CN105254916A - Preparation method for oxidized graphene-poly-dopamine composite aerogel - Google Patents
Preparation method for oxidized graphene-poly-dopamine composite aerogel Download PDFInfo
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Abstract
The invention provides a preparation method for oxidized graphene-poly-dopamine composite aerogel. The preparation method comprises the following steps that 1, 0.15-0.7 g of dopamine powder is dissolved in 10-18 ml of distilled water, the dopamine aqueous solutions are mixed with 50-60 ml of oxidized graphene aqueous solutions with the concentration of 5-6 mg/ml, and stirring is performed to obtain oxidized graphene-dopamine mixed solutions; 2, 3-9 ml of tris aminomethane buffer solutions with the concentration of 0.1-0.12 mol/L are dropwise added into the mixed solutions while stirring is performed, stirring is continuously performed for 2-2.5 h, and standing is performed to enable the dopamine to be fully polymerized to obtain oxidized graphene-poly-dopamine composite aquogel; 3, after being placed in an environment with the temperature ranging from minus 20 DEG C to minus 10 DEG C to be frozen for 24-30 h, the composite aquogel is processed through freeze drying, and then the oxidized graphene-poly-dopamine composite aerogel is obtained. The method is simple in technology, and the prepared composite aerogel has the advantages of being high in porosity, excellent in adsorptivity, high in strength and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of graphene oxide/poly-Dopamine HCL composite aerogel, belong to aerogel preparing technical field.
Background technology
Present stage, industrial and scientific and technological development inevitably brings a series of environmental problem, and protection and the improvement of therefore environmental pollution have become one of very important problem of society.Wherein, the daily life of water pollution problems on us has impact the most direct and serious.The source of pollution mainly trade effluent of water pollution problems, wherein comprises a large amount of heavy metal ion, organic dye molecule and organic solvent etc., and these materials are once enter in human body and will bring out various diseases, and the healthy of people in serious threat.In the last few years, investigator conducted in-depth research for Water Pollution, has carried out processing and achieve certain effect by multiple method to water pollution problems, the advantage such as wherein absorption method is efficient with it, simple to operate, with low cost and extensively being approved.Absorption method mainly by the material with characterization of adsorption is placed in the pollutent that contaminated water body makes its adsorbed water body, thus reaches the object of purifying water body.The sorbent material that current absorption method adopts mainly concentrates on crystalline mineral, biomaterial, the Material Fields such as gac.But it is less to be subject to loading capacity, the impact that particularly loading capacity of heavy metal particle is less, further exploitation and the application of these materials are all affected.Therefore, a kind of novel absorption material with high-adsorption-capacity is sought extremely urgent.Aerogel refers to mutually to assemble with micro-nano granules and is formed nanoporous network structure, and in network hole, be full of the lightweight nano solid material of gaseous state dispersion medium, there is extra-low density, high-specific surface area, the feature of very high porosities and superelevation pore volume rate, be the ideal sorbing material of water treatment, in fields such as water treatments, there is important using value.
In the last few years, Graphene is widely used in the research of water pollution problems with the performance of himself excellence, its great specific surface area, heavy metal ion, organic dye etc. have high adsorption efficiency, simultaneously in water body, the study hotspot that feature becomes water treatment field such as can to stablize by holding structure again.The aerogel composite how prepared based on Graphene develops the hot issue of high planar water process sorbing material.The wherein dispersion of graphene sheet layer and stripping, the interaction of Graphene and matrix, firm in aerogel material of graphene three-dimensional structure is all gordian techniquies of the aerogel composite prepared based on Graphene with building.The surface energy that Graphene is higher makes it be easy to reunite in the process preparing sorbing material, and its surface exists without functional group, presents certain hydrophobicity, this greatly reduces its service efficiency; So present stage Graphene or the preparation of graphite oxide thiazolinyl aerogel usually need to introduce linking agent etc. and increase its structural stability, the introducing of linking agent then affects the adsorptive power of aerogel material of knowing clearly to a certain extent, reduce the service efficiency of material, virtually substantially increase the tooling cost of material; And if do not introduce linking agent, its structural stability is then difficult to ensure in organic solvent or water surrounding, thus cannot be applied to actual sewage treatment area.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of graphene oxide/poly-Dopamine HCL composite aerogel.The method environmental friendliness, technique is simple and be beneficial to scale operation; The graphene oxide prepared/poly-Dopamine HCL composite aerogel has complete gel network structure, porosity is high, adsorptivity is excellent, intensity advantages of higher.
The present invention realizes the technical scheme that its goal of the invention takes: the preparation method of a kind of graphene oxide/poly-Dopamine HCL composite aerogel, and its step is as follows:
A, being dissolved in 10-18ml distilled water by 0.15-0.7g Dopamine HCL powder, is at room temperature that the graphene oxide water solution of 5-6mg/ml mixes with 50-60ml concentration, stirs 30-40min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 3-9mL concentration is the Tutofusin tris of 0.1-0.12mol/L while stirring, continue after being added dropwise to complete to stir 2-2.5h; Then leave standstill, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, B walked the graphene oxide/poly-Dopamine HCL matrix material hydrogel obtained and be placed under-20 ~-10 DEG C of environment after freezing 24-30h, lyophilize process, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
Reaction principle of the present invention is:
There is a large amount of functional group in graphene oxide lamella surface, there is stronger interaction between the functional group on Dopamine HCL and graphene oxide lamella surface, makes dopaminergic be adsorbed in graphene oxide lamella surface.Add the damping fluid of Tutofusin tris, for reaction provides alkaline environment, at alkaline condition and under having oxygen existent condition, the catechol group of Dopamine HCL is easy to oxidized, generate the Dopamine HCL naphtoquinone compounds with adjacent benzene two quinone structure, disproportionation reaction is there is between Dopamine HCL and Dopamine HCL quinone, produce Semiquinone Radicals, then coupling forms cross-link bond, finally obtain poly-DOPA amine layer at graphene oxide lamella surface aggregate, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel.Before lyophilize under-20 ~-10 DEG C of environment freezing 24-30h, graphene oxide/poly-Dopamine HCL matrix material hydrogel can be made to form stable three-dimensional net structure.Again through lyophilize process, the stable graphene oxide with good three dimensional network structure/poly-Dopamine HCL composite aerogel can be obtained.
Compared with prior art, the invention has the beneficial effects as follows:
One, due to Dopamine HCL and graphene oxide all can in water good distribution, simultaneously based on the interaction between polar functional group, in position in polymerization process, Dopamine HCL can adsorb in surface of graphene oxide, form poly-Dopamine HCL, not only maintain limellar stripping and the good distribution in the solution of graphene oxide, optimize the formation of the gentle gel porous material of structure of graphene oxide tridimensional network from structure, ensure that integrity and the stability of graphene oxide network structure in the rear matrix material of polymerization.
Two, poly-Dopamine HCL itself has adsorption, therefore can form synergic sorption with graphene oxide, realize the high adsorption efficiency of multiple dimensioned various dimensions, particularly have good adsorption to polar organic solvent.
Four, raw material of the present invention is graphene oxide and Dopamine HCL, and raw material sources are extensive, and cost is low, simple and easy to get.
Five, utilize Dopamine HCL autoxidation polymerization process in the basic conditions to prepare matrix material, this process reaction gentleness is controlled, and productive rate is high, and has environment friendly.
Six, Freeze Drying Technique is adopted can to ensure the good distribution of graphene oxide lamella in gel, obtain larger specific surface area, the composite aerogel of preparation has high porosity, and this technology does not need complex apparatus simultaneously, simple to operation, do not relate to High Temperature High Pressure, do not need surface modification, solvent exchange supervisor, pollution-free, with low cost, suitable production in enormous quantities.
Further, in steps A of the present invention, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
Hummers method can be prepared in dispersed graphene oxide dispersion preferably in water, and can by the power of acid oxidant and oxidization time, the degree of oxidation of regulation and control graphene oxide, regulates the lamellar spacing of graphene oxide and the degree of scatter in water further.
Further, mixed mutually by Dopamine HCL in steps A of the present invention with graphene oxide water solution, the stirring velocity stirring 30-40min is 60-80r/min.
Such stirring velocity energy accelerating oxidation Graphene and the mutual mixing of Dopamine HCL, mutually absorption and the dispersion in water.
Further, the stirring velocity in step B of the present invention when the buffer reagent of graphene oxide/Dopamine HCL mixed solution and dripping Tutofusin tris and the stirring velocity continuing to stir 2-2.5h after being added dropwise to complete are 60-80r/min.
Can ensure that under such stirring velocity buffer reagent spreads fully in mixing solutions, make Dopamine HCL obtain poly-Dopamine HCL in surface of graphene oxide polymerization.
Further, leave standstill in step B of the present invention, the time of repose that Dopamine HCL is fully polymerized is 24-30h.This can ensure the polymerization completely of Dopamine HCL.
Further, the actual conditions of lyophilize process in step C of the present invention is: pressure 20-30Pa, and temperature is-50 ~-60 DEG C, and the time is 48-50h.
20-30Pa, the lyophilize parameter of-50 ~-60 DEG C, can ensure that the solid water in hole well can be gasificated into gaseous state, the structure that very large capillary force destroys hole can not be produced like this, avoid allowing hole cave in, and the sublimation drying of 48-50h can ensure that the moisture in hybrid aerogel is fully dry.
Below in conjunction with the drawings and specific embodiments, the present invention is described further.
Accompanying drawing explanation
Fig. 1 is the scanning section electron microscopic picture of the amplification 200 times of graphene oxide/poly-Dopamine HCL composite aerogel prepared by the embodiment of the present invention one.
Fig. 2 is the scanning section electron microscopic picture of the amplification 5000 times of graphene oxide/poly-Dopamine HCL composite aerogel prepared by the embodiment of the present invention one.
Fig. 3 is that the graphite oxide aerogel (right figure) of graphene oxide/poly-Dopamine HCL composite aerogel (left figure) of preparing of the embodiment of the present invention one and comparative example one preparation is to the adsorption efficiency comparison diagram of methylene blue solution.
Embodiment
Comparative example one
Be that dropwise to add 50ml concentration be in the graphene oxide water solution of 6g/ml for the damping fluid 3mL of the Tutofusin tris of 0.1mol/L by concentration, continue to stir 2h, stirring velocity is 60r/min, is poured into by the mixture obtained in beaker and leaves standstill 24h.
Freezing 24h under product being placed in-20 DEG C of environment, is then placed in freeze drier, at-50 DEG C, lyophilize 48h under the condition of 20Pa, obtains final graphite oxide aerogel.
Embodiment one
A preparation method for graphene oxide/poly-Dopamine HCL composite aerogel, its step is as follows:
A, being dissolved in 10ml distilled water by 0.6g Dopamine HCL powder, is at room temperature that the graphene oxide water solution compound of 6mg/ml mixes with 50ml concentration, and stir 30min, stirring velocity is 60r/min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 3mL concentration is the Tutofusin tris of 0.1mol/L while stirring, continue after being added dropwise to complete to stir 2h, stirring velocity is 60r/min; Then leave standstill 24h, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, by after freezing 24h under graphene oxide/poly-Dopamine HCL matrix material hydrogel is placed in-20 DEG C of environment, at pressure 20Pa, lyophilize 48h under-50 DEG C of conditions, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
In steps A described in this example, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
Fig. 1 is the scanning section electron microscopic picture of the amplification 200 times of graphene oxide/poly-Dopamine HCL composite aerogel prepared by the present embodiment, and as can be seen from the figure, the composite aerogel of preparation has good vesicular structure.Fig. 2 is the scanning section electron microscopic picture of the amplification 5000 times of graphene oxide/poly-Dopamine HCL composite aerogel prepared by the present embodiment, as can be seen from the figure, and the laminated structure of graphene oxide in poly-Dopamine HCL under high multiple.
Fig. 3 is that the graphite oxide aerogel prepared of graphene oxide/poly-Dopamine HCL composite aerogel of preparing of the embodiment of the present invention one and comparative example one is to the adsorption efficiency comparison diagram of methylene blue solution.As seen from the figure, the composite aerogel adsorption efficiency of the embodiment of the present invention one preparation is apparently higher than independent graphite oxide aerogel.
Embodiment two
A preparation method for graphene oxide/poly-Dopamine HCL composite aerogel, its step is as follows:
A, being dissolved in 10ml distilled water by 0.3g Dopamine HCL powder, is at room temperature that the graphene oxide water solution compound of 6mg/ml mixes with 50ml concentration, and stir 30min, stirring velocity is 60r/min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 9mL concentration is the Tutofusin tris of 0.1mol/L while stirring, continue after being added dropwise to complete to stir 2h, stirring velocity is 60r/min; Then leave standstill 24h, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, by after freezing 24h under graphene oxide/poly-Dopamine HCL matrix material hydrogel is placed in-20 DEG C of environment, at pressure 20Pa, lyophilize 48h under-50 DEG C of conditions, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
In steps A described in this example, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
Embodiment three
A preparation method for graphene oxide/poly-Dopamine HCL composite aerogel, its step is as follows:
A, being dissolved in 18ml distilled water by 0.7g Dopamine HCL powder, is at room temperature that the graphene oxide water solution compound of 5mg/ml mixes with 60ml concentration, and stir 40min, stirring velocity is 80r/min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 6mL concentration is the Tutofusin tris of 0.12mol/L while stirring, continue after being added dropwise to complete to stir 2.5h, stirring velocity is 80r/min; Then leave standstill 30h, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, by after freezing 30h under graphene oxide/poly-Dopamine HCL matrix material hydrogel is placed in-10 DEG C of environment, at pressure 30Pa, lyophilize 50h under-60 DEG C of conditions, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
In steps A described in this example, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
Embodiment four
A preparation method for graphene oxide/poly-Dopamine HCL composite aerogel, its step is as follows:
A, being dissolved in 11ml distilled water by 0.15g Dopamine HCL powder, is at room temperature that the graphene oxide water solution compound of 5.5mg/ml mixes with 55ml concentration, and stir 35min, stirring velocity is 70r/min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 5mL concentration is the Tutofusin tris of 0.11mol/L while stirring, continue after being added dropwise to complete to stir 2.3h, stirring velocity is 75r/min; Then leave standstill 27h, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, by after freezing 27h under graphene oxide/poly-Dopamine HCL matrix material hydrogel is placed in-15 DEG C of environment, at pressure 25Pa, lyophilize 49h under-55 DEG C of conditions, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
In steps A described in this example, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
Embodiment five
A preparation method for graphene oxide/poly-Dopamine HCL composite aerogel, its step is as follows:
A, being dissolved in 15ml distilled water by 0.4g Dopamine HCL powder, is at room temperature that the graphene oxide water solution compound of 5.5mg/ml mixes with 55ml concentration, and stir 35min, stirring velocity is 70r/min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 5mL concentration is the Tutofusin tris of 0.11mol/L while stirring, continue after being added dropwise to complete to stir 2.3h, stirring velocity is 75r/min; Then leave standstill 27h, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, by after freezing 27h under graphene oxide/poly-Dopamine HCL matrix material hydrogel is placed in-15 DEG C of environment, at pressure 25Pa, lyophilize 49h under-55 DEG C of conditions, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
In steps A described in this example, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
Claims (6)
1. a preparation method for graphene oxide/poly-Dopamine HCL composite aerogel, its step is as follows:
A, being dissolved in 10-18ml distilled water by 0.15-0.7g Dopamine HCL powder, is at room temperature that the graphene oxide water solution compound of 5-6mg/ml mixes with 50-60ml concentration, stirs 30-40min, obtains graphene oxide/Dopamine HCL mixing solutions;
B, in graphene oxide/Dopamine HCL mixing solutions, dropwise add the damping fluid that 3-9mL concentration is the Tutofusin tris of 0.1-0.12mol/L while stirring, continue after being added dropwise to complete to stir 2-2.5h; Then leave standstill, Dopamine HCL is fully polymerized, obtain graphene oxide/poly-Dopamine HCL matrix material hydrogel;
C, to be placed in by graphene oxide/poly-Dopamine HCL matrix material hydrogel under-20 ~-10 DEG C of environment after freezing 24-30h, lyophilize process, obtains graphene oxide/poly-Dopamine HCL composite aerogel.
2. the preparation method of a kind of graphene oxide according to claim 1/poly-Dopamine HCL composite aerogel, is characterized in that: in described steps A, the graphene oxide of graphene oxide water solution is prepared by Hummers method.
3. the preparation method of a kind of graphene oxide according to claim 1/poly-Dopamine HCL composite aerogel, it is characterized in that: mixed mutually with graphene oxide water solution by Dopamine HCL in described steps A, the stirring velocity stirring 30-40min is 60-80r/min.
4. the preparation method of a kind of graphene oxide according to claim 1/poly-Dopamine HCL composite aerogel, is characterized in that: the stirring velocity in described step B when the buffer reagent of graphene oxide/Dopamine HCL mixed solution and dripping Tutofusin tris and the stirring velocity continuing to stir 2-2.5h after being added dropwise to complete are 60-80r/min.
5. the preparation method of a kind of graphene oxide according to claim 1/poly-Dopamine HCL composite aerogel, is characterized in that: leave standstill in described step B, the time of repose that Dopamine HCL is fully polymerized is 24-30h.
6. the preparation method of a kind of graphene oxide according to claim 1/poly-Dopamine HCL composite aerogel, it is characterized in that: the actual conditions of lyophilize process in described step C is: pressure 20-30Pa, temperature is-50 ~-60 DEG C, and the time is 48-50h.
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