CN113786782B - Preparation method and application of self-blackened quinoa cellulose/graphene oxide aerogel - Google Patents
Preparation method and application of self-blackened quinoa cellulose/graphene oxide aerogel Download PDFInfo
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- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- Y02A20/124—Water desalination
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- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
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- Y02A20/138—Water desalination using renewable energy
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- Y02A20/20—Controlling water pollution; Waste water treatment
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Abstract
The invention discloses a preparation method and application of self-darkening quinoa cellulose/graphene oxide aerogel, and belongs to the technical field of material chemistry and photothermal conversion materials. Firstly, extracting and purifying cellulose in quinoa bran by a chemical extraction method; then compounding cellulose and graphene oxide to prepare aerogel with the color changing from light brown to dark black under the synergistic stimulation of water and light; finally, the aerogel is applied to the field of sea water desalination by the boundary, and the sunlight intensity is simulated in a certain range (1000W m ‑2 ) Under irradiation, the evaporation rate reached 3.6kg m ‑2 h ‑1 The method comprises the steps of carrying out a first treatment on the surface of the The outdoor experiment lasts for 15 days, and the evaporation rates of the simulated seawater and the distilled water reach 12.6kg m respectively ‑ 2 day ‑1 And 12kg m ‑2 day ‑1 The method comprises the steps of carrying out a first treatment on the surface of the Meanwhile, the aerogel is improved to have good self-cleaning performance in the field of sea water desalination.
Description
Technical Field
The invention belongs to the technical field of material chemistry and photothermal conversion materials, and particularly relates to a preparation method and application of self-darkening quinoa cellulose/graphene oxide aerogel.
Background
In the course of human activities, a large amount of domestic and industrial sewage is produced, and the sewage brings great adverse effect to the ecological environment, and directly affects the development of human society. In addition, the problem of global water resource starvation is becoming more serious, and especially in some undeveloped areas, how to convert domestic industrial sewage into a water source which can be drunk and is needed industrially is one of the main directions of scientific research in the world today.
The traditional means for sea water desalination and sewage purification are as follows: reverse osmosis, ion exchange, distillation, multi-stage flash evaporation, adsorption and the like, and the technologies have the greatest characteristics of high equipment construction cost and high maintenance cost, and have great requirements on fossil energy, and are directly restricted from being popularized and widely used. Solar energy is a widely existing, inexhaustible renewable resource on earth. The conversion of non-water resources such as seawater, wastewater and the like into potable fresh water by utilizing a solar water vapor evaporation technology is a low-cost, easy-to-operate, environment-friendly and possibly large-scale application fresh water resource regeneration scheme developed in recent years, and has attracted wide attention of scientists in various countries.
The efficiency of solar water vapor evaporation is closely related to the absorption of sunlight and the 'photo-thermal' conversion performance of the photo-thermal conversion material. The ideal photothermal conversion material has the following characteristics: (1) broad spectral absorption capability in the ultraviolet to infrared (200-2500 nm) range; (2) high photo-thermal conversion efficiency; (3) lower internal heat loss; (4) providing sufficient water supply channels and water vapor escape channels; (5) the material has good durability. Depending on the mechanism of photothermal conversion, photothermal conversion materials can be divided into: (1) metallic materials such as gold (Au), silver (Ag), palladium (Pa), platinum (Pt), chromium (Cr), nickel (Ni), copper (Cu), aluminum (Al) nanoparticles, and the like; (2) semiconductor materials, such as; titanium dioxide (TiO) 2 ) Copper sulphide (CuS), cu 2 -xSe, iron oxide (Fe 3 O 4 ) Titanium nitride (TiN), mxene (Ti) 3 C 2 ) Etc.; (3) organic polymers such as polypyrrole, polydopamine, some two-dimensional conjugated polymers, and the like; (4) carbon materials such as carbon nanotubes, graphene, carbon nanoparticles, carbon aerogels, biochar, and the like.
Among the numerous photothermal conversion materials, carbon materials are attracting attention because of wide sources and excellent broadband light absorption performance and physicochemical stability, wherein biomass-based carbon materials are very abundant in sources, simple in preparation process and unique in pore structure, and provide good channels for water flow transportation and water vapor escape, which has become an important point of research on the current photothermal conversion materials. The nature produces about billions or even trillions of tons of biomass resources per year. Biomass is the most abundant renewable, green, environmentally friendly, biodegradable natural polymer resource for storage on earth, however, most of these biomasses are treated in the manners of incineration, natural spoilage and direct disposal, resulting in huge resource waste and environmental pollution. In addition, the photo-thermal conversion materials reported so far accumulate a large amount of crystalline salt on the surface during the use process in the seawater treatment process, so that the performance of the photo-thermal conversion materials is reduced. Therefore, how to combine cellulose and solar energy together with two natural renewable resources synergistically and efficiently designs an efficient solar water vapor evaporation system, and meanwhile, the solar water vapor evaporation system is a functional evaporator capable of automatically cleaning crystalline salt when seawater is treated, so that the solar water vapor evaporation system becomes a research hot spot and a technical challenge in the current world.
Disclosure of Invention
Aiming at the problem that the existing photo-thermal conversion material can accumulate a large amount of crystal salt on the surface in the use process in the seawater treatment process, so that the performance of the photo-thermal conversion material is reduced, the invention provides a preparation method and application of self-darkening quinoa cellulose/graphene oxide aerogel.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of self-darkening quinoa cellulose/graphene oxide aerogel comprises the following steps:
step 1, extracting quinoa cellulose;
step 2, extracting the quinoa cellulose in the step 1 to prepare quinoa cellulose aqueous dispersion;
and step 3, adding graphene oxide dispersion liquid into the quinoa cellulose aqueous dispersion liquid, mixing to prepare a plurality of parts of composite liquid, uniformly mixing the plurality of parts of composite liquid by ultrasonic, filtering to form a paste cake, and freeze-drying to obtain the quinoa cellulose/graphene oxide aerogel. A large number of cavity channels are formed in the aerogel formed through freeze drying, so that a good channel is provided for conveying moisture, and meanwhile, a channel can be provided for conveying salt, and a self-cleaning effect is achieved.
Further, the step 1 of extracting quinoa cellulose further comprises the following steps:
step 1.1, crushing and sieving quinoa skin, collecting powder, and drying to obtain quinoa skin powder;
step 1.2, extracting quinoa peel powder with benzene/ethanol solution to obtain a first extract;
step 1.3 subjecting the first extract to NaClO 2 Heating and stirring the solution, regulating Ph with acetic acid, filtering, washing with distilled water to neutrality, and obtaining second extract;
step 1.4, heating and stirring the second extract by using NaOH solution, and carrying out suction filtration, wherein the filtrate is washed by distilled water to be not alkaline, so as to obtain a suction filtration filter cake;
and 1.5, heating the filter cake subjected to suction filtration by using an HCl solution, performing suction filtration, washing to be neutral by using distilled water, drying and crushing.
Further, the number of crushed and screened meshes in the step 1.1 is 80 meshes; the drying temperature in the step 1.1 is 60 ℃ and the drying time is 12 hours.
Further, the device extracted in the step 1.2 is a Soxhlet extractor;
in the step 1.2, the relation between quinoa peel powder and liquid benzene/ethanol solution is that 150-250 mL benzene/ethanol solution with the volume ratio of 2:1 is selected for each 60g quinoa peel powder; the extraction temperature of the extraction in the step 1.2 is 85-95 ℃ and the extraction time is 12h.
Further, naClO in the step 1.3 2 The mass fraction of the solution is 1-5%, the Ph is regulated by acetic acid, specifically, ph=4-5 is regulated by acetic acid with the concentration of 5%, the temperature of heating and stirring treatment is 75 ℃, and the stirring treatment time is 1.5h; the stirring operation in the step 1.3 adopts a heat collection type magnetic stirrer.
Further, in the step 1.4, the mass fraction of the NaOH solution is 1-10%, the heating temperature of the heating and stirring treatment is 85-95 ℃, and the stirring treatment time is 1.5h.
Further, in the step 1.5, the mass fraction of the HCl solution is 1-5%, the temperature of the heating treatment is 70-90 ℃, the time is 2 hours, the drying temperature is 60 ℃, and the drying time is 24 hours.
Further, the mass fraction of the quinoa cellulose aqueous dispersion liquid in the step 2 is 0.5-5%;
the specific method for preparing the quinoa cellulose aqueous dispersion liquid in the step 2 comprises the following steps: treatment with a cantilever high speed disperser for 1h followed by additional sonication for 1h is repeated 5-10 times until a uniform suspension is formed.
Further, the graphene oxide content in the composite liquid in the step 3 is 2.5wt%, 5wt% and 10wt% respectively; the concentration of the graphene oxide dispersion liquid in the step 3 is 2mg mL -1 The method comprises the steps of carrying out a first treatment on the surface of the And (3) the ultrasonic time for ultrasonic uniform mixing in the step (3) is 1h.
Application of self-darkening quinoa cellulose/graphene oxide aerogel in lightAnd under the combined stimulation of water, the light brown color is changed into dark black color, and the light absorption is enhanced; the self-cleaning function is carried out on the crystallized salt with accumulated surface area under the condition of no illumination or weak illumination in the sea water desalting process; the weak illumination condition is that the illumination is less than 300W m -2 The method comprises the steps of carrying out a first treatment on the surface of the The self-cleaning function is specifically that under the condition of no or weak illumination, the crystal salt accumulated on the surface can be dissolved in the seawater body under the action of chemical potential; the time required for blackening is 30-240 min.
Compared with the prior art, the invention has the following advantages:
the cellulose used by the aerogel is extracted from the wheat bran of the quinoa by a chemical method; the color of the aerogel prepared by the extracted cellulose and the graphene oxide is changed from light brown to dark black under the synergistic stimulation of water and light; the blackened aerogel has excellent photo-thermal conversion performance and can be applied to interface water vapor evaporation; meanwhile, the evaporator composed of the aerogel has excellent self-cleaning performance of self-desalination, and has good self-desalination performance and long-term stable usability in the sea water desalination process.
The invention provides a new way for utilizing the byproduct of quinoa processing, the evaporator does not need high-temperature treatment, the pollution can be effectively relieved, and the evaporator for high-efficiency seawater treatment can be prepared.
The evaporator prepared by the invention has a good self-cleaning function of the crystallized salt, and the evaporation performance is stable after long-time use.
Drawings
FIG. 1 is a physical picture of a laboratory evaporator;
FIG. 2 SEM scan of quinoa cellulose/graphene oxide aerogel;
FIG. 3 SBA under water only stimulation 10 A color change;
FIG. 4 SBA under "Water-light" Combined stimulation 10 A color change;
FIG. 5 sample SBA 10 Ultraviolet-visible-near infrared absorption spectra before and after the combined stimulus of "water-light";
FIG. 6 evaporator SBA 10 At 1Simulating the change of quality with time under sunlight;
FIG. 7 evaporator SBA 10 The evaporation rate varies with time in 1 simulated daylight;
FIG. 8 is a real-life diagram of the experimental device under real sunlight;
FIG. 9 the amount of water evaporated per day and the average intensity of sunlight in real sunlight;
FIG. 10 evaporator SBA 10 Surface crystalline salts change with time;
FIG. 11 evaporator SBA 10 After the simulated seawater is treated, ions in the water change.
Detailed Description
Example 1
Extracting quinoa fibers:
(1) 100g of quinoa skin is crushed by a crusher, passes through a 80-mesh screen, collects powder, and is dried in an oven at 60 ℃ for 12 hours to remove water.
(2) 60g of the dried quinoa peel powder is accurately weighed, tightly packed by filter paper, and placed in a Soxhlet extractor, and benzene/ethanol solution with the volume ratio of 2:1 is extracted for 12 hours at the temperature of 85-95 ℃.
(3) Placing the extract into NaClO with mass fraction of 1% 2 In the solution, ph=4-5 (PH test paper) is adjusted by acetic acid (5%), the solution is placed in a heat-collecting magnetic stirrer for heating and uniformly stirring for 1.5h at 75 ℃, suction filtration is carried out, distilled water is used for washing 5 times, and the pH test paper is used for measuring that the solution is neutral.
(4) Placing the extract into NaOH solution with mass fraction of 5%, heating and stirring at 85-95 ℃ for 1.5h, then carrying out suction filtration, washing with distilled water, and testing with pH test paper until the filtrate does not show alkalinity.
(5) Treating the filter cake by pumping filtration with HCl with the mass fraction of 1% at 70-90 ℃ for 2 hours, pumping filtration, washing with distilled water for 15 times until neutral, drying in a 60 ℃ oven for 24 hours, and crushing after drying. Preparing an aqueous solution with the mass fraction of 1% from the extracted quinoa cellulose. The specific method comprises the following steps: treatment with a cantilever high speed disperser for 1h followed by additional sonication for 1h is repeated 5-10 times until a uniform suspension is formed.
Example 2
In a 50mL beaker of water, the mixture,22.5g of the aqueous cellulose solution prepared in example 1 and 2.89g (2 mg mL) of graphene oxide dispersion were weighed -1 ) Ultrasonic treatment is carried out for 1h to ensure that the materials are uniformly mixed; filtering to obtain paste cake, placing in-18deg.C refrigerator, taking out after 24 hr, lyophilizing with a lyophilizing machine for 48 hr to remove water to obtain quinoa cellulose/graphene oxide aerogel, named SBA 2.5 。
Placing the freeze-dried sample in a scanning electron microscope image shown in figure 1 and figure 2, wherein the internal structure is composed of cellulose nano-sheets and graphene oxide nano-sheets; as shown in figures 6-7, experiments are carried out under the condition of simulating a sunlight xenon lamp light source, and the illumination intensity is 1000W m -2 The evaporation rate of the catalyst reaches 2.3kg m -2 h -1 。
Example 3
22.5g of the aqueous cellulose solution prepared in example 1 and 5g of graphene oxide dispersion (2 mg mL) were weighed in a 50mL beaker -1 ) Ultrasonic treatment is carried out for 1h to ensure that the materials are uniformly mixed; filtering to obtain paste cake, placing in-18deg.C refrigerator, taking out after 24 hr, lyophilizing with a lyophilizing machine for 48 hr to remove water to obtain quinoa cellulose/graphene oxide aerogel, named SBA 5 。
Placing the freeze-dried sample in a scanning electron microscope image shown in figure 1 and figure 2, wherein the internal structure is composed of cellulose nano-sheets and graphene oxide nano-sheets; as shown in figures 6-7, experiments are carried out under the condition of simulating a sunlight xenon lamp light source, and the illumination intensity is 1000W m -2 The evaporation rate of the catalyst reaches 2.6kg m -2 h -1 。
Example 4
22.5g of the aqueous cellulose solution prepared in example 1 and 10g of graphene oxide dispersion (2 mg mL) were weighed in a 50mL beaker -1 ) Ultrasonic treatment is carried out for 1h to ensure that the materials are uniformly mixed; filtering to obtain paste cake, placing in-18deg.C refrigerator, taking out after 24 hr, lyophilizing with a lyophilizing machine for 48 hr to remove water to obtain quinoa cellulose/graphene oxide aerogel, named SBA 10 。
Placing the freeze-dried sample in a container as shown in the accompanying drawingsThe scanning electron microscope image shown in 1 is shown in figure 2, and the internal structure is composed of cellulose nano-sheets and graphene oxide nano-sheets; as shown in figures 6-7, experiments are carried out under the condition of simulating a sunlight xenon lamp light source, and the illumination intensity is 1000W m -2 The evaporation rate reaches 3.6kg m -2 h -1 The color of the sample under the irradiation of the light with the irradiation time was recorded with a camera, and as shown in fig. 3 to 4, the sample became dark black after 240 minutes under the combined stimulation of light and water, and became dark brown only in the presence of water. In addition, as shown in fig. 5, after 6h of 'water-light' stimulation, the absorption performance of quinoa cellulose/graphene oxide in the ultraviolet-visible-far infrared region is improved from 34.5% to 77.0%.
Example 5
The outdoor experimental device is shown in fig. 8, and is provided with SBA 10 Is placed in a transparent drum, is filled with about 200g of water and is placed on a roof, so that the evaporator is beneficial to solar irradiation all the day, and the placement time is 8:00 a.m. to 18 a.m.: 00, for a total of ten hours. Recording the initial evaporator mass (8:00) and the mass after the end of the experiment (18:00); simultaneously, the solar light intensity is recorded by an irradiator (recorded every 1 h) for evaluating the radiation intensity of the real sun; additionally record SBA during evaporation 10 In the case of surface crystallized salts, the experiment lasted for 15 days. As shown in FIG. 9, the average evaporation rates for deionized water and simulated seawater reached 12.6kg m for 15 days, respectively -2 day -1 And 12kg m -2 day -1 The requirements of 5-6 people on daily drinking water can be met; in addition, as shown in fig. 10, after the evaporator works for one day, a small amount of crystal salt is accumulated on the surface, and the accumulated crystal salt disappears in the morning for the next day, which indicates that the prepared quinoa cellulose aerogel has a good self-cleaning function, and the excellent self-cleaning function ensures that the evaporator has good durability and long-time high-performance evaporation performance. As shown in FIG. 11, SBA 10 After the evaporator processes the simulated seawater, the obtained water contains Na + 、K + 、Ca 2+ 、Mg 2+ From 11619,376.6,1203.2, 1052.8mg.L -1 Becomes 4.14,1.789,0.9489,0.0981mg·L -1 Meets the standard of safe drinking water.
What is not described in detail in the present specification belongs to the prior art known to those skilled in the art. While the foregoing describes illustrative embodiments of the present invention to facilitate an understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as protected by the accompanying claims insofar as various changes are within the spirit and scope of the present invention as defined and defined by the appended claims.
Claims (8)
1. The application of the self-darkening quinoa cellulose/graphene oxide aerogel is characterized in that:
under the combined stimulation of light and water, the aerogel can change from light brown to dark black, and the absorption of light is enhanced; the self-cleaning function is carried out on the crystallized salt with accumulated surface area under the condition of no illumination or weak illumination in the sea water desalting process; the weak illumination condition is that the illumination is less than 300W m -2 The method comprises the steps of carrying out a first treatment on the surface of the The self-cleaning function is specifically that under the condition of no or weak illumination, the crystal salt accumulated on the surface can be dissolved in the seawater body under the action of chemical potential; the time required for blackening is 30-240 min;
the preparation method of the self-darkening quinoa cellulose/graphene oxide aerogel comprises the following steps:
step 1, extracting quinoa cellulose;
step 2, preparing the quinoa cellulose extracted in the step 1 into quinoa cellulose aqueous dispersion;
step 3, adding graphene oxide dispersion liquid into the quinoa cellulose aqueous dispersion liquid, mixing to prepare a plurality of parts of composite liquid, uniformly mixing the plurality of parts of composite liquid by ultrasonic, filtering to form a paste cake, and freeze-drying to obtain quinoa cellulose/graphene oxide aerogel;
the step 1 of extracting quinoa cellulose further comprises the following steps:
step 1.1, crushing and sieving quinoa skin, collecting powder, and drying to obtain quinoa skin powder;
step 1.2, extracting quinoa peel powder with benzene/ethanol solution to obtain a first extract;
step 1.3 subjecting the first extract to NaClO 2 Heating and stirring the solution, regulating pH with acetic acid, suction filtering, washing with distilled water to neutrality to obtain second extract;
step 1.4, heating and stirring the second extract by using NaOH solution, and carrying out suction filtration, wherein the filtrate is washed by distilled water to be not alkaline, so as to obtain a suction filtration filter cake;
and 1.5, heating the filter cake subjected to suction filtration by using an HCl solution, performing suction filtration, washing to be neutral by using distilled water, drying and crushing.
2. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: the number of the crushed screening meshes in the step 1.1 is 80 meshes; the drying temperature in the step 1.1 is 60 ℃ and the drying time is 12h.
3. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: the device extracted in the step 1.2 is a Soxhlet extractor; in the step 1.2, the relation between quinoa flour and benzene/ethanol solution is that 150-250 mL benzene/ethanol solution with the volume ratio of 2:1 is selected for extraction every 60g quinoa flour; the extraction temperature in the step 1.2 is 85-95 ℃ and the extraction time is 12h.
4. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: naClO in step 1.3 2 The mass fraction of the solution is 1-5%, the pH is specifically adjusted by acetic acid with the concentration of 5% by acetic acid=4-5, the temperature of heating and stirring treatment is 75 ℃, and the stirring treatment time is 1.5h; the stirring operation in the step 1.3 adopts a heat collection type magnetic stirrer.
5. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: in the step 1.4, the mass fraction of the NaOH solution is 1-10%, the heating temperature of the heating and stirring treatment is 85-95 ℃, and the stirring treatment time is 1.5-h.
6. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: the mass fraction of the HCl solution in the step 1.5 is 1-5%, the temperature of the heating treatment is 70-90 ℃, the time of the heating treatment is 2h, the temperature of the drying is 60 ℃, and the drying time is 24-h.
7. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: the mass fraction of the quinoa cellulose aqueous dispersion liquid in the step 2 is 0.5-5%; the specific method for preparing the quinoa cellulose aqueous dispersion liquid in the step 2 comprises the following steps: treatment with a cantilever high speed disperser 1h followed by additional sonication 1h is repeated 5-10 times until a uniform suspension is formed.
8. The use of a self-darkening quinoa cellulose/graphene oxide aerogel according to claim 1, characterized in that: the graphene oxide content in the multiple parts of composite liquid in the step 3 is 2.5wt%, 5wt% and 10wt% respectively; the concentration of the graphene oxide dispersion liquid in the step 3 is 2mg mL -1 The method comprises the steps of carrying out a first treatment on the surface of the The ultrasonic time for ultrasonic mixing in the step 3 is 1h.
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| CN109925746A (en) * | 2019-04-02 | 2019-06-25 | 福建农林大学 | A kind of water-oil separating automatically cleaning alginic acid alkali composite titanium dioxide aerogel material and preparation method thereof |
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