CN111252836B - GSP film material for solar photo-thermal steam conversion and preparation method thereof - Google Patents
GSP film material for solar photo-thermal steam conversion and preparation method thereof Download PDFInfo
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Images
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- 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
- C02F1/14—Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- 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
- C02F1/043—Details
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- 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
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F22—STEAM GENERATION
- F22B—METHODS OF STEAM GENERATION; STEAM BOILERS
- F22B1/00—Methods of steam generation characterised by form of heating method
- F22B1/006—Methods of steam generation characterised by form of heating method using solar heat
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
- F24S70/00—Details of absorbing elements
- F24S70/10—Details of absorbing elements characterised by the absorbing material
- F24S70/12—Details of absorbing elements characterised by the absorbing material made of metallic material
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- C02F2103/08—Seawater, e.g. for desalination
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Abstract
The invention relates to a preparation method of GSP film material for solar photo-thermal steam conversion in the technical field of energy materials, which comprises the steps of dispersing organic silicon powder in water, adding chloroauric acid solution, carrying out ultrasonic reaction to obtain gold-complexed organic silicon spheres, freezing by liquid nitrogen, carrying out vacuum drying to obtain gold-complexed organic silicon sphere powder, calcining the gold-complexed organic silicon sphere powder at the temperature of 500-1000 ℃ under the protection of protective gas to obtain gold nanoparticle-doped carbonized organic silicon sphere powder, dispersing the gold-nanoparticle-doped carbonized organic silicon sphere powder in water, dripping the gold-doped carbonized organic silicon sphere powder on fiber filter paper, carrying out vacuum filtration to obtain the GSP film material, wherein the GSP film material prepared by the invention has the advantages that the sunlight is fully absorbed by the surface plasmon effect generated by the irradiation of the sunlight, and the GSP film material has better heat conduction effect due to lower heat conductivity coefficient and higher heat diffusion coefficient, the heat loss in the heat transfer process is reduced, so that the GSP film material has a faster water evaporation rate.
Description
Technical Field
The invention relates to the technical field of energy materials, in particular to a preparation method of a GSP (glutathione-p) film material applied to solar photo-thermal steam conversion.
Background
Water resources are related to human health and the future, but with the development of economy and industry, the problems of water pollution and water resource shortage are increasingly serious, the current state is continued, and more than two thirds of people on the earth face the problem of water resources in the future, so that the treatment and reutilization of wastewater or the desalination of seawater are always researched and hot spots for human use. Solar energy has been always noticed by human as a renewable, clean and pollution-free resource, is widely used for wastewater treatment, seawater desalination, sterilization, catalysis and other aspects, and has a very wide application prospect.
However, the technology applied to the solar steam conversion is not mature at present, and the solar energy is not fully utilized due to the large photothermal conversion loss, so that the popularization and the expansion of the solar energy on the technology are limited to a great extent, and therefore, finding a suitable sunlight absorber to reduce the heat loss and improve the conversion rate becomes the breakthrough point of the current technology.
Disclosure of Invention
The invention solves the problems of low sunlight absorption rate and low photo-thermal conversion efficiency of the technical material, and designs and prepares the method for preparing the photo-thermal conversion absorber GSP film material with small optical loss and high solar photo-thermal conversion efficiency.
The invention aims to realize the preparation method of the GSP film material for solar photo-thermal steam conversion, which comprises the following steps:
1) preparing gold complex organic silicon balls: uniformly dispersing the organic silicon powder in water, adding chloroauric acid solution, carrying out ultrasonic reaction until the color does not change, centrifugally collecting precipitate, freezing by using liquid nitrogen, and carrying out vacuum drying to obtain gold-complexed organic silicon pellet powder;
2) preparing gold nanoparticle-doped carbonized organic silicon pellets: calcining the gold complex organic silicon pellet powder prepared in the step 1) for 6-10 h at the temperature of 500-1000 ℃ under the protection of protective gas to obtain gold nanoparticle doped carbonized organic silicon pellet powder;
3) preparing a GSP membrane material: uniformly dispersing the gold nanoparticle doped carbonized organic silicon pellet powder prepared in the step 2) in water, then placing fiber filter paper in a Buchner funnel, performing vacuum filtration, uniformly dripping the gold nanoparticle doped carbonized organic silicon pellet powder dispersion liquid on the fiber filter paper, and performing vacuum filtration for 10-30 min to obtain the GSP membrane material.
The method comprises the steps of taking water as a medium, uniformly dispersing organic silicon powder in the water, adding a chloroauric acid aqueous solution, replacing the position of H in-SH in organic silicon with gold in the chloroauric acid under the energy vibration of ultrasonic waves to obtain gold-complexed organic silicon spheres, calcining the gold-complexed organic silicon spheres at 500-1000 ℃, carbonizing organic elements in the gold-complexed organic silicon spheres, reducing the complexation of Au and S in the gold-complexed organic silicon spheres to form gold nanoparticles, obtaining gold nanoparticle-doped carbonized organic silicon spheres, uniformly dispersing the gold nanoparticle-doped carbonized organic silicon spheres on Fiber Filter Paper (FFP), performing vacuum filtration to remove excessive water, uniformly dispersing the gold nanoparticle-doped carbonized organic silicon spheres on the fiber, and enabling a certain vacuum effect to serve as a weak bonding effect, the small balls are not easy to fall off, and finally the fiber filter paper coated with the gold nanoparticle doped carbonized organic silicon small balls, namely the GSP membrane material is obtained.
Further, the step 1) specifically comprises the following steps:
1.1) when preparing organosilicon powder, uniformly dispersing gamma-mercaptopropyl trimethoxysilane in water, preparing a gamma-mercaptopropyl trimethoxysilane solution with the concentration of 0.8-10 mg/mL, adding ammonia water to adjust the pH value of the solution to 9-11, hydrolyzing for 10-24 h, centrifuging at the rotating speed of 3000-5000 rpm to remove supernatant, adding deionized water, washing for 1-5 times, freezing by using liquid nitrogen, and drying in vacuum to obtain organosilicon powder; in the invention, the gamma-mercaptopropyl-trimethoxysilane generates organic silicon by hydrolysis reaction under alkaline condition; the reaction process is as follows:
1.2) uniformly dispersing the purchased or prepared organosilicon powder in the step 1.1) in water, preparing organosilicon dispersion liquid with the concentration of 10-100 mg/mL, then adding chloroauric acid solution with the concentration of 0.25 mol/L, performing ultrasonic treatment until the color of the solution is not changed, centrifuging to remove supernatant, freezing by using liquid nitrogen, performing vacuum drying, and then obtaining gold-complexed organosilicon pellet powder; in the invention, gold in the chloroauric acid solution replaces H on-SH in the organic silicon globule to form Au (I) -S bond under the energy of ultrasonic vibration, so as to obtain the gold-complexed organic silicon globule.
Further, the step 3) specifically comprises the following steps:
3.1) dispersing the gold nanoparticle doped carbonized organic silicon beads prepared in the step 2) into water, uniformly dispersing by ultrasonic, and preparing a gold nanoparticle doped carbonized organic silicon bead dispersion liquid with the concentration of 0.5-2 mg/mL;
3.2) laying 4-6 double-ring qualitative filter paper on a Buchner funnel, cutting the fiber filter paper according to the specification of the Buchner funnel, putting the fiber filter paper into the Buchner funnel, laying the cut fiber filter paper on the upper side of the double-ring qualitative filter paper, carrying out vacuum filtration under the condition that the pressure of a vacuum pump is 0.05-0.1 Mpa, uniformly dripping the gold nanoparticle-doped carbonized organosilicon pellet dispersion liquid dispersed in the step 3.1) on the fiber filter paper, and continuing the vacuum filtration for 10-30 min to obtain the GSP membrane material.
Further, in the step 1.2), the mass ratio of the gold in the chloroauric acid to the organosilicon pellet powder is 1: 1-10.
Further, in the step 1.1) and the step 1.2), the vacuum drying condition is that the pressure of 10-100 Pa acts for 12-24 hours.
Further, the protective gas is argon, helium or nitrogen.
The GSP membrane material prepared by the method is used for solar photothermal steam conversion, the gold nanoparticles are doped with the uniform black carbonized organic silicon spheres, the surface plasmon effect excited by the gold nanoparticles with low surface sizes under the irradiation of light improves the sunlight absorption rate of the GSP membrane material, and the fiber filter paper is used as a support body and has good toughness and filtration water permeability, so that the light absorption capacity of the GSP membrane material is improved, the heat transfer effect is improved due to lower heat conductivity and higher heat diffusion coefficient, and the photothermal conversion efficiency is further improved.
Drawings
Fig. 1 is an SEM image of gold complex silicone globules.
Fig. 2 is an SEM image of gold nanoparticle doped silicon carbide.
Fig. 3 is an SEM image of the fibrous filter paper.
Fig. 4 is an SEM image of the GSP membrane material.
Fig. 5 is a front view of a GSP film material.
Fig. 6 is a side view of a GSP film material.
Figure 7 is a TEM image of gold complexed silicone beads.
Fig. 8 is a Mapping plot of gold complexed silicone beads.
Fig. 9 is a TEM image of gold nanoparticle doped carbonized silicone pellets.
Fig. 10 is a Mapping diagram of gold nanoparticle doped carbonized silicone pellets.
Fig. 11 is a lattice diagram of gold nanoparticles in gold nanoparticle doped carbonized silicone spheres.
Fig. 12 is an X-ray diffraction pattern (XRD) of gold nanoparticle-doped silicon carbide pellets.
Fig. 13 is a total high power X-ray photoelectron spectrum (XPS) of silicone beads and gold-complexed silicone beads.
FIG. 14 is a high power X-ray photoelectron spectroscopy (XPS) of Au elements in silicone pellets and gold-complexed silicone pellets.
Fig. 15 is a high power X-ray photoelectron spectrum (XPS) of the Au element in gold-complexed organosilicon spheres and gold nanoparticle-doped carbonized organosilicon spheres.
Fig. 16 is a uv-visible diffuse reflectance spectrum of the FFP film, SP film, GSP film material, and gold nanoparticle doped silicon carbide.
Fig. 17 is an infrared spectrum of silicone pellets, gold-complexed silicone pellets, and gold nanoparticle-doped carbonized silicone pellets.
Fig. 18 is a graph of thermal conductivity and thermal diffusivity for wetted and dried GSP membrane materials.
Fig. 19 is a graph showing the temperature of the upper surfaces of pure water, an FFP film, an SP film, and a GSP film material as a function of time under one solar radiation.
Fig. 20 is a graph of the upper surface temperature of the GSP film material in air as a function of time under one solar radiation.
Fig. 21 is a graph of temperature of gold nanoparticle-doped carbonized silicone pellets and graphite in air and water as a function of time under solar radiation.
Fig. 22 shows the evaporation rate and thermal conversion efficiency of pure water, FFP film, SP film, and GSP film material under one sun irradiation.
Fig. 23 is the dye concentration before and after the GSP film material was used for solar water purification.
Fig. 24 is the heavy metal ion concentration before and after the GSP membrane material was used for solar water purification.
Fig. 25 is the ion concentration in seawater before and after the GFP membrane was used for solar water purification.
FIG. 26 is a graph of evaporation rate versus time for GSP membrane material in purifying seawater under one solar radiation.
Fig. 27 is a TEM image of gold nanoparticle-doped carbonized organosilicon spheres with GSP membrane material used for seawater purification cycle recycling.
Fig. 28 shows that the evaporation rate of the GSP film material and the GSP film material prepared by cyclically recycling gold nanoparticle-doped silicon carbide changes with time under one solar radiation.
Fig. 29 is a statistical distribution graph of the particle size of the silicone beads.
Fig. 30 is a statistical distribution diagram of the particle size of gold nanoparticle doped carbonized silicone beads.
Fig. 31 is a statistical distribution graph of gold nanoparticles in gold nanoparticle doped carbonized silicone spheres.
Fig. 32 is a statistical distribution diagram of the particle size of gold nanoparticles doped with silicon carbide after recycling.
Fig. 33 is an isothermal adsorption desorption curve (BET) of silicone pellets and gold nanoparticles doped with silicone carbide.
Detailed Description
The present invention is further analyzed, illustrated and compared by the following specific examples and comparative examples.
Example 1
(1) Taking 0.5g of gamma-mercaptopropyl trimethoxy silane in 200mL of water, mechanically stirring at 200 rpm until the solution is clear and transparent, then adjusting the pH to be about 9 by using ammonia water, continuously mechanically stirring for 12 hours until the solution is changed from a transparent solution to a milky solution, then centrifuging at 3000 rpm to remove a supernatant, adding deionized water to wash for 5 times, freezing by using liquid nitrogen at-196 ℃, and drying for 24 hours under the vacuum condition of 10 Pa to obtain white organic silicon pellet powder for later use;
(2) 0.5g of organic silicon pellets are weighed, evenly dispersed in 50mL of water by ultrasonic, and then 100 mu L of 0.25 mol L of organic silicon pellets are added under the ultrasonic state-1Carrying out ultrasonic reaction on the solution until the color does not change any more, then centrifuging at the rotating speed of 3000 rpm to remove supernatant, and drying for 12 hours under the vacuum condition of 10 Pa to obtain gold-complexing organic silicon small ball powder;
(3) placing the gold complex organosilicon pellet powder in a quartz boat, placing in a tube furnace, and protecting with high-purity argon gas at 5 deg.C for 5 min-1Heating to 800 ℃ and calcining for 6 h at high temperature to obtain gold nanoparticle doped carbonized organic silicon pellet powder;
(4) weighing 50 mg of gold nanoparticle-doped carbonized organic silicon bead powder, ultrasonically dispersing the powder in 80 mL of water, paving 4 double-circle qualitative filter papers on a Buchner funnel, cutting a Fiber Filter Paper (FFP) according to the specification of the Buchner funnel, putting the fiber filter paper into the Buchner funnel, paving the cut fiber filter paper on the upper side of the double-circle qualitative filter paper, performing vacuum filtration under the condition that the pressure of a vacuum pump is 0.05Mpa, slowly and uniformly dripping the gold nanoparticle-doped carbonized organic silicon bead dispersion liquid on the fiber filter paper by using a disposable dropper, performing the vacuum filtration while dripping the dispersion liquid so as to remove excessive moisture in time, continuing the vacuum filtration for 30min after the dripping is finished, and finally obtaining a GSP membrane material.
Comparative example 1
(1) Taking 0.5g of gamma-mercaptopropyl trimethoxy silane in 200mL of water, magnetically stirring at the stirring speed of 500 rpm until the solution is clear and transparent, then adjusting the pH to be about 9 by using ammonia water, continuously magnetically stirring for 12 hours, changing the solution from the transparent solution into a milky solution, then centrifuging at the rotating speed of 3000 rpm to remove a supernatant, adding deionized water to wash for 5 times, freezing by using liquid nitrogen at the temperature of-196 ℃, and drying for 24 hours under the vacuum condition of 10 Pa to obtain white organic silicon pellet powder for later use;
(2) placing the organosilicon pellet powder in a quartz boat, and then protecting the quartz boat in a tube furnace with high-purity argon gas for 5 ℃ min-1Heating to 800 ℃, calcining for 6 h at high temperature, and finally obtaining carbonized organic silicon pellet powder;
(3) weighing 50 mg of carbonized organosilicon pellet powder, ultrasonically dispersing the carbonized organosilicon pellet powder in 80 mL of water, laying 4 pieces of double-circle qualitative filter paper on a Buchner funnel, cutting the fiber filter paper according to the specification of the Buchner funnel, putting the fiber filter paper into the Buchner funnel, laying the cut fiber filter paper on the upper side of the double-circle qualitative filter paper, performing vacuum filtration under the condition that the pressure of a vacuum pump is 0.05Mpa, slowly and uniformly dripping the fiber filter paper by using a disposable dropper on the fiber filter paper, dripping and performing the vacuum filtration while coating so as to remove redundant moisture in time, continuing the vacuum filtration for about 30min after dripping is completed, and finally obtaining the fiber filter paper coated with the carbonized organosilicon pellet, namely an SP (SP) film.
Application example 1
Taking four quartz beakers, cutting three pieces of heat insulation foam with the same diameter as the quartz beakers to enable the heat insulation foam to be clamped on the beakers and not to freely move without external force, cutting two rectangular holes with the specification of 2mm multiplied by 3.5 cm on the heat insulation foam, enabling two holes to be parallel and spaced by 4 cm, then enabling cotton cloth capable of conveying water to pass through the two holes, keeping two ends long, then injecting 100 mL of water into the three quartz beakers, respectively clamping the three pieces of heat insulation foam on the three quartz beakers, keeping a section of air column with the water surface, playing the same heat insulation effect, keeping two ends of the cotton cloth just deep into the water, continuously conveying a water source in the quartz beakers to the cotton cloth on the surface of each piece of heat foam under the action of capillary force, respectively cutting fiber filter paper, the GSP film prepared in example 1 and the SP film prepared in comparative example into the specification of 3.5 cm multiplied by 4 cm, and enabling black surfaces of the GSP film material prepared in example 1 and the SP film material prepared in comparative example 1 to face upwards, pure fiber filter paper, the GSP membrane material prepared in example 1 and the SP membrane material prepared in comparative example 1 were placed on the upper side of cotton cloth, three sets of evaporators were made by the user to purify water, and a thermal insulation foam was not placed on the fourth quartz beaker to serve as a blank control.
The indoor environment is room temperature and the humidity is 65%, and the relative steady state is maintained through an air conditioner and a dehumidifier. The light intensity of the xenon lamp was adjusted to 100 mW cm by means of a light power densitometer with the addition of an AM1.5G filter-2The change in weight of water was measured with a balance of 0.1 mg by weight.
First, the water of the blank control group is evaporated, and the light intensity is 100 mW cm-2The mass change of the quartz beaker within 1 h was measured by a weight meter under the light intensity of (1), and the photothermal steam conversion efficiency was calculated. At the same 100 mW cm-2Under irradiation, the mass change of three groups of evaporators within 1 h was measured by weight, and the photothermal steam conversion efficiency was calculated. As a result of statistics, as shown in FIG. 22, the evaporation rate of pure water was 0.39 kg m-2 h-1The photothermal steam conversion efficiency was 26.62%, and the evaporation rates of the fiber filter paper, the GSP film material and the SP film material were 0.47 kg m, respectively-2 h-1，1.11 kg m-2 h-1，1.5 kg m-2 h-1The conversion efficiency of light, heat and steam is 21.9%, 70% and 94.6% respectively.
Application example 2
Three quartz beakers are taken, and three pieces of heat insulation foam with the same diameter as the quartz beakers are cut, so that the heat insulation foam can be clamped on the beakers and cannot move freely without external force. Two rectangular holes with the specification of 2mm multiplied by 3.5 cm are cut on the heat insulation foam, the two holes are parallel and are 4 cm away, then cotton cloth capable of conveying water penetrates through the two holes, the two ends of the cotton cloth are kept long, 100 mL of methylene blue with the concentration of 100 ppm, rhodamine B and methyl orange dye are respectively placed in three quartz beakers, the three heat insulation foams are respectively clamped on the quartz beakers, a section of air column is kept between the three heat insulation foams and the water surface, the heat insulation effect is also achieved, the two ends of the cotton cloth are just long enough to penetrate into the water, then a water source in the quartz beakers is continuously conveyed to the cotton cloth on the surface of each hot foam under the action of capillary force, the application example 1 shows that the evaporation efficiency of the GSP film material is the highest, three films with the specification of 3.5 cm multiplied by 4 cm are cut from the GSP film material prepared in the example 1, the three self-made evaporators are respectively formed by carefully placing the three cotton cloths on the upper sides, and (4) carrying out dye degradation.
Placing the three groups of evaporators in a transparent closed collecting container at a concentration of 100 mW cm-2Under the irradiation of light intensity, evaporating solutions are respectively collected, and then the concentration of the evaporated evaporating solutions is measured by liquid chromatography to obtain the degradation efficiency. The concentration of the evaporated solution (as shown in fig. 23) and the degradation rate result are respectively 0.1 ppm and 99.9% of methylene blue; rhodamine B0.26 ppm, 99.74%; methyl orange 0.32 ppm, 99.68%.
Application example 3
Three quartz beakers are taken, and three pieces of heat insulation foam with the same diameter as the quartz beakers are cut, so that the heat insulation foam can be clamped on the beakers and cannot move freely without external force. Cutting two rectangular holes with specification of 2mm × 3.5 cm on the heat insulation foam, wherein the two holes are parallel and have a distance of 4 cm, then passing cotton cloth capable of conveying water through the two holes, keeping the two ends long, and selecting three typical heavy metal ions Cr2+，Pb2+，Cd2+As an experimental subject, 100 mL of Cr was prepared from chromium acetate, lead acetate and cadmium acetate2+，Pb2+，Cd2+The solution with the ion concentration of 100 ppm is respectively added into three quartz beakers, three heat insulation foams are respectively clamped on the three quartz beakers, a section of air column is reserved on the water surface, the same heat insulation effect is achieved, two ends of the cotton cloth are just long enough to penetrate into water, then the solution in the quartz beakers is continuously conveyed to the cotton cloth on the surface of the heat foams under the action of capillary force, similarly, the application example 1 shows that the evaporation efficiency of the GSP film material is the highest, three films with the specification of 3.5 cm multiplied by 4 cm are cut out from the GSP film material prepared in the example 1, the three films are respectively carefully placed on the upper sides of the three cotton cloths to form three groups of self-made evaporators, and heavy metal ions are removed.
Also in the same manner as in application example 2, three sets of self-made evaporators were each placed in a transparent closed vessel at 100 mW cm-2Collecting the evaporated solution under light intensity, measuring the concentrations of the metal stock solution and the ions in the collected evaporated solution by inductively coupled plasma emission spectroscopy (ICP) (as shown in FIG. 24), and calculating the removal rate, wherein the specific results are as follows, respectively, for Cr2+104.2 ppm of stock solution, 46.58 ppb of evaporated solution and 99.96 percent of removal rate; pb2+100.1 ppm of stock solution, 6.14 ppb of evaporated solution, 99.99% of removal rate and Cd2+104.8 ppm of stock solution, 2.02 ppb of evaporated solution and 99.99 percent of removal rate.
Application example 4
A quartz beaker is taken, and a piece of heat insulation foam with the same diameter as the quartz beaker is cut, so that the quartz beaker can be clamped on the beaker and can not move freely without external force. Cutting two rectangular holes on heat insulation foam, wherein the specification is 2mm multiplied by 3.5 cm, the two holes are parallel and are 4 cm apart, then enabling cotton cloth capable of conveying water to penetrate through the two holes, keeping two long ends, then injecting 100 mL of water into a beaker, clamping the whole heat insulation foam on a quartz beaker, keeping a section of air column with the water surface, playing the same heat insulation effect, keeping two long ends of the cotton cloth right to penetrate into the water, then continuously conveying a water source in the quartz beaker onto the cotton cloth on the surface of hot foam under the action of capillary force, and similarly, knowing from an application example 1, the GSP film material has the highest evaporation efficiency, preparing 500 mL of artificial seawater according to the American energy department seawater standard for standby, specifically Na is used for standby+ 10.78 g L-1，Mg2+ 1.28 g L-1，Ca2+ 0.4 g L-1，K+ 0.41 g L-1Similarly, the GSP film material prepared in example 1 was cut into a film with a specification of 3.5 cm × 4 cm, and the cut GSP film material was placed on cotton cloth to form a home-made evaporator for seawater desalination and evaporation.
Similar to application example 2 and application example 3, the whole homemade evaporator was placed in a closed transparent container at 100 mW cm-2The ICP test was performed with continuous irradiation under light intensity to collect the evaporated solution and the removal rate was calculated. The specific result is (as shown in FIG. 25) Na+The concentration of the stock solution is 10860 ppm, the concentration of the evaporated solution is 0.7217 ppmThe removal rate is 99.99 percent; mg (magnesium)2+The concentration of the stock solution is 1581 ppm, the concentration of the evaporated solution is 0.1909 ppm, and the removal rate is 99.99 percent; ca2+The concentration of the stock solution is 431.6 ppm, the concentration of the evaporated solution is 0.5517 ppm, and the removal rate is 99.87%; k+The concentration of the stock solution is 406.6 ppm, the concentration of the evaporated solution is 0.218 ppm, and the removal rate is 99.95%.
In order to verify the durability of the GSP membrane material, a simulated seawater evaporation cycle experiment was performed. The specific operation is as follows, 200mL of prepared artificial seawater is added into a self-made evaporator, and then the mixture is added at 100 mW cm-2Continuously irradiating for 12 h under the light intensity irradiation, recording the weight change of each hour by using a weight meter (as shown in figure 26), observing the lasting durability of the GSP film material, continuously repeating the experiment for 5 days, recording the state change of the film by using a professional camera before and after each day, and confirming that the lasting durability of the film is good after five days, taking the data as an example, the distilled water amount of 12 h per day for 5 days continuously is respectively: 17.4913 kg m-2，17.43119 kg m-2，17.38066 kg m-2，16.98577 kg m-2，16.67215 kg m-2Through five-day cycle experiments, the distilled water amount per hour and the total distilled water amount per continuous day for 12 hours do not fluctuate too much, and the GSP film material is good in durability.
In order to verify the reusability of the gold nanoparticle-doped organic silicon carbide pellets, after five continuous seawater evaporation cycle experiments, the gold nanoparticle-doped organic silicon carbide pellets coated on the GSP membrane material are recovered by a simple ultrasonic method, and after simple washing and freeze-drying treatment, the morphology size and the size of the gold nanoparticles are not changed (as shown in fig. 27 and 32).
FIG. 1 is an SEM image of gold complex silicone pellets prepared in example 1, the pellets having a uniform particle size distribution of about 500 nm.
Fig. 2 is an SEM image of gold nanoparticle-doped silicon carbide pellets prepared in example 1, the pellets having a uniform particle size distribution of about 400 nm.
FIG. 3 is an SEM image of a fibrous filter paper having, on a microscopic scale, interstitial pores between the fibrous filter paper that facilitate water evaporation.
Fig. 4 is an SEM image of the GSP film material in example 1, where the gold nanoparticle-doped carbonized organosilicon spheres are distributed on the fiber filter paper, which further shows the uniformity of the particle size distribution of the prepared gold nanoparticle-doped carbonized organosilicon spheres.
Fig. 5 is a front view of the GSP film material prepared in example 1, which is black.
Fig. 6 is a reverse image of the GSP membrane material prepared in example 1, which is relatively lighter in color than the front image of fig. 5, because the gold nanoparticle carbonized silicone beads are distributed on only one side of the fibrous filter paper.
Fig. 7 is a TEM image of the gold complex silicone bead prepared in example 1, and it can be seen from a combination of fig. 7 (a) and 7 (b) that the bead has a particle size of about 500 nm and a uniform particle size distribution.
FIG. 8 is a Mapping chart of the gold complex silicone beads prepared in example 1, containing elements of C, O, S, Si, Au.
Fig. 9 is a TEM image of gold nanoparticle-doped silicon carbide pellets prepared in example 1, the pellets having a particle size of about 400 nm and a uniform particle size distribution.
FIG. 10 is a Mapping chart of gold nanoparticle doped carbonized silicone beads prepared in example 1, containing C, O, S, Si, Au as elements.
Fig. 11 is a crystal lattice diagram of gold nanoparticles in gold nanoparticle-doped silicon carbide pellets prepared in example 1, wherein the crystal plane type is 111 planes, and the crystal lattice is 0.235 nm.
Fig. 12 is an XRD diffractogram of the gold nanoparticle-doped silicon carbide pellets prepared in example 1, which correspond to silica 200, C110, Au 111, Au 200, and Au 220 at 13.891 °, 29.705 °, 38.184 °, 44.392 °, 64.576 °, respectively.
FIG. 13 is an X-ray photoelectron Spectroscopy XPS analysis of the silicone pellets and gold-complexed silicone pellets prepared in example 1, the silicone pellets containing the elements C, O, S, Si; the gold complex organic silicon globule contains elements C, O, S, Si and Au.
FIG. 14 is an X-ray photoelectron spectroscopy XPS analysis of Au in silicone pellets prepared in example 1 and gold-complexed silicone pellets, in which no Au element is contained, showing 88.4 eV and 84.7 eV signals in the Au4f orbital, while standard Au signals are at 87.7 eV and 84.0 eV, confirming that the Au is not a Au nanoparticle but exists in the form of Au (I) -S bond.
Fig. 15 is an X-ray photoelectron spectroscopy XPS analysis of Au in the gold-complexed silicone beads and the gold nanoparticle-doped carbonized silicone beads prepared in example 1, and the Au4f signal in the gold nanoparticle-doped carbonized silicone beads was 87.7 eV and 84.0 eV, respectively, relative to the signal of Au in the gold-complexed silicone beads in fig. 14, further confirming the presence of the gold nanoparticles.
Fig. 16 is uv-visible diffuse reflectance spectra of fiber filter paper FFP, gold nanoparticle-doped carbonized silicone pellets prepared in example 1, GSP film material, and SP film prepared in comparative example 1. Compared with an FFP (flexible flat panel) membrane, an SP (SP) membrane and gold nanoparticles doped with carbonized organic silicon pellets, the GSP membrane material can absorb about 95% of sunlight within the range of 200-2500 nm, and the improvement of the photo-thermal steam conversion efficiency is greatly promoted.
FIG. 17 is a Fourier transform infrared spectroscopy analysis of the silicone beads, gold complexed silicone beads and gold nanoparticle doped carbonized silicone beads prepared in example 1, with the-SH signal appearing at 2551 cm-1The signal of the organic silicon globule is strongest, and the-SH signal is weakened because Au is complexed with S in the gold-complexing organic silicon globule; as the gold nanoparticles are formed by carbonization, the-SH signals in the gold nanoparticle-doped carbonized organic silicon spheres disappear. -CH2The signal appears at 2928 cm-1The same disappears in the gold nanoparticle-doped carbonized silicone globules due to carbonization, as in the presence of the silicone globules and the gold-complexed silicone globules.
Fig. 18 is a graph showing thermal conductivity and thermal diffusivity of the GSP film material prepared in example 1 in a wet state and a dry state. As can be seen from the figure, the dry GSP membrane material has a lower thermal conductivity and a high thermal diffusivity compared to the GSP membrane material in the wet state, which indicates that the dry GSP membrane material has a better heat transfer effect relative to the wet GSP membrane material, and is consistent with the results of fig. 19 and 20.
FIG. 19 shows pure H2O, fiber Filter paper FFP and GSP film prepared in example 1 and SP film prepared in comparative example 1 were at 100 mW cm-2The temperature change curve of the inner membrane surface layer within 1 h under the irradiation of light intensity has the fastest heating rate of the GSP membrane material within the same time, and can be kept stable at the highest temperature of about 47 ℃, which is beneficial to water evaporation.
FIG. 20 shows the GSP membrane material prepared in example 1 at 100 mW cm in air-2The temperature change of the inner surface is 1 h under the irradiation of the light intensity, and finally the temperature is stable at about 64 ℃ after the rapid heating process.
FIG. 21 shows graphite, carbonized silicone pellets, and SP film and graphite/fiber filter paper prepared in comparative example 1 in air and water at 100 mW cm, respectively-2Surface temperature profile over 1 h.
FIG. 22 shows the thickness of each film in application example 1 at 100 mW cm-2The evaporation rate and the thermal efficiency of water under the irradiation of light intensity. Pure H2O, FFP film, SP film and GSP film are respectively as follows: 0.39, 26.62%; 0.47, 21.9%, 1.11; 70 percent; 1.5, 94.6 percent.
FIG. 23 is a comparison of the dye concentrations in application example 2, wherein the concentrations of methylene blue, rhodamine B and methyl orange are as follows: 100 ppm, 0.32 ppm; 100 ppm, 0.26 ppm; 100 ppm, 0.1 ppm.
FIG. 24 is a comparison of the concentrations of heavy metal ions before and after application example 3, Cr2+，Pb2+，Cd2+The ion concentrations before and after evaporation are respectively: 104.2 ppm, 46.58 ppb; 100.1 ppm, 6.14 ppb; 104.8 ppm, 2.02 ppb.
FIG. 25 is a comparison of sea water evaporating ions before and after in application example 4, Na+，K+，Mg2+，Ca2+The ion concentrations before and after evaporation are respectively: 10860 ppm, 0.7217 ppm; 406.6 ppm, 0.218 ppm; 1581 ppm, 0.1909 ppm; 431.6 ppm and 0.5517 ppm.
Fig. 26 is a graph showing sea water circulation in application example 4, wherein the evaporation rate of the GSP film material remained substantially constant for 5 consecutive days of 12 h cycles, and did not decrease slightly until the fifth day, indicating that the GSP film material had durability.
Fig. 27 is a TEM image of gold nanoparticle-doped carbonized silicone pellets on the GSP film material recovered after seawater circulation in application example 4, in which the particle size is about 400 nm and the morphology is unchanged from that before circulation, which shows that the gold nanoparticle-doped carbonized silicone pellets have good stability.
FIG. 28 shows GSP membrane material prepared from SiC pellets obtained by recycling gold nanoparticles after seawater circulation in example 4 at a concentration of 100 mW cm-2The water evaporation rates under the light intensity irradiation are compared, and the comparison is unchanged, which shows that the gold nanoparticle doped silicon carbide pellet has reusability.
FIG. 29 is a statistical graph of the particle size of the silicone beads prepared in example 1, with a uniform particle size distribution, mostly between 500-510 nm.
FIG. 30 is a particle size statistical chart of the gold nanoparticle-doped silicon carbide pellets prepared in example 1, wherein the particle size distribution is uniform, and most of the particle sizes are 390-400 nm.
Fig. 31 is a particle size statistical chart of gold nanoparticles in the gold nanoparticle-doped organic silicon carbide pellet prepared in example 1, where the particle size distribution of the gold nanoparticles is uniform, and most of the gold nanoparticles are between 3.9 nm and 4.1 nm.
Fig. 32 is a distribution diagram of the particle size of the gold nanoparticles in the recovered gold nanoparticles doped with the carbonized organosilicon spheres after the seawater circulation in application example 4, where the particle size distribution of the gold nanoparticles is uniform and nearly consistent with the particle size distribution of the gold nanoparticles shown in fig. 31 before the seawater circulation, and further illustrates that the stability of the gold nanoparticles doped with the carbonized organosilicon spheres is good.
FIG. 33 is a surface area (BET) analysis of silicone pellets and gold nanoparticle doped carbonized silicone pellets prepared in example 1, the silicone pellets having a surface area of 3.14 m2 g-1The surface area of the gold nanoparticle-doped carbonized organic silicon globule is 5.24 m2 g-1The particles of gold nano-particles doped with carbonized organic silicon globules are provedThe grain diameter is larger than that of the organic silicon pellets.
Claims (6)
1. The preparation method of the GSP membrane material for solar photothermal steam conversion is characterized by comprising the following steps of taking fiber filter paper as a support body, coating gold nanoparticle-doped carbonized organic silicon beads on the surface layer of the fiber filter paper, and finally forming the GSP membrane material:
1) preparing gold complex organic silicon balls: uniformly dispersing the organic silicon powder in water, adding chloroauric acid solution, carrying out ultrasonic reaction until the color does not change, centrifugally collecting precipitate, freezing by using liquid nitrogen, and carrying out vacuum drying to obtain gold-complexed organic silicon pellet powder;
2) preparing gold nanoparticle-doped carbonized organic silicon pellets: calcining the gold-complexed organic silicon pellet powder prepared in the step 1) for 6-10 h at the temperature of 500-1000 ℃ under the protection of protective gas to obtain gold nanoparticle-doped carbonized organic silicon pellet powder;
3) preparing a GSP membrane material: uniformly dispersing the gold nanoparticle doped carbonized organic silicon pellet powder prepared in the step 2) in water, then placing fiber filter paper in a Buchner funnel, performing vacuum filtration, uniformly dripping the gold nanoparticle doped carbonized organic silicon pellet powder dispersion liquid on the fiber filter paper, and performing vacuum filtration for 10-30 min to obtain the GSP membrane material.
2. The preparation method of the GSP film material according to claim 1, wherein the step 1) comprises the following steps:
1.1) when preparing organosilicon powder, uniformly dispersing gamma-mercaptopropyl trimethoxysilane in water, preparing a gamma-mercaptopropyl trimethoxysilane solution with the concentration of 0.8-10 mg/mL, adding ammonia water to adjust the pH value of the solution to 9-11, hydrolyzing for 10-24 h, centrifuging at the rotating speed of 3000-5000 rpm to remove supernatant, adding deionized water, washing for 1-5 times, freezing by using liquid nitrogen, and drying in vacuum to obtain organosilicon powder; the reaction process is as follows:
1.2) uniformly dispersing the purchased or prepared organosilicon powder in the step 1.1) in water, preparing organosilicon dispersion liquid with the concentration of 10-100 mg/mL, then adding chloroauric acid solution with the concentration of 0.25 mol/L, performing ultrasonic treatment until the color of the solution is not changed, centrifuging to remove supernatant, freezing by using liquid nitrogen, performing vacuum drying, and then obtaining gold-complexed organosilicon pellet powder.
3. The preparation method of the GSP film material according to claim 1, wherein the step 3) comprises the following steps:
3.1) dispersing the gold nanoparticle doped carbonized organic silicon beads prepared in the step 2) into water, uniformly dispersing by ultrasonic, and preparing a gold nanoparticle doped carbonized organic silicon bead dispersion liquid with the concentration of 0.5-2 mg/mL;
3.2) laying 4-6 double-circle qualitative filter paper on a Buchner funnel, cutting the fiber filter paper according to the specification of the Buchner funnel, putting the fiber filter paper into the Buchner funnel, laying the cut fiber filter paper on the upper side of the double-circle qualitative filter paper, carrying out vacuum filtration under the condition that the pressure of a vacuum pump is 0.05-0.1 Mpa, uniformly dripping the dispersed gold nanoparticle doped carbonized organic silicon bead dispersion liquid obtained in the step 3.1) on the fiber filter paper, and continuing the vacuum filtration for 10-30 min to obtain the GSP membrane material.
4. The preparation method of the GSP film material according to claim 2, wherein in the step 1.2), the mass ratio of the gold in the chloroauric acid to the silicone bead powder is 1: 1-10.
5. The preparation method of the GSP film material according to claim 2, wherein in the step 1.1) and the step 1.2), the vacuum drying condition is that the pressure of 10-100 Pa is acted for 12-24 h.
6. The method of preparing a GSP film material of claim 1, wherein said shielding gas is argon, helium or nitrogen.
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| CN109399659A (en) * | 2018-11-16 | 2019-03-01 | 华东理工大学 | A kind of Ti-Si zeolite and preparation method thereof that small size is gold-nanoparticle-supported |
| CN109734148A (en) * | 2019-03-20 | 2019-05-10 | 菏泽学院 | A kind of preparation method and applications of the biomass carbon material for solar energy evaporation water |
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| CN105031950A (en) * | 2015-06-05 | 2015-11-11 | 上海交通大学 | Method capable of controlling temperature of evaporation surface based on porous composite material |
| CN109399659A (en) * | 2018-11-16 | 2019-03-01 | 华东理工大学 | A kind of Ti-Si zeolite and preparation method thereof that small size is gold-nanoparticle-supported |
| CN109734148A (en) * | 2019-03-20 | 2019-05-10 | 菏泽学院 | A kind of preparation method and applications of the biomass carbon material for solar energy evaporation water |
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