CN113926397B - Graphene pyrrole aerogel and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a graphene pyrrole aerogel and a preparation method and application thereof, the method is based on the characteristics that a graphene-based material is strong in chemical stability and good in corrosion resistance and has light absorption in all bands, a photo-thermal high polymer material is modified on the surface of the graphene-based aerogel to obtain the graphene-based aerogel with regular nanometer apertures, solar energy is absorbed in a divided manner and is converted to be local to a gas-liquid interface through the characteristic that the surface of the graphene-based aerogel is similar to a black body under the irradiation of sunlight, and meanwhile, the energy consumption is reduced and efficient material separation is realized by combining with a test means of joule heat, so that the effect of seawater desalination is achieved. The invention utilizes clean sustainable energy solar energy and combines a joule heat test means to alternately and continuously carry out seawater desalination test, and is a novel seawater desalination method with lower energy consumption and high efficiency.
Description
Technical Field
The invention relates to a graphene pyrrole aerogel, a preparation method and application thereof.
Background
With the rapid development of modern industry and the continuous increase of world population, the water crisis has become one of the major challenges facing human beings in the 21 st century, reverse Osmosis (RO) is the key technology for relieving the water shortage problem in China at present, and the membrane which is the most key component in the whole reverse osmosis desalination device determines the separation performance of the whole device to a great extent, but the process energy consumption is large, and the low permeability limits the development of the reverse osmosis desalination device. In recent years, the generation of clean water from seawater and even industrial wastewater by using solar energy is a promising approach to solve the water resource shortage, which has certain requirements on the performance of membranes, strong corrosion resistance, high desalination rate, cyclic utilization and low energy consumption, so that the development of novel seawater desalination membrane materials is needed.
CN201811474338.5 discloses a preparation method of graphene aerogel, which includes subjecting a sample obtained by spraying pre-reduced graphene oxide sol to freeze drying and thermal reduction treatment to obtain a graphene aerogel film, and adding a noble nano-metal into the graphene aerogel film to prepare the graphene aerogel. However, the disadvantages of the invention are: 1. noble metal nanoparticles are needed, so that the cost is high; 2. the preparation method is complex, particularly a series of complicated operations of spraying, freeze drying, thermal reduction treatment, compounding of the hydrophilic material (sodium alginate) and addition of the nano noble metal particles not only consumes long time, but also fails in material preparation if one link goes wrong, so that the success rate of material preparation is low; 3. the noble metal nano particles are easy to agglomerate, so that the surface plasma resonance effect cannot occur.
Disclosure of Invention
The invention mainly aims to provide a simple preparation method of graphene pyrrole aerogel, which can be used for seawater desalination efficiently through regulation and control of an external field (a light field and an electric field).
The technical scheme of the invention is as follows:
a preparation method of graphene pyrrole aerogel comprises the following steps:
1) Preparing graphene oxide;
2) Adjusting the concentration of graphene oxide to be 5-50mg/ml, then adding a reducing agent into the graphene oxide dispersion liquid, wherein the volume ratio of the graphene oxide dispersion liquid to the graphene oxide dispersion liquid is 1-10; if the hydrothermal reaction is less than 1h, the product is too hydrophilic; and above 3h, too hydrophobic.
3) Preparing 0.1-5V/V% pyrrole aqueous solution; and preparing 0.5-5M ammonium persulfate hydrochloride solution; if the concentration of the ammonium persulfate hydrochloride is lower than 0.5M, the recombination rate is too slow; if the molecular weight is higher than 5M, the speed of the composite polypyrrole is too high, so that agglomeration is caused; slowly immersing the obtained RGO aerogel into a pyrrole solution until the RGO aerogel is completely soaked, and naturally drying the soaked RGO; slowly immersing the dried RGO into a hydrochloric acid ammonium persulfate solution, polymerizing for 5-12h at 1-5 ℃, and if the polymerization time is less than 5h, ensuring that no polypyrrole is compounded on the RGO aerogel; if it is higher than 12 hours, the polypyrroles are compounded too much to cause polymerization agglomeration; and finally, washing the sample with deionized water, and drying to obtain the graphene polypyrrole aerogel. And/or
4) And (4) placing the graphene polypyrrole aerogel prepared in the step (3) in a 1% Polytetrafluoroethylene (PTFE) solution for slow hydrophobic treatment for 1-3 hours, and drying to obtain the graphene polypyrrole aerogel with a hydrophobic surface.
In an embodiment of the present invention, step 2) is: preparing reduced graphene oxide hydrogel from the prepared graphene oxide according to the mass concentration of 8-20mg/ml, adding 5-10ml of reducing agent ammonia water into 5-10ml of GO dispersion liquid of 8-20mg/ml, uniformly stirring the solution, pouring the solution into a reaction kettle, then placing the reaction kettle into an oven with the temperature of 170-190 ℃, carrying out hydrothermal reaction for 1.5-2.5 hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times, and carrying out freeze drying to form RGO aerogel.
In an embodiment of the present invention, the reducing agent in step 2) is ammonia water.
The invention also provides the graphene pyrrole aerogel prepared by the preparation method.
The graphene pyrrole aerogel provided by the invention has an average pore diameter of 5-15 μm.
The invention also provides application of the graphene pyrrole aerogel in seawater desalination.
The invention also provides a seawater desalination method based on graphene-based aerogel interface film evaporation, which comprises the following steps:
1) Preparing graphene pyrrole aerogel according to the preparation method;
2) Soaking and suspending the prepared graphene-based aerogel on the surface of seawater, and then realizing interface photothermal conversion of the graphene-based aerogel through local heating under the irradiation of sunlight so as to desalt seawater and/or
3) Fixing the graphene-based aerogel subjected to hydrophobic treatment on a seawater desalination device, and realizing seawater desalination with low energy consumption by utilizing a mode of generating joule heat.
The invention provides a novel seawater desalination method based on interface film evaporation, which is characterized in that the unique advantages (high solar energy absorption rate) of graphene-based aerogel are utilized, solar energy is absorbed in a divided manner and energy is converted to a local gas-liquid interface, so that the light-steam energy conversion efficiency is effectively improved, heat is generated at the local gas-liquid interface, and then water vapor is condensed through an internal aperture channel of the graphene-based aerogel, so that the separation and concentration of seawater are realized; on the other hand, the seawater desalination process is realized under the condition of low energy consumption by adopting the joule heat effect of the seawater desalination device. The graphene-based aerogel in the process has excellent characteristics of high mass transfer flux, high water transfer capacity, corrosion resistance, high efficiency utilization rate and the like, can obtain very high brine recovery rate, and is a good seawater desalination membrane material.
The invention has the beneficial effects that:
1. the preparation process flow is simple and easy to operate;
2. the hydrophilic and hydrophobic properties of the graphene-based aerogel can be regulated and controlled by controlling the hydrothermal reaction time; the hydrophilic material can be completely soaked and suspended on the surface of seawater, and in the evaporation process, the seawater can be continuously transported to the surface of the material, so that the evaporation process is continuously carried out, and the hydrophobic material is not beneficial to the continuous operation of the evaporation process. The solar energy absorption rate of the graphene-based aerogel is further improved by utilizing the photothermal property of the polypyrrole, so that the seawater desalination efficiency is improved.
3. Meanwhile, the seawater desalination process can be alternately and continuously realized by designing a membrane material and combining a joule heat test means. The invention develops a novel seawater desalination membrane material. And the high-efficiency substance separation is realized under the condition of reducing energy consumption by utilizing the joule heat effect of the material.
Drawings
The invention is further illustrated by the following figures and examples.
Fig. 1 is a schematic diagram of a preparation process of graphene-based aerogel.
Fig. 2 SEM topography of graphene-based aerogel.
Fig. 3 is an ir thermographic comparison of three graphene-based aerogels.
Fig. 4 shows a photo-thermal test chart and a stability test chart of the graphene-based aerogel.
Fig. 5 is an infrared thermal imaging graph of graphene-based aerogel solar evaporation and joule heating test.
Detailed Description
Comparative example 1
Step one, weighing 2.5g of dried graphite powder, adding concentrated sulfuric acid and concentrated phosphoric acid (volume ratio 9; slowly adding 170ml of ultrapure water into the solution under the condition of an ice water bath (3 ℃), and stirring for half an hour until the solution is dark brown; then adding 15% H to the above solution2O2Until no bubble is generated, the solution turns into golden yellow, and then the solution is poured into a dialysis bag to be dialyzed in distilled water solution until the solution is dialyzed to be neutral;
secondly, drying the prepared Graphene Oxide (GO) to calculate the mass concentration of the Graphene Oxide (GO), fixing the mass concentration of the Graphene Oxide (GO) at 10mg/ml and the volume of the Graphene Oxide (GO) at 10ml, and then pouring the Graphene Oxide (GO) into a polytetrafluoroethylene grinding tool to freeze and dry the Graphene Oxide (GO) by using a freeze dryer to obtain Graphene Oxide (GO) aerogel;
thirdly, putting the Graphene Oxide (GO) aerogel prepared in the second step into a beaker filled with 100g/L NaCl heavy salt water solution, ensuring that the Graphene Oxide (GO) aerogel is suspended on the water surface, arranging collecting devices above and below the beaker, and turning on a sunlight simulator to adjust the power of the sunlight simulator to be 1,2,4 and 6KW m respectively-2Shine Graphene Oxide (GO) aerogel, material surface temperature constantly rises among the experimentation, obtains retrieving in collection device department after the steam condensation and continuously carries out 30 minutes, 6 KWm-2The maximum evaporation rate under the light intensity is 4.84kg m-2h-1The evaporation efficiency was 50%.
Comparative example 2
In the first step, 2.5g of dried graphite powder is weighed, concentrated sulfuric acid and concentrated phosphoric acid (volume ratio 9Slowly adding into the solution, continuing the process for two hours, removing the ice water bath device, and stirring the solution for two hours; 170ml of ultrapure water was slowly added to the above solution in an ice water bath (3 ℃), followed by heating to 30 ℃ and stirring for half an hour (the solution was dark brown); adding 15% to the above solution2O2Until no bubble is generated, the solution turns into golden yellow, and then the solution is poured into a dialysis bag to be dialyzed in distilled water solution until the solution is dialyzed to be neutral;
secondly, drying the prepared Graphene Oxide (GO) to calculate the mass concentration, then preparing reduced graphene oxide hydrogel with the mass concentration of 10mg/ml, adding 7.4ml of reducing agent ammonia water into 6.4ml of GO dispersion liquid of 10mg/ml, uniformly stirring the solution, pouring the solution into a 100ml reaction kettle, then putting the reaction kettle into an oven at 180 ℃, performing hydrothermal reaction for two hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times to be neutral, and then performing freeze drying to form RGO aerogel;
thirdly, putting the RGO aerogel prepared in the second step into a beaker filled with 100g/L NaCl heavy salt water solution and ensuring that the RGO aerogel is suspended on the water surface, arranging collecting devices above and below the beaker, and turning on a solar simulator to adjust the power of the solar simulator to be 1,2,4 and 6KW m respectively-2Irradiating Graphene Oxide (GO) aerogel at 2KW m in the experimental process-2Under the action of light intensity, the surface temperature of the material can reach 60 ℃ within 10 minutes, and the steam is condensed and then recycled at a collecting device for 30 minutes, namely 6KW m-2The maximum evaporation rate under the light intensity is 7.0226kg m-2h-1The evaporation efficiency was 73%.
Example 1
Step one, weighing 2.5g of dried graphite powder, adding concentrated sulfuric acid and concentrated phosphoric acid (volume ratio 9; slowly adding into the solution under the condition of ice water bath (3 deg.C)Slowly adding 170ml of ultrapure water, then heating to 30 ℃ and stirring for half an hour (the solution is dark brown); adding 15% to the above solution2O2The solution is added into a dialysis bag to be dialyzed in distilled water solution until the solution is neutral;
secondly, drying the prepared Graphene Oxide (GO) to calculate the mass concentration, then preparing reduced graphene oxide hydrogel with the mass concentration of 10mg/ml, adding 7.4ml of reducing agent ammonia water into 6.4ml of GO dispersion liquid of 10mg/ml, uniformly stirring the solution, pouring the solution into a 100ml reaction kettle, then putting the reaction kettle into an oven at 180 ℃, performing hydrothermal reaction for two hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times to be neutral, and then performing freeze drying to form RGO aerogel;
in the third step, 100. Mu.L (after distillation under reduced pressure) of pyrrole was poured into 10ml of deionized water and stirred at room temperature to form a pyrrole solution. 0.456g Ammonium Persulfate (APS) and 2mL concentrated hydrochloric acid (HCl) were dissolved in 18mL deionized water to form a 1.2M ammonium persulfate hydrochloride solution; the RGO aerogel obtained above was slowly immersed in a pyrrole solution, and after total adsorption of pyrrole monomers, py-RGO was transferred to a petri dish and allowed to air dry for about 1h. Then, py-RGO was slowly immersed in APS/HCl and polymerized at 4 ℃ for 12 hours; finally, removing residual PPy particles from the sample by using deionized water, and drying at 70 ℃ to obtain PPy-RGO aerogel;
fourthly, putting the PPy-RGO aerogel prepared in the third step into a beaker filled with 100g/L NaCl heavy salt water solution and ensuring that the PPy-RGO aerogel is suspended on the water surface, arranging collecting devices above and below the beaker, and turning on a solar simulator to adjust the power of the solar simulator to be 1,2,4 and 6KW m respectively-2Irradiating Graphene Oxide (GO) aerogel at 2KW m-2Under the action of light intensity, the surface temperature of the material can reach 65 ℃ within 10 minutes, and the steam is condensed and then recovered at a collecting device for 30 minutes, 6KW m-2The evaporation rate under the light intensity is 8.272kg m-2h-1The evaporation efficiency was 86.4%.
Example 2
Step one, weighing 2.5g of dried graphite powder, adding concentrated sulfuric acid and concentrated phosphoric acid (volume ratio 9; 170ml of ultrapure water is slowly added into the solution under the condition of ice water bath (3 ℃), then the temperature is raised to 30 ℃ and the solution is stirred for half an hour (the solution is dark brown); adding 15% to the above solution2O2Until no bubble is generated, the solution turns into golden yellow, and then the solution is poured into a dialysis bag to be dialyzed in distilled water solution until the solution is dialyzed to be neutral;
step two, drying the prepared Graphene Oxide (GO) to calculate the mass concentration of the graphene oxide, then preparing reduced graphene oxide hydrogel according to the mass concentration of 10mg/ml, adding 7.4ml of reducing agent ammonia water into 6.4ml of GO dispersion liquid of 10mg/ml, uniformly stirring the solution, pouring the solution into a 100ml reaction kettle, then putting the reaction kettle into an oven at 180 ℃, performing hydrothermal reaction for two hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times, neutralizing the hydrogel, and performing freeze drying to form RGO aerogel;
in the third step, 100. Mu.L (after distillation under reduced pressure) of pyrrole was poured into 10ml of deionized water and stirred at room temperature to form a pyrrole solution. 0.456g Ammonium Persulfate (APS) and 2mL concentrated hydrochloric acid (HCl) were dissolved in 18mL deionized water to form a 1.2M ammonium persulfate hydrochloride solution; the RGO aerogel obtained above was slowly immersed in the pyrrole solution, and after total adsorption of pyrrole monomers, py-RGO was transferred to a petri dish and allowed to air dry for about 1h. Then, py-RGO was slowly immersed in APS/HCl and polymerized at 4 ℃ for 12 hours; finally, removing residual PPy particles from the sample by using deionized water, and drying at 70 ℃ to obtain PPy-RGO aerogel;
fourthly, putting the prepared graphene-based aerogel into a beaker filled with 100g/L NaCl heavy salt water solution, ensuring that the graphene-based aerogel is suspended on the water surface, arranging collecting devices above and below the beaker, and turning on a solar simulator to adjust the power of the solar simulator to be 1,2,4 and 6KW m respectively-2Paired stonesThe ink-based aerogel was irradiated at 2KW m during the experiment-2Under the action of light intensity, the surface temperature of the material is continuously increased to 65 ℃, the steam is condensed and then recovered at a collecting device for 30 minutes, the desalination rate is up to 99.3 percent, and the material can continuously work for more than 5 hours.
Example 3
Step one, weighing 2.5g of dried graphite powder, adding concentrated sulfuric acid and concentrated phosphoric acid (volume ratio 9; 170ml of ultrapure water was slowly added to the above solution in an ice water bath (3 ℃), followed by heating to 30 ℃ and stirring for half an hour (the solution was dark brown); adding 15% to the above solution2O2The solution is added into a dialysis bag to be dialyzed in distilled water solution until the solution is neutral;
step two, drying the prepared Graphene Oxide (GO) to calculate the mass concentration of the graphene oxide, then preparing reduced graphene oxide hydrogel according to the mass concentration of 10mg/ml, adding 7.4ml of reducing agent ammonia water into 6.4ml of GO dispersion liquid of 10mg/ml, uniformly stirring the solution, pouring the solution into a 100ml reaction kettle, then putting the reaction kettle into an oven at 180 ℃, performing hydrothermal reaction for two hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times, neutralizing the hydrogel, and performing freeze drying to form RGO aerogel;
in the third step, 100. Mu.L (after distillation under reduced pressure) of pyrrole was poured into 10ml of deionized water and stirred at room temperature to form a pyrrole solution. 0.456g Ammonium Persulfate (APS) and 2mL concentrated hydrochloric acid (HCl) were dissolved in 18mL deionized water to form a 1.2M ammonium persulfate hydrochloride solution; the RGO aerogel obtained above was slowly immersed in the pyrrole solution, and after total adsorption of pyrrole monomers, py-RGO was transferred to a petri dish and allowed to air dry for about 1h. Then, py-RGO was slowly immersed in APS/HCl and polymerized at 4 ℃ for 12 hours; finally, removing residual PPy particles from the sample by using deionized water, and drying at 70 ℃ to obtain PPy-RGO aerogel;
and fourthly, putting the prepared graphene-based aerogel into a 1% PTFE solution for hydrophobic treatment, testing that the contact angle is 144 degrees, and then fixing the graphene-based aerogel in a seawater desalination prototype device, wherein under the condition of external voltage, the material locally heats seawater due to the self Joule heat effect, so that the energy consumption is reduced, and efficient substance separation is realized. The experimental result shows that the evaporation efficiency is increased along with the increase of the applied voltage.
While particular embodiments of the present invention have been described in the foregoing specification, various modifications and alterations to the previously described embodiments will become apparent to those skilled in the art from this description without departing from the spirit and scope of the invention.
Claims (9)
1. The preparation method of the graphene pyrrole aerogel comprises the following steps:
1) Preparing graphene oxide;
2) Preparing reduced graphene oxide hydrogel from the prepared graphene oxide according to the mass concentration of 8-20mg/ml, adding 5-10ml of reducing agent ammonia water into 5-10ml of GO dispersion liquid of 8-20mg/ml, uniformly stirring the solution, pouring the solution into a reaction kettle, then putting the reaction kettle into an oven with the temperature of 170-190 ℃, carrying out hydrothermal reaction for 1.5-2.5 hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times, and then carrying out freeze drying to form RGO aerogel;
3) Preparing 0.1-5V/V% pyrrole aqueous solution; and 0.5-5M ammonium persulfate hydrochloride solution; slowly immersing the obtained RGO aerogel into a pyrrole aqueous solution until the RGO aerogel is completely soaked, and naturally drying the soaked RGO; slowly immersing the dried RGO into ammonium persulfate hydrochloride solution, and polymerizing for 5-10 h at 1-5 ℃; and finally, washing the sample by using deionized water, and drying to obtain the graphene pyrrole aerogel.
2. The method for preparing graphene pyrrole aerogel according to claim 1, wherein: the reducing agent in the step 2) is ammonia water.
3. The method for preparing graphene pyrrole aerogel according to claim 1, wherein: the step 2) is as follows: preparing reduced graphene oxide hydrogel from the prepared graphene oxide according to the mass concentration of 10mg/ml, adding 7.4ml of reducing agent ammonia water into 6.4ml of 10mg/ml GO dispersion liquid, uniformly stirring the solution, pouring the solution into a 100ml reaction kettle, then placing the reaction kettle into an oven at 180 ℃, performing hydrothermal reaction for two hours to prepare RGO hydrogel, taking the hydrogel out of the reaction kettle, washing the hydrogel for several times, and performing freeze drying to obtain the RGO aerogel.
4. The method for preparing graphene pyrrole aerogel according to claim 1, wherein: the step 3) is as follows: 100. injecting 10ml of deionized water into the microliter of pyrrole, and stirring at room temperature to form a pyrrole solution; dissolving 0.456g ammonium persulfate and 2mL concentrated hydrochloric acid in 18mL deionized water to form a 1.2M ammonium persulfate hydrochloride solution; slowly immersing the obtained RGO aerogel into a pyrrole solution, fully adsorbing, transferring the soaked RGO into a culture dish, and naturally drying for 1 h; then, the dried RGO is slowly immersed into ammonium persulfate hydrochloride solution to be polymerized for 12 hours at the temperature of 4 ℃; and finally, washing the sample with deionized water, and drying at 70 ℃ to obtain the graphene pyrrole aerogel.
5. The method for preparing the graphene pyrrole aerogel according to claim 1, further comprising the steps of: and (3) placing a part of the prepared graphene polypyrrole aerogel in a 1% polytetrafluoroethylene solution for hydrophobic treatment for 1-5h.
6. Graphene pyrrole aerogel, prepared according to the method for the preparation of graphene pyrrole aerogel according to any one of claims 1 to 5.
7. The graphene pyrrole aerogel of claim 6, wherein the aerogel has an average pore size of 5 to 15 μm.
8. Use of the graphene pyrrole aerogel according to claim 6 in seawater desalination.
9. A seawater desalination method based on graphene-based aerogel interface film evaporation comprises the following steps:
1) Preparing graphene pyrrole aerogel according to the preparation method of any one of claims 1 to 5;
2) Soaking and suspending the prepared graphene-based aerogel on the surface of seawater, and then carrying out interface photothermal conversion on the graphene-based aerogel through local heating under the irradiation of sunlight so as to desalt the seawater; and/or
3) Fixing the graphene-based aerogel subjected to hydrophobic treatment on a seawater desalination device, and realizing seawater desalination with low energy consumption by utilizing a mode of generating joule heat.
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