CN109433166A - A kind of preparation method of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol tri compound aeroge adsorbent material - Google Patents
A kind of preparation method of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol tri compound aeroge adsorbent material Download PDFInfo
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Abstract
The invention discloses a kind of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol (GO/MWCNTs/PVA) tri compound aeroge adsorbent materials and preparation method thereof.GO/MWCNTs/PVA tri compound aeroge is made by circulating frozen-freezing process.The preparation method is environmentally protective, simple, low in cost without any toxic by-product generation, preparation process.Tri compound aeroge obtained has good adsorption capacity to aqueous solution Methylene Blue dyestuff, it may be implemented to be rapidly achieved adsorption equilibrium by adjusting the content of MWCNTs and the pH of solution in composite aerogel, there is important application value in the process field of industrial dye waste water.
Description
Technical field
The invention belongs to adsorption functional material technical fields, and in particular to a kind of graphene oxide/multi-walled carbon nanotube/poly-
The preparation method of vinyl alcohol tri compound aeroge adsorbent material.
Background technique
With the fast development of printing and dyeing industry, problem of environmental pollution caused by waste water from dyestuff is on the rise.However it is traditional
Adsorbent material usually has that adsorption rate is low, the high disadvantages such as low with cyclic utilization rate of processing cost, therefore develops environmentally friendly height
Performance Dye Adsorption material is increasingly becoming a research hotspot of materials science field.
Aeroge is a kind of three-dimensional crosslinked network structural material, with extremely low density, flourishing porosity and huge
Specific surface area, therefore it is a kind of potential adsorbent material.Graphene oxide (GO) is a kind of single layer sheet Two-dimensional Carbon nanometer material
Material, a large amount of oxygen-containing functional groups are contained on its surface and edge, therefore have good solution dispersion energy.Regulate and control GO aqueous dispersions
Lamella concentration, three-dimensional netted GO hydrogel can be obtained by solution self assembly.
Contain great amount of hydroxy group on polyvinyl alcohol (PVA) strand, there is good water solubility.Pass through circulating frozen-defrosting
Method can prepare the PVA hydrogel of physical crosslinking, which has many advantages, such as the high and low toxicity of water content and good biocompatibility.
Therefore, PVA is introduced in GO aqueous solution, is controlled concentration of component, can be obtained GO/PVA composite hydrogel.
Multi-walled carbon nanotube (MWCNTs) is a kind of one-dimensional carbon nano material, have unique tubular structure, big L/D ratio,
Low-density, excellent mechanical property.Therefore, MWCNTs is introduced into GO/PVA composite aerogel, its mechanics not only can be enhanced
Performance, and the Dye Adsorption performance of composite aerogel can be improved.
The present invention passes through ultrasound using amphiphilic (class surfactant) feature of graphene oxide (GO) in aqueous dispersions
Directly disperse original MWCNTs, obtain stable GO/MWCNTs dispersion liquid, PVA aqueous solution is then added and is uniformly mixed
Graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol (GO/MWCNTs/PVA) mixed liquor is obtained, by circulating frozen-defrosting
GO/MWCNTs/PVA tri compound hydrogel is obtained, further freeze-drying obtains GO/MWCNTs/PVA tri compound airsetting
Glue.Using the content and pH value of ultra-violet absorption spectrum research MWCNTs to the shadow of the Dye Adsorption performance of tri compound aeroge
It rings.As a result, it has been found that tri compound aeroge obtained has good adsorption capacity to aqueous solution Methylene Blue dyestuff, pass through
Adjusting the content of MWCNTs and the pH of solution in composite aerogel may be implemented to be rapidly achieved adsorption equilibrium, therefore the compound gas
Gel has important application value in the process field of industrial dye waste water.
Summary of the invention
The purpose of the present invention is to provide a kind of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol tri compound airsettings
Glue adsorbent material and preparation method thereof, the composite material not only have the spies such as density is low, adsorption rate is high, absorption property easy-regulating
Point, and its preparation process is simple, environmentally protective.
The invention is realized by the following technical scheme:
A kind of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol tri compound aeroge adsorbent material, the ternary
The three-dimensional friendship that composite aerogel adsorbent material is self-assembly of by two-dimensional sheet GO, one-dimensional tubulose MWCNTs and PVA strand etc.
Networking network structure composition.
A kind of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol tri compound aeroge adsorbent material, the ternary
The preparation method of composite aerogel adsorbent material, its step are as follows:
(1) 3 50mL beakers are taken, 10mL deionized water is separately added into, are then respectively adding 60mg graphite oxide, ultrasound
30min, graphene oxide (GO) aqueous dispersions that 1.5h obtains concentration as 6mg/mL are vigorously stirred, are then respectively adding 0,5 and
The multi-walled carbon nanotube (MWCNTs) of 10mg, ultrasonic 30min are evenly spread in GO dispersion liquid, obtain a series of differences
The GO/MWCNTs aqueous dispersions of MWCNTs concentration.
(2) precise 1g polyvinyl alcohol (PVA) is added in 99mL deionized water, and it is completely molten to be vigorously stirred 5h in 95 DEG C
Solution is cooled to room temperature to obtain the PVA aqueous solution that concentration is 1wt%.
(3) the PVA aqueous solution that the concentration that 10mL step (2) obtain is 1wt% is measured, the GO/ that step (1) obtains is added to
In MWCNTs aqueous dispersions, it is stirred at room temperature for 24 hours to uniformly mixed.
(4) reaction solution is transferred in the long glass tube of internal diameter 2cm, volume 30mL, preservative film sealing, in -18 DEG C of refrigerators
Middle freezing 20h, then thaw 4h at room temperature, recycles 3 times repeatedly, obtains GO/MWCNTs/PVA tri compound hydrogel.
Obtained hydrogel is completely soaked and is dialysed in deionized water, changes a water every 6h, altogether lasting 48h.
(5) hydrogel after dialysis is taken out with tweezers, after blotting paper blots the water of hydrogel surface, is put into refrigerator
Pre-freeze, then vacuum freeze drying 48h obtains GO/MWCNTs/PVA tri compound aeroge in freeze drier.It is fixed anti-
It is 5 mg/mL that the concentration for answering GO in system, which is the concentration of 3mg/mL, PVA, changes concentration (0mg/mL, the 0.25mg/mL of MWCNTs
And 0.5mg/mL).
Compared with prior art, advantageous effects of the invention embody in the following areas:
1, the present invention uses circulating frozen-freezing process, and GO/MWCNTs/PVA tri compound gas is made in conjunction with being freeze-dried
Gel, easy to operate, green safe, no any poisonous and harmful substance generates, it is not necessary that any surfactant is added.
2, original MWCNTs is directly dispersing in GO aqueous dispersions by the present invention using ultrasonic dispersion, so that enhancing is multiple
Close the mechanical property of aeroge；It is environmentally protective without carrying out concentrated acid acidification MWCNTs.
3, the absorption property of GO/MWCNTs/PVA tri compound aerogel material prepared by the present invention is good, has density
Low, the features such as adsorption rate is high, absorption property easy-regulating.By the content and solution that adjust MWCNTs in composite aerogel
PH, which may be implemented to adsorb methylene blue dye, is rapidly achieved balance.
Detailed description of the invention
Fig. 1 is Fourier transform infrared spectroscopy (FT-IR) spectrogram of product in embodiment 1,2,3；
Fig. 2 be in embodiment 1,2,3 absorbance of the product in pH=7 with the change curve of wavelength；
Fig. 3 be in embodiment 2 absorbance of the product S2 in pH=2 with the change curve of wavelength；
Fig. 4 is the absorption standard curve of aqueous solution of methylene blue；
Fig. 5 is the normalization concentration versus time curve of product in embodiment 1,2,3.
Specific implementation method
Now in conjunction with embodiment and attached drawing, the invention will be further described:
Embodiment 1
1,3 50mL beakers are taken, 10mL deionized water is separately added into, are then respectively adding 60mg graphite oxide, ultrasound
30min, graphene oxide (GO) aqueous dispersions that 1.5h obtains concentration as 6mg/mL are vigorously stirred.
2, precise 1g polyvinyl alcohol (PVA) is added in 99mL deionized water, and it is completely molten to be vigorously stirred 5h in 95 DEG C
Solution is cooled to room temperature to obtain the PVA aqueous solution that concentration is 1wt%.
3, the PVA aqueous solution that the concentration that 10mL step (2) obtain is 1wt% is measured, the GO that step (1) obtains is added to
In aqueous dispersions, it is stirred at room temperature for 24 hours to uniformly mixed.
4, reaction solution is transferred in the long glass tube of internal diameter 2cm, volume 30mL, preservative film sealing, in -18 DEG C of refrigerators
20h is freezed, then thaw 4h at room temperature, recycles 3 times repeatedly, obtains GO/PVA binary composite hydrogel.The water that will be obtained
Gel is completely soaked dialyses in deionized water, changes a water every 6h, altogether lasting 48h.
5, the hydrogel after dialysis is taken out with tweezers, after blotting paper blots the water of hydrogel surface, is put into refrigerator
Pre-freeze, then vacuum freeze drying 48h obtains GO/PVA binary composite aerogel in freeze drier, is labeled as S1.
The FT-IR spectrogram of 1 product of embodiment is shown in Fig. 1.The accurately MB aqueous solution of 100 μm of ol/L of configuration, then dilution obtains
A series of MB solution of various concentrations, and absorbance standard curve is drawn, see Fig. 4.Accurately configure pH=7's with deionized water
50 μM of 100mL of MB aqueous solution.The aeroge sample (S1) for taking 5mg to be lyophilized, puts into 50 μM of MB aqueous solution of above-mentioned configuration
In (volume 20mL), certain time is then vibrated at a slow speed in constant temperature oscillator；Separated in time takes MB solution, passes through purple
Outside-visible spectrophotometer measurement different moments MB solution absorbance, obtains absorbance with the change curve of wavelength, sees figure
2.By the MB solution standard curve control with drafting, the concentration versus time curve for obtaining MB solution is calculated.By solution
Concentration is plotted against time to obtain normalization concentration versus time curve, sees Fig. 5 divided by initial concentration (50 μM).Sample S1
In maximum characteristic absorption peak (wavelength 664nm) and pH=7, the minimum absorption values of MB aqueous solution are 0.082, corresponding
Equilibrium concentration be 0.232 μM.
Embodiment 2
1,3 50mL beakers are taken, 10mL deionized water is separately added into, are then respectively adding 60mg graphite oxide, ultrasound
30min, graphene oxide (GO) aqueous dispersions that 1.5h obtains concentration as 6mg/mL are vigorously stirred, the multi wall of 5mg is then added
Carbon nanotube (MWCNTs), ultrasonic 30min are evenly spread in GO dispersion liquid, obtain GO/MWCNTs aqueous dispersions.
2, precise 1g polyvinyl alcohol (PVA) is added in 99mL deionized water, and it is completely molten to be vigorously stirred 5h in 95 DEG C
Solution is cooled to room temperature to obtain the PVA aqueous solution that concentration is 1wt%.
3, the PVA aqueous solution that the concentration that 10mL step (2) obtain is 1wt% is measured, the GO/ that step (1) obtains is added to
In MWCNTs aqueous dispersions, it is stirred at room temperature for 24 hours to uniformly mixed.
4, reaction solution is transferred in the long glass tube of internal diameter 2cm, volume 30mL, preservative film sealing, in -18 DEG C of refrigerators
Middle freezing 20h, then thaw 4h at room temperature, recycles 3 times repeatedly, obtains GO/MWCNTs/PVA tri compound hydrogel.
Obtained hydrogel is completely soaked and is dialysed in deionized water, changes a water every 6h, altogether lasting 48h.
5, the hydrogel after dialysis is taken out with tweezers, after blotting paper blots the water of hydrogel surface, is put into refrigerator
Pre-freeze, then vacuum freeze drying 48h obtains GO/MWCNTs/PVA tri compound aeroge in freeze drier, is labeled as
S2。
The FT-IR spectrogram of 2 product of embodiment is shown in Fig. 1.The accurately MB aqueous solution of 100 μm of ol/L of configuration, then dilution obtains
A series of MB solution of various concentrations, and absorbance standard curve is drawn, see Fig. 4.Distinguished with deionized water and HCl standard solution
50 μM of 100mL of the MB aqueous solution of accurate configuration pH=7 and pH=2.2 parts of aeroge sample (S2) for taking 5mg to be lyophilized, investment
In 50 μM of MB aqueous solution (volume 20mL) of above-mentioned configuration, certain time is then vibrated at a slow speed in constant temperature oscillator；Between
MB solution is taken every certain time, the absorbance of different moments MB solution is measured by ultraviolet-visible spectrophotometer, is inhaled
Luminosity is shown in Fig. 2 and Fig. 3 with the change curve of wavelength.By the MB solution standard curve control with drafting, calculates and obtain MB solution
Concentration versus time curve.By solution concentration divided by initial concentration (50 μM), it is plotted against time to obtain normalization concentration
Versus time curve is shown in Fig. 5.Sample S2 is in maximum characteristic absorption peak (wavelength 664nm) and pH=7, MB aqueous solution
Minimum absorption values be 0.069, corresponding equilibrium concentration be 0.016 μM；When pH=2, the minimum absorbance of MB aqueous solution
Numerical value is 0.264, and corresponding equilibrium concentration is 3.252 μM.
Embodiment 3
1,3 50mL beakers are taken, 10mL deionized water is separately added into, are then respectively adding 60mg graphite oxide, ultrasound
30min, graphene oxide (GO) aqueous dispersions that 1.5h obtains concentration as 6mg/mL are vigorously stirred, the more of 10mg is then added
Wall carbon nano tube (MWCNTs), ultrasonic 30min are evenly spread in GO dispersion liquid, obtain GO/MWCNTs aqueous dispersions.
2, precise 1g polyvinyl alcohol (PVA) is added in 99mL deionized water, and it is completely molten to be vigorously stirred 5h in 95 DEG C
Solution is cooled to room temperature to obtain the PVA aqueous solution that concentration is 1wt%.
3, the PVA aqueous solution that the concentration that 10mL step (2) obtain is 1wt% is measured, the GO/ that step (1) obtains is added to
In MWCNTs aqueous dispersions, it is stirred at room temperature for 24 hours to uniformly mixed.
4, reaction solution is transferred in the long glass tube of internal diameter 2cm, volume 30mL, preservative film sealing, in -18 DEG C of refrigerators
Middle freezing 20h, then thaw 4h at room temperature, recycles 3 times repeatedly, obtains GO/MWCNTs/PVA tri compound hydrogel.
Obtained hydrogel is completely soaked and is dialysed in deionized water, changes a water every 6h, altogether lasting 48h.
5, the hydrogel after dialysis is taken out with tweezers, after blotting paper blots the water of hydrogel surface, is put into refrigerator
Pre-freeze, then vacuum freeze drying 48h obtains GO/MWCNTs/PVA tri compound aeroge in freeze drier, is labeled as
S3。
The FT-IR spectrogram of 3 product of embodiment is shown in Fig. 1.The accurately MB aqueous solution of 100 μm of ol/L of configuration, then dilution obtains
A series of MB solution of various concentrations, and absorbance standard curve is drawn, see Fig. 4.Accurately configure pH=7's with deionized water
50 μM of 100mL of MB aqueous solution.The aeroge sample (S1) for taking 5mg to be lyophilized, puts into 50 μM of MB aqueous solution of above-mentioned configuration
In (volume 20mL), certain time is then vibrated at a slow speed in constant temperature oscillator；Separated in time takes MB solution, passes through purple
Outside-visible spectrophotometer measurement different moments MB solution absorbance, obtains absorbance with the change curve of wavelength, sees figure
2.By the MB solution standard curve control with drafting, the concentration versus time curve for obtaining MB solution is calculated.By solution
Concentration is plotted against time to obtain normalization concentration versus time curve, sees Fig. 5 divided by initial concentration (50 μM).Sample S1
In maximum characteristic absorption peak (wavelength 664nm) and pH=7, the minimum absorption values of MB aqueous solution are 0.151, corresponding
Equilibrium concentration be 1.372 μM.
By the test result of above embodiments it is found that GO/ is made using simple circulating frozen-freezing process in the present invention
MWCNTs/PVA tri compound aeroge adsorbent material, this method is easy to operate, safe green, nonhazardous substance generate.It is compound
The Dye Adsorption of aeroge is functional, and product S2 is optimal to the absorption property of methylene blue in neutral conditions.Pass through adjusting
The content of MWCNTs and the pH of solution, which may be implemented to adsorb methylene blue dye, in composite aerogel is rapidly achieved balance,
Therefore GO/MWCNTs/PVA tri compound aeroge is a kind of ideal industrial dye waste water adsorbent material.
Claims (10)
1. a kind of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol (GO/MWCNTs/PVA) tri compound aeroge adsorption material
Material, it is characterised in that: the composite aerogel adsorbent material is by two-dimensional sheet GO, one-dimensional tubulose MWCNTs and PVA strand
Etc. the three-dimensional crosslinked network structure composition being self-assembly of.
2. GO/MWCNTs/PVA tri compound aeroge adsorbent material according to claim 1, it is characterised in that: described
Adsorbent material is prepared by the following method:
(1) 3 50mL beakers are taken, 10mL deionized water is separately added into, are then respectively adding 60mg graphite oxide, ultrasonic 30min,
It is vigorously stirred 1.5h and obtains graphene oxide (GO) aqueous dispersions that concentration is 6mg/mL, be then respectively adding 0,5 and 10mg's
Multi-walled carbon nanotube (MWCNTs), ultrasonic 30min are evenly spread in GO dispersion liquid, obtain a series of difference MWCNTs concentration
GO/MWCNTs aqueous dispersions.
(2) precise 1g polyvinyl alcohol (PVA) is added in 99mL deionized water, is vigorously stirred 5h in 95 DEG C and is completely dissolved,
It is cooled to room temperature to obtain the PVA aqueous solution that concentration is 1wt%.
(3) the PVA aqueous solution that the concentration that 10mL step (2) obtain is 1wt% is measured, the GO/ that step (1) obtains is added to
In MWCNTs aqueous dispersions, it is stirred at room temperature for 24 hours to uniformly mixed.
(4) reaction solution is transferred in the long glass tube of internal diameter 2cm, volume 30mL, preservative film sealing is cold in -18 DEG C of refrigerators
Freeze 20h, then thaw 4h at room temperature, recycles 3 times repeatedly, obtains GO/MWCNTs/PVA tri compound hydrogel.It will obtain
Hydrogel be completely soaked and dialyse in deionized water, change a water every 6h, altogether lasting 48h.
(5) hydrogel after dialysis is taken out with tweezers, after blotting paper blots the water of hydrogel surface, is put into refrigerator pre-
Freeze, then vacuum freeze drying 48h obtains GO/MWCNTs/PVA tri compound aeroge in freeze drier.Fixed reaction
It is 5mg/mL that the concentration of GO, which is the concentration of 3mg/mL, PVA, in system, change MWCNTs concentration (0mg/mL, 0.25mg/mL and
0.5mg/mL)。
3. preparation method according to claim 2, it is characterised in that: the ultrasonic time that the step (1) prepares GO is
30min.Ultrasonic time is too long to damage the structure snd size of GO lamella, cause GO that cannot effectively be self-assembly of three-dimensional
Network structure.
4. preparation method according to claim 2, it is characterised in that: what is be added in the step (1) is original
MWCNTs can be effectively retained the prototype structure and length of MWCNTs, enhance the mechanical property of composite aerogel；It is dense without carrying out
Sour acidification, it is environmentally protective.
5. preparation method according to claim 2, it is characterised in that: PVA is acute in 95 DEG C of hot water in the step (2)
Strong stirring 5h obtains the PVA aqueous solution that concentration is 1wt% to being completely dissolved.
6. preparation method according to claim 2, it is characterised in that: in the step (3), by isometric 1wt%'s
PVA aqueous solution is added in GO/MWCNTs aqueous dispersions, is then stirred at room temperature for 24 hours to being mixed thoroughly.
7. preparation method according to claim 2, it is characterised in that: in the step (4), reaction solution is sealed in long glass
In glass pipe, 3 circulating frozen-defrostings are carried out, obtain GO/MWCNTs/PVA tri compound hydrogel.Composite hydrogel dialysis
When, a water is changed every 6h, altogether lasting 48h, it is ensured that completely remove the impurity in reaction system.
8. preparation method according to claim 2, it is characterised in that: the drying of the step (5) is vacuum freeze drying,
Drying time is 48h.
9. preparation method according to claim 2, it is characterised in that: the additive amount of MWCNTs in control reaction system, from
And regulate and control the Nomenclature Composition and Structure of Complexes of composite aerogel, study its influence to the Dye Adsorption performance of composite aerogel；Meanwhile it burning
A certain amount of deionized water, graphite oxide, MWCNTs and PVA aqueous solution are sequentially added in cup, and each step must assure that addition
Substance be completely dispersed uniformly, eventually by circulating frozen-defrosting, GO/MWCNTs/PVA tri- is made in conjunction with vacuum freeze drying
First composite aerogel.
10. the preparation of graphene oxide/multi-walled carbon nanotube/polyvinyl alcohol tri compound aeroge adsorbent material be in strict accordance with
The claims are prepared.
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| CN111171340A (en) * | 2019-12-25 | 2020-05-19 | 浙江浙能技术研究院有限公司 | Photo-thermal evaporation material based on PVA hydrogel and preparation and application thereof |
| CN111321135A (en) * | 2020-03-11 | 2020-06-23 | 中国科学院长春应用化学研究所 | Integrated enzyme aerogel composite material, preparation method thereof and detection method of glucose content |
| CN113480781A (en) * | 2021-07-27 | 2021-10-08 | 东北林业大学 | Graphene/nanocellulose/polyvinyl alcohol ternary composite aerogel and preparation method thereof |
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| CN111321135B (en) * | 2020-03-11 | 2021-07-23 | 中国科学院长春应用化学研究所 | Integrated enzyme aerogel composite material, preparation method thereof and detection method of glucose content |
| CN113480781A (en) * | 2021-07-27 | 2021-10-08 | 东北林业大学 | Graphene/nanocellulose/polyvinyl alcohol ternary composite aerogel and preparation method thereof |
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