CN108654579A - A kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel - Google Patents
A kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel Download PDFInfo
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- CN108654579A CN108654579A CN201810474138.3A CN201810474138A CN108654579A CN 108654579 A CN108654579 A CN 108654579A CN 201810474138 A CN201810474138 A CN 201810474138A CN 108654579 A CN108654579 A CN 108654579A
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Abstract
The present invention relates to a kind of preparation methods of sodium alginate/cattail/graphene oxide composite aerogel, belong to biomass-based functional material preparing technical field；Specific steps：Sodium alginate powder and cattail fiber are mixed and are added in graphene oxide dispersion, stirring obtains uniform mixed solution；It is freeze-dried by the method for two-way freezing casting, obtains uncrosslinked composite aerogel, immersed and contain CaCl2Ethanol/water mixed solution in, carry out secondary freeze drying, obtain sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking.The present invention using be simple and efficient, economic and environment-friendly synthetic method, obtained three-dimensional parallel sheet structure is connected with each other by honeycomb hole between parallel sheet, has excellent underwater superoleophobic property；And after the composite aerogel and filtering apparatus assembling, the insoluble oil of removal and water-soluble dyestuff can be synchronized, there are good application value and extensive market prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of sodium alginate/cattail/graphene oxide composite aerogel, belong to biomass
Base functional material preparing technical field.
Background technology
Due to a large amount of discharges of the water-soluble organic pollutants such as the oily wastewater increased year by year and dyestuff, a variety of organic contaminations
Object coexists in waste water, how to synchronize and removes the organic pollution in these water and already become the coke paid close attention in world wide
Point.No matter the removal of oil water mixture separation and water-soluble organic pollutant rapidly and efficiently is protected the improvement of ecological environment
Shield, or be all of great practical significance for recycling for regenerated resources.However, traditional organic pollution is gone
Except method, for example pass through burning, mechanical treatment, addition dispersant, biological treatment etc..Some removal efficiency are not high, some by
Secondary pollution is easily caused in addition chemical agent, energy consumption also is excessively high, somewhat expensive.Therefore carry out synchronizing for novel green
The material of removal organic polluter, the research of methods and techniques have become the hot spot in field of functional materials.
Aeroge is a kind of solid material of high porosity, has lower density and three-dimensional net structure, therefore can be with
Good selection as high efficiency oil-water separation.Biogas gel is because having renewable, inexpensive, environmental-friendly, more active sites
Point is easy many merits such as modified, and is widely used in water-oil separating field.However, to apply this biogas on a large scale
Gel, it is still necessary to overcome the problems, such as that its mechanical strength is relatively low.Many scholars are successfully prepared out the life for capableing of water-oil separating
Substance aeroge, but there is no biogas gel mechanical poor performance is considered, in order to improve biogas gel
The low problem of mechanical strength, effective method, which has, is added reinforced phase, chemical crosslinking, the method etc. for changing freezing casting.Although
These methods improve the mechanical performance of biogas gel, but how effectively to be combined these methods so that prepare
It is still current problem to be solved that biogas gel, which has super-elasticity,.
Invention content
Above-mentioned in order to solve the problems, such as, the object of the present invention is to provide a kind of sodium alginate/cattail/graphene oxides
The preparation method of composite aerogel.The present invention is using sodium alginate as " skeleton ", using graphene oxide and cattail fiber as increasing
Strong filler introduces the inside of sodium alginate three-dimensional net structure, by two-way freezing casting method, changes aeroge network lamella row
The mode of row, later by being simply freeze-dried, it is multiple to construct a kind of sodium alginate/cattail/graphene oxide for ionomer
Aeroge is closed, Some Organic Pollutants in water removal can be synchronized.
Present invention firstly provides a kind of sodium alginate/cattail/graphene oxide composite aerogel, the composite aerogel be by
Three kinds of sodium alginate, cattail, graphene oxide Material claddings are prepared；The internal structure of gained composite aerogel is parallel layers
Shape structure is sandwiched between honeycomb porous structure.
The present invention also provides a kind of preparation methods of sodium alginate/cattail/graphene oxide composite aerogel, and step is such as
Under：
(1) sodium alginate/cattail/graphene oxide mixed solution is prepared：
A, graphene oxide dispersion is prepared；
B, cattail fiber is prepared：First, deionized water is added in sodium chlorite, stirs, obtains sodium chlorite solution, carried out
PH is adjusted；Cattail flower spike is then added, stirring, it is 6 to be cleaned to pH with deionized water, then washes repeatedly three with absolute ethyl alcohol
It is secondary, it is dry, finally obtain dry cattail fiber；
C, sodium alginate/cattail/graphene oxide mixed solution is prepared：Sodium alginate powder and cattail fiber are added to
It in graphene oxide dispersion, stirs, is ultrasonically treated, obtain mosanom/cattail/graphene oxide homogeneous mixture solotion；
(2) preparation of uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel：The sea that step (1) is obtained
Mosanom/cattail/graphene oxide mixed solution pours into silica gel mould of the bottom with chock, mold exterior cladding heat preservation glue
Band prevents temperature from mutually conducting；Two-way freezing is carried out at the top of the copper rod that the bottom contact of silica gel mould is persistently cooled down by liquid nitrogen
Casting, when solution is frozen into ice cube, is freeze-dried, it is compound to obtain uncrosslinked sodium alginate/cattail/graphene oxide
Aeroge；
(3) preparation of sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking：Step (2) is obtained
Uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel immerse calcium chloride ethanol/water mixed solution in, instead
Ying Hou carries out cleaning aeroge repeatedly with absolute ethyl alcohol, then carries out secondary freeze drying, obtain the seaweed of calcium ion crosslinking
Sour sodium/cattail/graphene oxide composite aerogel.
Preferably, sodium chlorite described in the B of step (1) and the amount ratio of deionized water are 4g：400mL；The pH
It is 4.5 that adjusting, which is with second acid for adjusting pH,.
Preferably, the mass ratio of cattail flower spike and sodium chlorite described in the B of step (1) is 1:1.
Preferably, the stirring described in the B of step (1) is to be stirred 2 hours under the conditions of 1000rpm and 80 DEG C；It is described dry
Dry temperature is 60 DEG C.
Preferably, the mass ratio of sodium alginate powder described in the C of step (1) and cattail fiber is 1:9~9:1；It is described
The dosage of graphene oxide accounts for 1wt%~10wt% of sodium alginate powder and cattail fiber total amount.
Preferably, the angle of the bottom chock described in step (2) is 10 °~15 °.
Preferably, step (2) and step (3) the freeze-drying condition are -40 DEG C of temperature, absolute pressure 20pa, time
48h。
Preferably, anti-described in a concentration of 2wt%-4wt% of ethanol/water mixed solution of the calcium chloride described in step (3)
It is 8-12h between seasonable.
Sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention is applied to water-oil separating and water solubility
The Adsorption of dyestuff.
A kind of performance test of sodium alginate/cattail/graphene oxide composite aerogel of the present invention, method are as follows：
(1) measuring mechanical property
The mechanical performance of aeroge is tested with digital display type Tension-pressure tester.I.e. under 40%, 60% and 80% strain,
The stress variation for testing the underwater superoleophobic sodium alginate/cattail/graphene oxide composite aerogel of this super-elasticity, 80%
Strained condition under, repeatedly recycle the variation of compression verification its stress.
(2) air Zhong Shui and oil can be surveyed in sodium alginate/cattail/graphene oxide composite aerogel wettability of the surface
Examination：
Air Zhong Shui and oil are in sodium alginate/cattail/graphene oxide composite aerogel wettability of the surface energy；Acid-alkali salt
In, oil is in sodium alginate/cattail/graphene oxide composite aerogel wettability of the surface energy；Using Drop Shape Analysis System
It is assessed by contact angle test.
(3) synchronous removal insoluble oil and water-soluble dye test
Between sodium alginate/cattail/graphene oxide composite aerogel is clipped in filter device, different oil and dyestuff are tested
Separative efficiency after hybrid filtering.Wherein, test oil product includes toluene, rapeseed oil, hexane, pump oil, silicone oil, hexadecane；Dyestuff
Including methylene blue, gentian violet, rhodamine B.
(4) circulation absorption desorption test
Between sodium alginate/cattail/graphene oxide composite aerogel is clipped in filter device, methylene blue solution is adsorbed
After (10ppm), it is desorbed with the hydrochloric acid of 0.5M.Loop test 100 times obtains it and adsorbs the variation of methylene blue amount.
Advantageous effect：
(1) present invention obtains a kind of sodium alginate/cattail/oxidation that can synchronize removal insoluble oil and water-soluble dye
Graphene composite aerogel, the preparation process being related to is simple, raw material it is of low cost, obtained compound aeroge is environment
It is friendly, pollution-free.
(2) sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention has excellent mechanical performance,
Outstanding affinity and high-specific surface area；Meanwhile graphene oxide and cattail fiber are added into sodium alginate base as reinforcing filler
In body, the load that sodium alginate matrix is born can be effectively shifted, the more excellent three-dimensional network of mechanical performance can be built
Structure.
(3) sodium alginate/cattail/graphene oxide composite aerogel that the present invention obtains, the aeroge have three-dimensional flat
Row laminated structure, there are cellular porous interconnections between piece and piece, show superior mechanical performance, by repeatedly compressing
Circulation experiment, it is basic that elastic loss does not occur, can effectively it restore to the original-shape of the compound aeroge, 80%
Strained condition under, after 100 second compressions, can still restore to the 86% of its original-shape, compressive strength maintains original
The 81% of beginning intensity.
(4) a kind of sodium alginate/cattail/graphene oxide composite aerogel that the present invention obtains shows underwater superoleophobic
Property, it is up to 171.74 ° with the contact angle of oil；Under conditions of acid-alkali salt, contact angle is still up to 150 °.
(5) it is insoluble can to synchronize removal for a kind of sodium alginate/cattail/graphene oxide composite aerogel that the present invention obtains
Property oil and solubility dyestuff；The removal efficiency of oil is up to 99.59%, and the removal efficiency of dyestuff is up to 99.05%.
(6) a kind of sodium alginate/cattail/graphene oxide composite aerogel that the present invention obtains can be desorbed with circulation absorption
Water soluble contaminants, by 100 circulation absorption detachment assays, adsorbance can still maintain original adsorbance
86.88%.And in shape without any significant change.
Description of the drawings
Fig. 1 is that embodiment 4 prepares a kind of sodium alginate/cattail/graphene oxide composite aerogel pictorial diagram.
Fig. 2 is that embodiment 4 prepares a kind of microscopic appearance figure of sodium alginate/cattail/graphene oxide composite aerogel,
Middle a is low range structure chart, and b is high magnification structure chart.
Fig. 3 is sodium alginate/cattail/graphene oxide composite aerogel prepared by embodiment 4 in differently strained condition
Under (40%, 60%, 80%) recycle compressed stress strain diagram a, under 80% strained condition by repeatedly compressed
Stress strain diagram b, by 100 times compressed plastic deformation rate c and intensity recovery rate d are recycled under 80% strained condition.
Fig. 4 is that sodium alginate/cattail/graphene oxide composite aerogel surface oil prepared by embodiment 4 drips in water
Photo a, wetting behavior schematic diagram b-d, the contact angle e of underwater different oil droplets, n-hexane are in NaCl (10wt%), HCl (1mol/
L) and in NaOH (1mol/L) with sodium alginate/cattail/graphene oxide composite aerogel contact angle figure f.
Fig. 5 is that sodium alginate/cattail/graphene oxide composite aerogel prepared by embodiment 4 is clipped between filter device
Synchronous removal insoluble oil and water-soluble dye.
Fig. 6 be embodiment 4 prepare aeroge oil and dyestuff mixing condition under to different oil a and different dyes b
Removal efficiency and flux；By 100 cycle desorption absorption, to the variation c of the adsorbance of dyestuff.
Fig. 7 is that sodium alginate/cattail/graphene oxide composite aerogel prepared by embodiment 4 is desorbed by 100 cycles
The variation of shape after absorption.
Specific implementation mode
In order to fully disclose a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel of the invention,
With reference to embodiment, the present invention is described in further detail.
Embodiment 1：
(1) sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：
A, graphene oxide dispersion is prepared：Graphene oxide powder is add to deionized water, 2h is ultrasonically treated, makes
It obtains graphene oxide powder to be uniformly dispersed in deionized water, obtains uniform graphene oxide dispersion；
B, cattail fiber is prepared：First, 50 grams of cattail flower spikes are cleaned successively with 1L water and 1L ethyl alcohol, equipped with mechanical agitation
Sodium chlorite 4g and deionized water 400mL is added in the flask of device and thermometer, stirring is allowed to fully dissolve, with 1.2ml acetic acid
Adjust the pH to 4.5 of sodium chlorite solution.Then be added 4g cattail flower spikes, stirred 2 hours at 1000rpm and 80 DEG C, spend from
Sub- water is cleaned to pH=6, is then washed three times with absolute ethyl alcohol, and residual water, and drying in 60 DEG C of baking oven by it are removed.Most
Dry cattail fiber is obtained afterwards.
C, sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：Sodium alginate powder and cattail fiber are added
Enter into graphene oxide dispersion, magnetic agitation 3h, is allowed to be sufficiently mixed uniformly, by being ultrasonically treated, bubble removing is gone to obtain
Mosanom/cattail/graphene oxide homogeneous mixture solotion.Wherein, the mass ratio of sodium alginate powder and cattail fiber is 1:9,
The quality of graphene oxide is the 1wt% of sodium alginate powder and cattail fiber quality summation.
(2) preparation of uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel：Step (1) is obtained equal
Even mixed solution pours into silica gel mould of the bottom with chock, mold exterior is coated one layer of heat preservation adhesive tape, to play
The angle of insulation, the effect for preventing temperature from mutually conducting, bottom chock is 10 °, and liquid is passed through in the bottom contact of silica gel mould
Two-way freezing casting is carried out at the top of the copper rod that nitrogen persistently cools down, and when solution is frozen into ice cube, is put into lyophilization system progress
Freeze-drying, will obtain uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel.
(3) preparation of sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking：Step (2) is obtained
Uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel immerse a concentration of 2wt% calcium chloride ethanol/water
(v:V=8:2) in mixed solution, after reacting 8h, cleaning aeroge repeatedly is carried out with a large amount of absolute ethyl alcohol, then carries out two
Secondary freeze-drying obtains sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking.It will be this multiple with cutter
The size that aeroge is cut into 20 × 15 × 40mm is closed, for carrying out the follow-up performance test of this composite aerogel.Use cutter
This composite aerogel is cut into diameter 25mm, the size of thickness 10mm, for carrying out this composite aerogel later separation
It can test.
Embodiment 2：
(1) sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：
A, graphene oxide dispersion is prepared：Graphene oxide powder is add to deionized water, 2h is ultrasonically treated, makes
It obtains graphene oxide powder to be uniformly dispersed in deionized water, obtains uniform graphene oxide dispersion；
B, cattail fiber is prepared：First, 50 grams of cattail flower spikes are cleaned successively with 1L water and 1L ethyl alcohol, equipped with mechanical agitation
Sodium chlorite 4g and deionized water 400mL is added in the flask of device and thermometer, stirring is allowed to fully dissolve, with 1.2ml acetic acid
Adjust the pH to 4.5 of sodium chlorite solution.Then be added 4g cattail flower spikes, stirred 2 hours at 1000rpm and 80 DEG C, spend from
Sub- water is cleaned to pH=6, is then washed three times with absolute ethyl alcohol, and residual water, and drying in 60 DEG C of baking oven by it are removed.Most
Dry cattail fiber is obtained afterwards.
C, sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：Sodium alginate powder and cattail fiber are added
Enter into graphene oxide dispersion, magnetic agitation 3h, is allowed to be sufficiently mixed uniformly, by being ultrasonically treated, bubble removing is gone to obtain
Mosanom/cattail/graphene oxide homogeneous mixture solotion.Wherein, the mass ratio of sodium alginate powder and cattail fiber is 3:7,
The quality of graphene oxide is the 5wt% of sodium alginate powder and cattail fiber quality summation.
(2) preparation of uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel：Step (1) is obtained equal
Even mixed solution pours into silica gel mould of the bottom with chock, mold exterior is coated one layer of heat preservation adhesive tape, to play
The angle of insulation, the effect for preventing temperature from mutually conducting, bottom chock is 15 °, and liquid is passed through in the bottom contact of silica gel mould
Two-way freezing casting is carried out at the top of the copper rod that nitrogen persistently cools down, and when solution is frozen into ice cube, is put into lyophilization system progress
Freeze-drying, will obtain uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel.
(3) preparation of sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking：Step (2) is obtained
Uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel immerse a concentration of 4wt% calcium chloride ethanol/water
(v:V=8:2) in mixed solution, after reacting 10h, cleaning aeroge repeatedly is carried out with a large amount of absolute ethyl alcohol, is then carried out
Secondary freeze drying obtains sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking.It will be this with cutter
Composite aerogel is cut into the size of 20 × 15 × 40mm, for carrying out the follow-up performance test of this composite aerogel.Use knife
This composite aerogel is cut into diameter 25mm, the size of thickness 10mm, for carrying out this composite aerogel later separation by tool
Performance test.
Embodiment 3：
(1) sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：
A, graphene oxide dispersion is prepared：Graphene oxide powder is add to deionized water, 3h is ultrasonically treated, makes
It obtains graphene oxide powder to be uniformly dispersed in deionized water, obtains uniform graphene oxide dispersion；
B, cattail fiber is prepared：First, 50 grams of cattail flower spikes are cleaned successively with 1L water and 1L ethyl alcohol, equipped with mechanical agitation
Sodium chlorite 4g and deionized water 400mL is added in the flask of device and thermometer, stirring is allowed to fully dissolve, with 1.2ml acetic acid
Adjust the pH to 4.5 of sodium chlorite solution.Then be added 4g cattail flower spikes, stirred 2 hours at 1000rpm and 80 DEG C, spend from
Sub- water is cleaned to pH=6, is then washed three times with absolute ethyl alcohol, and residual water, and drying in 60 DEG C of baking oven by it are removed.Most
Dry cattail fiber is obtained afterwards.
C, sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：Sodium alginate powder and cattail fiber are added
Enter into graphene oxide dispersion, magnetic agitation 3h, is allowed to be sufficiently mixed uniformly, by being ultrasonically treated, bubble removing is gone to obtain
Mosanom/cattail/graphene oxide homogeneous mixture solotion.Wherein, the mass ratio of sodium alginate powder and cattail fiber is 7:3,
The quality of graphene oxide is the 10wt% of sodium alginate powder and cattail fiber quality summation.
(2) preparation of uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel：Step (1) is obtained equal
Even mixed solution pours into silica gel mould of the bottom with chock, mold exterior is coated one layer of heat preservation adhesive tape, to play
The angle of insulation, the effect for preventing temperature from mutually conducting, bottom chock is 10 °, and liquid is passed through in the bottom contact of silica gel mould
Two-way freezing casting is carried out at the top of the copper rod that nitrogen persistently cools down, and when solution is frozen into ice cube, is put into lyophilization system progress
Freeze-drying, will obtain uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel.
(3) preparation of sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking：Step (2) is obtained
Uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel immerse a concentration of 2wt% calcium chloride ethanol/water
(v:V=8:2) in mixed solution, after reacting 12h, cleaning aeroge repeatedly is carried out with a large amount of absolute ethyl alcohol, is then carried out
Secondary freeze drying obtains sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking.It will be this with cutter
Composite aerogel is cut into the size of 20 × 15 × 40mm, for carrying out the follow-up performance test of this composite aerogel.Use knife
This composite aerogel is cut into the size of diameter 25mm thickness 10mm by tool, for carrying out this composite aerogel later separation
It can test.
Embodiment 4：
(1) sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：
A, graphene oxide dispersion is prepared：Graphene oxide powder is add to deionized water, 2h is ultrasonically treated, makes
It obtains graphene oxide powder to be uniformly dispersed in deionized water, obtains uniform graphene oxide dispersion；
B, cattail fiber is prepared：First, 50 grams of cattail flower spikes are cleaned successively with 1L water and 1L ethyl alcohol, equipped with mechanical agitation
Sodium chlorite 4g and deionized water 400mL is added in the flask of device and thermometer, stirring is allowed to fully dissolve, with 1.2ml acetic acid
Adjust the pH to 4.5 of sodium chlorite solution.Then be added 4g cattail flower spikes, stirred 2 hours at 1000rpm and 80 DEG C, spend from
Sub- water is cleaned to pH=6, is then washed three times with absolute ethyl alcohol, and residual water, and drying in 60 DEG C of baking oven by it are removed.Most
Dry cattail fiber is obtained afterwards.
C, sodium alginate/cattail/graphene oxide homogeneous mixture solotion is prepared：Sodium alginate powder and cattail fiber are added
Enter into graphene oxide dispersion, magnetic agitation 3h, is allowed to be sufficiently mixed uniformly, by being ultrasonically treated, bubble removing is gone to obtain
Mosanom/cattail/graphene oxide homogeneous mixture solotion.Wherein, the mass ratio of sodium alginate powder and cattail fiber is 9:1,
The quality of graphene oxide is the 5wt% of sodium alginate powder and cattail fiber quality summation.
(2) preparation of uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel：Step (1) is obtained equal
Even mixed solution pours into silica gel mould of the bottom with chock, mold exterior is coated one layer of heat preservation adhesive tape, to play
The angle of insulation, the effect for preventing temperature from mutually conducting, bottom chock is 15 °, and liquid is passed through in the bottom contact of silica gel mould
Two-way freezing casting is carried out at the top of the copper rod that nitrogen persistently cools down, and when solution is frozen into ice cube, is put into lyophilization system progress
Freeze-drying, will obtain uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel.
(3) preparation of sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking：Step (2) is obtained
Uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel immerse a concentration of 2wt% calcium chloride ethanol/water
(v:V=8:2) in mixed solution, after reacting 10h, cleaning aeroge repeatedly is carried out with a large amount of absolute ethyl alcohol, is then carried out
Secondary freeze drying obtains sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking.It will be this with cutter
Composite aerogel is cut into the size of 20 × 15 × 40mm, for carrying out the follow-up performance test of this composite aerogel.Use knife
This composite aerogel is cut into diameter 25mm, thickness 10mm by tool, is surveyed for carrying out this composite aerogel later separation performance
Examination.
As shown in Figure 1, sodium alginate/cattail/graphene oxide composite aerogel surface prepared by the present invention is from macroscopically
Observation is still that parallel laminar structure is sandwiched between honeycomb porous structure.
As shown in Fig. 2, its inside of sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention has three
Parallel laminar structure is tieed up, there is cellular porous interconnection (Fig. 2 a) between layers；Image such as Fig. 2 b institutes are further amplified
Show, cattail fiber is embedded in lamellar structure, and towards different directions, sodium alginate and graphene oxide along cattail fiber
Growth, and then the porous structure of honeycomb is obtained in parallel laminar structure.
As shown in figure 3, sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention is by differently strained
Under the conditions of compression (Fig. 3 a) show superior mechanical performance.By the first second compression, maximum pressure improves up to 130kPa
The problem of biogas gel mechanical poor performance；(Fig. 3 b-d) is basic that elasticity does not occur by repeatedly compression circulation experiment
Loss, can effectively restore to the original-shape of the compound aeroge.Under 80% strained condition, pressed by 100 times
After contracting, can still it restore to the 86% of its original-shape, compressive strength maintains the 81% of green strength.
As shown in figure 4, sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention swims in the water surface,
In water, oil droplet is (Fig. 4 a, Fig. 4 d) spherical in shape on aeroge surface, shows underwater superoleophobic property；And in air, the aeroge
Surface be hydrophilic and oleophilic (Fig. 4 b, 4c)；(Fig. 4 e) test in water different oil droplets composite aerogel surface contact angle,
It was found that the contact angle with kerosene is up to 171.74 °；(Fig. 4 f) under conditions of acid-alkali salt, contact angle is still up to 150 °.
As shown in figure 5, sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention is clipped in filter device
Between synchronous removal insoluble oil and water-soluble dye；The removal efficiency of oil is up to 99.59% (Fig. 6 a), the removal efficiency of dyestuff
Up to 99.05% (Fig. 6 b).
Sodium alginate/cattail/graphene oxide composite aerogel prepared by the present invention can be desorbed water-soluble with circulation absorption
Pollutant, by 100 circulation absorption detachment assays, adsorbance can still maintain 86.88% (figure of original adsorbance
6c).And in shape without any significant change, remain to maintain original shape (Fig. 7) well.
Claims (10)
1. a kind of sodium alginate/cattail/graphene oxide composite aerogel, which is characterized in that the composite aerogel is by sea
Three kinds of mosanom, cattail and graphene oxide Material claddings are prepared；The internal structure of the composite aerogel is parallel layers
Shape structure is sandwiched between honeycomb porous structure.
2. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel, which is characterized in that including walking as follows
Suddenly：
（1）Prepare sodium alginate/cattail/graphene oxide mixed solution：
A. graphene oxide dispersion is prepared；
B. cattail fiber is prepared：First, deionized water is added in sodium chlorite, stirred, obtain sodium chlorite solution, carry out pH
It adjusts；Cattail flower spike is then added, stirring, it is 6 to be cleaned to pH with deionized water, then three times with absolute ethyl alcohol repeated washing,
It is dry, finally obtain dry cattail fiber；
C. sodium alginate/cattail/graphene oxide mixed solution is prepared：Sodium alginate powder and cattail fiber are added to oxygen
It in graphite alkene dispersion liquid, stirs, is ultrasonically treated, obtain mosanom/cattail/graphene oxide homogeneous mixture solotion；
（2）The preparation of uncrosslinked sodium alginate/cattail/graphene oxide composite aerogel：By step（1）Obtained alginic acid
Sodium/cattail/graphene oxide mixed solution pours into silica gel mould of the bottom with chock, mold exterior cladding heat preservation adhesive tape,
Prevent temperature from mutually conducting；Two-way freezing casting is carried out at the top of the copper rod that the bottom contact of silica gel mould is persistently cooled down by liquid nitrogen
It makes, when solution is frozen into ice cube, is freeze-dried, obtain uncrosslinked sodium alginate/compound gas of cattail/graphene oxide
Gel；
（3）The preparation of sodium alginate/cattail/graphene oxide composite aerogel of calcium ion crosslinking：By step（2）It obtains not
Crosslinked sodium alginate/cattail/graphene oxide composite aerogel immerses in the ethanol/water mixed solution of calcium chloride, after reaction,
Carry out cleaning aeroge repeatedly with absolute ethyl alcohol, then carry out secondary freeze drying, obtain the sodium alginate of calcium ion crosslinking/
Cattail/graphene oxide composite aerogel.
3. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel according to claim 2,
It is characterized in that, step（1）B described in sodium chlorite and the amount ratio of deionized water be 4g：400mL；The pH is adjusted
The use of second acid for adjusting pH is 4.5；The mass ratio of the cattail flower spike and sodium chlorite is 1:1.
4. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel according to claim 2,
It is characterized in that, step（1）B described in stirring be stirred 2 hours under the conditions of 1000 rpm and 80 DEG C；The temperature of the drying
Degree is 60 DEG C.
5. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel according to claim 2,
It is characterized in that, step（1）C described in the mass ratio of sodium alginate powder and cattail fiber be 1:9~9:1；The graphite oxide
The dosage of alkene accounts for 1wt% ~ 10wt % of sodium alginate powder and cattail fiber total amount.
6. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel according to claim 2,
It is characterized in that, step（2）The angle of the bottom chock is 10 ° ~ 15 °.
7. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel according to claim 2,
It is characterized in that, step（2）And step（3）The freeze-drying condition is -40 DEG C of temperature, absolute pressure 20pa, time 48h.
8. a kind of preparation method of sodium alginate/cattail/graphene oxide composite aerogel according to claim 2,
It is characterized in that, step（3）Reaction time described in a concentration of 2wt%-4wt% of ethanol/water mixed solution of the calcium chloride is
8-12h。
9. a kind of sodium alginate/cattail/graphene oxide composite aerogel described in claim 1 is applied to water-oil separating or water
The Adsorption of soluble dye.
10. application according to claim 9, which is characterized in that the water-soluble dye is gentian violet, methylene blue or sieve
Red bright B.
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| CN110697692A (en) * | 2019-09-27 | 2020-01-17 | 北京石墨烯技术研究院有限公司 | Graphene aerogel three-dimensional structure and preparation method thereof |
| CN112191234A (en) * | 2020-10-09 | 2021-01-08 | 厦门理工学院 | Sodium alginate adsorption stent and preparation method and application thereof |
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