
One kind of test 2, this test synthetic cellulose and graphene oxide and carbon nanometer pipe ternary under ionic liquid are answered
Closing the method for film is carried out according to the following steps:
First, 2g celluloses are added in the 1- butyl -3- methylimidazole villaumites of 50g, and stirring and dissolving 12h is to complete at 70 DEG C
CL, obtains cellulose solution;
2nd, by graphene oxide, CNT be added separately to be configured to concentration in DMF (DMF) be
The suspension and ultrasound of 50mg/ml makes it be uniformly dispersed, and obtains graphene oxide dispersion and carbon nano tube dispersion liquid;
3rd, the graphene oxide dispersion and carbon nano tube dispersion liquid for obtaining step 2 is added to the fibre that step one is obtained
In the plain solution of dimension, stirring reaction 12h at 80 DEG C obtains mixed solution;Wherein, the mass ratio of graphene oxide and CNT
For 1:1, the ratio of the quality sum and cellulose quality of graphene oxide and CNT is 1:5;
4th, the mixed solution obtained by step 3 is added to into cyclic washing 3 times in distilled water, then carries out filtration under diminished pressure,
Wet film is obtained, then wet film is put in vacuum drying oven, under vacuum drying at room temperature obtains cellulose/oxidation stone to constant weight
Black alkene/carbon nanometer pipe ternary composite membrane.
Fig. 8 is the Fourier transform infrared spectroscopy of material in this test, and wherein a is cellulose fourier-transform infrared light
Spectrum, the Fourier transform infrared spectroscopy of b graphene oxides, c is cellulose and CNT and graphite oxide prepared by this test
The Fourier transform infrared spectroscopy figure of alkene composite membrane.Relatively understand, with the addition of graphene oxide and CNT, cellulose
Absorption peak strength be greatly reduced.
One kind of test 3, this test synthetic cellulose and graphene oxide and carbon nanometer pipe ternary under ionic liquid are answered
Closing the method for film is carried out according to the following steps:
First, weigh 0.5g celluloses to be added in the 1- butyl -3- methylimidazole villaumites of 20g, the stirring and dissolving at 80 DEG C
12h obtains cellulose solution to being completely dissolved;
2nd, by graphene oxide, CNT be added separately to be configured to concentration in DMF (DMF) be
The suspension and ultrasound of 20mg/ml makes it be uniformly dispersed, and obtains graphene oxide dispersion and carbon nano tube dispersion liquid;
3rd, the graphene oxide dispersion and carbon nano tube dispersion liquid for obtaining step 2 is added to the fibre that step one is obtained
In the plain solution of dimension, stirring reaction 12h at 80 DEG C obtains mixed solution;Wherein, the mass ratio of graphene oxide and CNT
For 1:1, the ratio of the quality sum and cellulose quality of graphene oxide and CNT is 1:5;
4th, the mixed solution obtained by step 3 is added to into cyclic washing 3 times in distilled water, then carries out filtration under diminished pressure,
Wet film is obtained, then wet film is put in vacuum drying oven, under vacuum drying at room temperature obtains cellulose/oxidation stone to constant weight
Black alkene/carbon nanometer pipe ternary composite membrane.
The scanning electron microscope (SEM) of cellulose/graphene oxide/carbon nanometer pipe ternary composite membrane that this test is obtained
Plane graph it is as shown in Figure 9.From fig. 9, it can be seen that in material Graphene lamellar structure, and be by CNT in lamella
Support, what Graphene was covered, there is cellulose to link together.Stereochemical structure is obvious.
The scanning electron microscope (SEM) of cellulose/graphene oxide/carbon nanometer pipe ternary composite membrane that this test is obtained
Sectional view it is as shown in Figure 10.As can be seen from Figure 10 material is formed by accumulation from level to level, is clear that in section
The structure that CNT is interweaved, Graphene is covered in its surface, is connected together by cellulose, forms layered laminate.
Claims (4)
1. a kind of method of synthetic cellulose under ionic liquid and graphene oxide and carbon nanometer pipe ternary composite membrane, its feature
It is that the method is carried out according to the following steps:
First, the cellulose for weighing 1~15 part of parts by weight is added in the ionic liquid of 100 parts of parts by weight, at 60~100 DEG C
4~12h of stirring, obtains cellulose solution;
2nd, graphene oxide and CNT are separately added in solvent, are uniformly dispersed, obtain graphene oxide dispersion and carbon
Nanotube dispersion liquid;
3rd, the graphene oxide dispersion and carbon nano tube dispersion liquid for obtaining step 2 is added to the cellulose that step one is obtained
In solution, 8~24h of stirring reaction, obtains mixed solution at 70~100 DEG C;
4th, the mixed solution obtained by step 3 is added to into cyclic washing in distilled water, then carries out filtration under diminished pressure, obtain wet
Film, then wet film is put in vacuum drying oven, under vacuum drying at room temperature is to constant weight, obtain cellulose/graphene oxide/
Carbon nanometer pipe ternary composite membrane;
Cellulose wherein described in step one is chemical cellulose;CNT described in step 2 is surface treated
CNT, the process of surface treatment is:By the concentrated sulphuric acid that the concentrated nitric acid that mass concentration is 70% and mass concentration are 98%
Volume ratio is 1:3, concentrated nitric acid is mixed homogeneously with concentrated sulphuric acid, nitration mixture is obtained, CNT is dispersed in nitration mixture, be in temperature
Flow back 2h under conditions of 70 DEG C, then clean with deionized water with dilute hydrochloric acid successively, then is vacuum dried, and completes the table of CNT
Face is processed;Solvent described in step 2 is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide or dimethyl sulfoxide.
2. one kind according to claim 1 synthetic cellulose and graphene oxide and carbon nanometer pipe ternary under ionic liquid
The method of composite membrane, it is characterised in that step one intermediate ion liquid is 1- butyl -3- methylimidazole villaumites.
3. one kind according to claim 1 synthetic cellulose and graphene oxide and carbon nanometer pipe ternary under ionic liquid
The method of composite membrane, it is characterised in that stir 8h at 80 DEG C in step one.
4. one kind according to claim 1 synthetic cellulose and graphene oxide and carbon nanometer pipe ternary under ionic liquid
The method of composite membrane, it is characterised in that the ratio of the quality of the gross mass of graphene oxide and CNT and cellulose in step 3
For (0.5~10):100, the mass ratio of graphene oxide and CNT is (0.1~10):1.
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