CN114260011B - Preparation method of ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode - Google Patents
Preparation method of ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode Download PDFInfo
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Abstract
The invention discloses a preparation method of a ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode, which comprises the following steps: adding polyvinylidene fluoride powder into N, N-dimethylacetamide to obtain a polyvinylidene fluoride solution; will H 2 PtCl 6 Solution and H 2 IrCl 6 Dripping the solution into the solution to obtain orange-yellow solution; adding alkali liquor into the orange-yellow solution, and then adding RuCl 3 Obtaining black emulsion from the solution; centrifuging, washing, re-centrifuging and drying to obtain nano particles; stirring and heating the mixed solution of isopropanol and citric acid to obtain a colorless transparent solution; adding the nano particles into a colorless transparent solution, and refluxing to obtain black gel; adding active carbon powder and titanium compound powder into the mixture gel, coating the mixture gel on a substrate electrode sheet, and drying and calcining the mixture gel to obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode. The electrode prepared by the method can enhance the oxidability, conductivity and photocatalytic activity of the electrode material, prolong the service life of the electrode and improve the binding force of the catalyst and the membrane.
Description
Technical Field
The invention relates to the technical fields of electrocatalytic oxidation reduction and photoelectric composite catalysis, can be used for oxidative degradation of organic pollutants and electrodeposition purification of mercury pollution, and in particular relates to a preparation method of a ruthenium iridium titanium platinum doped quaternary photoelectric catalytic carbon-based electrode.
Background
Among them, metal oxides are known to be a semiconductor material excellent in physical and chemical properties, and have important applications in the fields of optics, optoelectronics, sensors, photocatalysis, dye-sensitized solar cells and the like. The metal oxide electrode is a composite electrode with excellent performance obtained by covering a metal oxide coating on the surface of a substrate, and ruthenium-iridium-titanium oxide is widely used at present. In the photoelectrocatalytic oxidation treatment, the material is not only the core of photoelectrocatalytic oxidation, but also the preparation method is particularly important. The electrode prepared in the prior art still has the problems of poor electrode activity, short service life of the electrode, easy falling of a coating, weak photoelectric composite performance and the like, and becomes a hot point problem for research.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode, and the preparation method can enhance the stability and photoelectrocomposite catalysis performance of materials and enhance the simultaneous removal performance of organic matters and heavy metals in pollutants.
In order to achieve the above purpose, the specific technical scheme adopted by the invention is as follows:
the preparation method of the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode comprises the following specific steps:
step a, adding 2.0-10.0 g of polyvinylidene fluoride powder into 50-200 ml of N, N-dimethylacetamide under rapid stirring to obtain polyvinylidene fluoride solution;
step b. 0.01 to 0.1g of H with concentration of 0.01 to 0.1g/mL 2 PtCl 6 Solution and 0.001-0.1 g H with concentration of 0.01-0.1g/mL 2 IrCl 6 Dropwise adding the solution into the polyvinylidene fluoride solution prepared in the step a, and continuously stirring for 5-10 h to obtain a yellow solution;
step c, adding excessive alkali liquor into the yellow solution prepared in the step b until the pH value is 8-10, stirring for 10-30 min, and then adding 0.001-0.1 g of RuCl with the concentration of 0.01-0.1g/mL 3 Obtaining black emulsion;
step d, centrifuging the black emulsion prepared in the step c for 10-30 min, washing, centrifuging for 10-30 min, and drying at 80-120 ℃ for 5-10 h to obtain nano particles;
step e, mixing and stirring isopropanol and citric acid according to the volume ratio of (1-3) to 1, and heating to obtain colorless transparent solution;
step f, adding the nano particles prepared in the step d into the colorless transparent solution prepared in the step e according to the mass ratio of (10-30), and refluxing for 1-5 h at 80-100 ℃ to obtain black gel;
step g, adding active carbon powder and titanium compound powder into the black gel prepared in the step f, wherein the mass ratio is (10-30): (1-3): 10, and uniformly stirring to obtain a mixture gel;
and h, coating the mixture gel prepared in the step g on a substrate electrode slice, drying for 10-60 min at 100-120 ℃, calcining for 10-60 min at 300-500 ℃, and repeating the coating, drying and calcining for 5-20 times to finally obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode.
Preferably, the alkali liquor in the step c is any one of ammonia water, KOH and NaOH solution.
Preferably, the titanium compound in the step g is any one or a combination of two or more of titanium oxide, titanium nitride, titanium carbide, titanium sulfide and titanium selenide.
Preferably, the substrate electrode sheet in the step h is any one of titanium-based, niobium-based, carbon-based, stainless steel-based, copper-based and carbon-steel-based.
Preferably, the substrate electrode sheet in the step h is any one of a substrate, a base net, and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode prepared by the method can enhance the stability of electrode materials, the effect of the electrode after recycling is still maintained, and the service life of the electrode is prolonged.
2. Noble metal platinum (Pt) has good conductivity and high visible light absorption capacity, and has high activity in noble metal, and is combined with metal oxideAfter the recombination, the metal oxide can be used as an electron capturing agent to effectively prevent the recombination of the excited electrons and holes, and can be used as a light capturing agent to obviously enhance the absorption of the metal oxide to visible light, so that the photoelectric property of the metal oxide is more excellent and the application range is wider. The noble metal oxide coating has better electrocatalytic activity and excellent corrosion resistance, so that the noble metal oxide coating becomes an ideal electrochemical conductive material and is widely applied to the fields of catalysis, chemical sensing, biological medicine and the like. Pt is introduced into the electrode, so that the electrocatalytic performance can be improved, and the Pt is easy to combine with Hg 0 To form an alloy, one platinum atom can bind up to four mercury atoms, which is compared to Hg compared to gold 0 Is 12 times greater than gold. Therefore, pt is doped on the ruthenium-iridium-titanium composite electrode, so that the electrocatalytic oxidation activity can be enhanced, and Hg can be enhanced 0 Is not limited, and the removal performance of the catalyst is improved.
3. The ruthenium iridium titanium platinum doping can improve the photoelectrocatalysis composite property, and especially the addition of titanium compounds such as titanium nitride, titanium carbide, titanium sulfide, titanium selenide and the like can greatly improve the photocatalytic activity and the heavy metal removal effect.
4. The active carbon is similar to an electrode made of platinum in power density, is an effective catalyst for oxidation reduction in the electrode, and introduces O-C-OH and-O-C groups through high-temperature calcination, so that the excellent activity of 2e-ORR of the active carbon is greatly improved, and the active carbon is better applied to the electrochemical advanced oxidation process.
Description of the drawings:
FIG. 1 is a graph showing the effect of the mercury removal test performed after each regeneration of the electrode prepared from the polyvinylidene fluoride solution in example 1, in which the electrode surface is regenerated by immersing and cleaning the electrode with strong acid after each mercury removal;
FIG. 2 is a graph showing the comparative effect of the titanium compound in example 1 on heavy metal removal;
FIG. 3 is an EDS schematic diagram of the surfaces of the front and rear electrodes for treating mercury-containing wastewater by the ruthenium iridium titanium platinum doped quaternary photoelectrocatalytic carbon-based electrode in example 2;
fig. 4. The continuous COD degradation effect of the paraffinic oil wastewater ruthenium iridium titanium platinum doped quaternary photoelectrocatalytic carbon-based electrode in example 3.
The specific embodiment is as follows:
example 1
The preparation method of the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode comprises the following specific steps:
step a. Adding 10.0g of polyvinylidene fluoride powder into 200ml of N, N-dimethylacetamide under rapid stirring to obtain a polyvinylidene fluoride solution;
step b. 0.1g H was added at a concentration of 0.1g/mL 2 PtCl 6 Solution and 0.1g H with concentration of 0.1g/mL 2 IrCl 6 Dropwise adding the solution into the polyvinylidene fluoride solution prepared in the step a, and continuously stirring for 10 hours to obtain a yellow solution;
step c. Adding excess alkali solution into the yellow solution prepared in step b until pH=10, stirring for 30min, and then adding 0.1g RuCl with concentration of 0.1g/mL 3 Obtaining black emulsion; the alkali liquor is any one of ammonia water, KOH and NaOH solution;
step d, centrifuging the black emulsion prepared in the step c for 30min, washing, centrifuging for 30min, and drying at 120 ℃ for 10h to obtain nano particles;
step e, mixing and stirring isopropanol and citric acid according to the volume ratio of 3:1, and heating to obtain colorless transparent solution;
step f, adding the nano particles prepared in the step d into the colorless transparent solution prepared in the step e according to the mass ratio of 1:30, and refluxing for 5 hours at 100 ℃ to obtain black gel;
step g, adding activated carbon powder and titanium compound powder into the black gel prepared in the step f, wherein the mass ratio is 30:3:10, and uniformly stirring to obtain a mixture gel; the titanium compound is any one or the combination of any two or more of titanium oxide, titanium nitride, titanium carbide, titanium sulfide and titanium selenide;
step h, coating the mixture gel prepared in the step g on a substrate electrode slice, drying at 120 ℃ for 60min, calcining at 500 ℃ for 60min, and repeating the coating, drying and calcining for 20 times to finally obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode; the substrate electrode sheet is any one of titanium base, niobium base, carbon base, stainless steel base, copper base and carbon steel base; and is any one of a substrate, a base net, and the like.
The noble metal platinum (Pt) has good conductivity and higher visible light absorption capacity, has higher activity in noble metal, can be used as an electron trapping agent after being compounded with metal oxide, not only effectively prevents the recombination of electrons and holes after being excited, but also can be used as a light trapping agent to obviously enhance the absorption of the metal oxide to visible light, so that the photoelectric property of the metal oxide is more excellent, and the application range is wider. The noble metal oxide coating has better electrocatalytic activity and excellent corrosion resistance, so that the noble metal oxide coating becomes an ideal electrochemical conductive material and is widely applied to the fields of catalysis, chemical sensing, biological medicine and the like. Pt is introduced into the electrode, so that the electrocatalytic performance can be improved, and the Pt is easy to combine with Hg 0 To form an alloy, one platinum atom can bind up to four mercury atoms, which is compared to Hg compared to gold 0 Is 12 times greater than gold. Therefore, pt is doped on the ruthenium-iridium-titanium composite electrode, so that the electrocatalytic oxidation activity can be enhanced, and Hg can be enhanced 0 Is not limited, and the removal performance of the catalyst is improved.
N, N-dimethylacetamide is a solvent of polyvinylidene fluoride powder, polyvinylidene fluoride (PVDF) is an emerging membrane material with excellent comprehensive performance, high mechanical strength, acid and alkali resistance and other harsh environmental conditions and good chemical stability, has the characteristics of outstanding dielectric property, biocompatibility, heat resistance, good electrochemical performance, high separation precision and high efficiency, and is one of important mediums for developing metallized membrane capacitors with high energy storage density.
According to the invention, polyvinylidene fluoride powder is added into N, N-dimethylacetamide to obtain a polyvinylidene fluoride solution, and the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode prepared by the method can enhance the stability of an electrode material; the electrode prepared by the polyvinylidene fluoride solution regenerates mercury on the surface of the electrode by dipping and cleaning with strong acid after each mercury removal, and carries out mercury removal test after each regeneration, 5 times of tests show that the mercury removal efficiency is not obviously different, and experimental data are shown in figure 1, which shows that the electrode has good stability and prolongs the service life of the electrode.
The ruthenium iridium titanium platinum doping can improve the photoelectrocatalysis composite property, and especially the addition of titanium compounds such as titanium nitride, titanium carbide, titanium sulfide, titanium selenide and the like can greatly improve the photocatalytic activity and the heavy metal removal effect; the structure of titanium nitride, titanium sulfide and the like is formed by mixing and combining nonmetallic ionic bonds, metal bonds and covalent bonds, wherein the p-orbit energy level of a nonmetallic element is lower than the fermi energy level, the movement of free electrons is similar to the movement on the d-orbit of metal, the electronic structure can lead the titanium nitride, the titanium sulfide and the like to have good conductivity, the optical performance of a film of the titanium nitride, the titanium nitride and the like to be similar to that of a noble metal film of gold, silver and the like, the nonmetallic doping is to introduce one or more nonmetallic elements into crystal lattices or crystal boundaries of the film, and the impurity energy level and the defect energy level formed by the nonmetallic doping are introduced into the bandgap of titanium dioxide, so that the excited energy is reduced, the bandgap of the titanium dioxide is reduced, the light absorption range of the titanium dioxide is widened, the photocatalytic performance can be generated in the visible light region and the infrared region, and the generation of active oxygen and the decomposition of H2O2 into hydroxyl free radicals can be enhanced. FIG. 2 is a graph showing the comparison of the effect of titanium compound on heavy metal removal, and illustrates the effect of titanium-doped compounds.
The active carbon in the invention is similar to an electrode made of platinum in terms of power density, is an effective catalyst for oxidation reduction in the electrode, and introduces O-C-OH and-O-C groups through high-temperature calcination, so that the excellent activity of 2e-ORR of the active carbon is greatly improved, and the active carbon is better applied to the electrochemical advanced oxidation process.
After the active carbon is calcined at 500 ℃ for oxidation treatment, the oxygen content is increased from the initial 1.14+/-0.10% to 4.92+/-0.20% and H is generated within 30min 2 O 2 The maximum value of (2) is 520.32mg/L, the removal rate of COD in 2min in the reactor is 91.1%, the effective mineralization rate is 75.8%, and the performance is obviously superior to that of the low-oxygen activated carbon catalyst (57.33 mg/L H) 2 O 2 Yield and effective mineralization of COD 19.6%
Example 2
2.0g of polyvinylidene fluoride powder was added to 100ml of N, N-dimethylacetamide under rapid stirring to obtain a polyvinylidene fluoride solution. Then 0.1g of H with a concentration of 0.1g/mL is added 2 PtCl 6 Solution and 0.1g H with concentration of 0.1g/mL 2 IrCl 6 The solution was added dropwise to the above solution, and stirring was continued for 6 hours to obtain a yellow solution. Excess sodium hydroxide solution was added to the yellow solution until ph=8.5, stirred for 10min, and then 0.01g of RuCl was added at a concentration of 0.1g/mL 3 The solution gave a black emulsion. Centrifuging the emulsion for 30min, washing with water, centrifuging for 10min, and drying at 100deg.C for 5 hr to obtain nanoparticle. Isopropanol and citric acid were mixed and stirred and heated to give a colorless clear solution, V (isopropanol): V (citric acid) = (2): 1. And adding the prepared nano particles into a colorless transparent solution prepared by mixing isopropanol and citric acid according to the mass ratio of 1:10, and refluxing for 2 hours at 100 ℃ to obtain black gel. Adding activated carbon powder and titanium nitride powder into black gel, and uniformly stirring according to the mass ratio of 10:3:10 to prepare gel coating liquid. And (3) coating the gel on a titanium substrate electrode slice, drying at 100 ℃ for 10min, calcining at 350 ℃ for 30min, and repeating the coating-drying-calcining steps for 7 times to finally obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode.
The obtained electrode is used as an anode, the titanium substrate is used as a cathode for mercury-containing sewage treatment, and an EDS schematic diagram of the surfaces of the electrode before and after the treatment of the mercury-containing sewage by the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode is shown in figure 3, wherein the total mercury content of raw water is 354.1ppb, and is reduced to 13.9ppb after being treated, and the removal rate reaches 96.07%.
Example 3
4.0g of polyvinylidene fluoride powder was added to 100ml of N, N-dimethylacetamide under rapid stirring to obtain a polyvinylidene fluoride solution. Then 0.05g of H with a concentration of 0.01g/mL 2 PtCl 6 Solution and 0.1g H with concentration of 0.01g/mL 2 IrCl 6 The solution was added dropwise to the above solution, and stirring was continued for 8 hours to obtain a yellow solution. Adding excessive potassium hydroxide solution into the yellow solutionUntil ph=9, stirring for 20min, then adding 0.1g of RuCl with concentration of 0.1g/mL 3 The solution gave a black emulsion. Centrifuging the emulsion for 10min, washing with water, centrifuging for 10min again, and drying at 108deg.C for 8 hr to obtain nanoparticle. Isopropanol and citric acid were mixed and stirred and heated to give a colorless clear solution, V (isopropanol): V (citric acid) = (3): 1. And adding the prepared nano particles into a colorless transparent solution prepared by mixing isopropanol and citric acid according to the mass ratio of 1:20, and refluxing for 3 hours at 100 ℃ to obtain black gel. Adding activated carbon powder and titanium oxide powder into black gel, and uniformly stirring according to the mass ratio of 10:3:10 to prepare gel coating liquid. And coating the gel on a niobium substrate electrode slice, drying at 108 ℃ for 20min, calcining at 400 ℃ for 15min, and repeating the coating-drying-calcining steps for 10 times to finally obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode.
The obtained electrode is used as an anode, the titanium substrate is used as a cathode, the titanium substrate is used for treating paraffin oil wastewater as shown in fig. 4, the COD of raw water is 3470ppm, the COD is reduced to 40ppm after 60min treatment, and the removal rate is 98.85%.
Example 4
5.0g of polyvinylidene fluoride powder was added to 200ml of N, N-dimethylacetamide under rapid stirring to obtain a polyvinylidene fluoride solution. Then 0.1g of H with a concentration of 0.1g/mL is added 2 PtCl 6 Solution and 0.1g H with concentration of 0.1g/mL 2 IrCl 6 The solution was added dropwise to the above solution, and stirring was continued for 10 hours to obtain a yellow solution. Adding excessive potassium hydroxide solution into the yellow solution until pH=10, stirring for 30min, and adding 0.1g RuCl with concentration of 0.1g/mL 3 The solution gave a black emulsion. Centrifuging the emulsion for 30min, washing with water, centrifuging for 30min, and drying at 100deg.C for 6 hr to obtain nanoparticle. Isopropanol and citric acid were mixed and stirred and heated to give a colorless clear solution, V (isopropanol): V (citric acid) = (2): 1. And adding the prepared nano particles into a colorless transparent solution prepared by mixing isopropanol and citric acid according to the mass ratio of 1:10, and refluxing for 1h at 100 ℃ to obtain black gel. Activated carbon powder and titanium nitride powderAdding the gel into black gel, and uniformly stirring according to the mass ratio of 20:1:10 to prepare gel coating liquid. And (3) coating the gel on a stainless steel net-shaped electrode plate, drying at 100 ℃ for 10min, calcining at 300 ℃ for 60min, and repeating the coating-drying-calcining steps for 10 times to finally obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode.
The obtained electrode is used as an anode, the titanium substrate is used as a cathode, the obtained electrode is used as the anode, the titanium substrate is used as the cathode, the titanium substrate is used for treating mixed waste liquid containing tetrahydrofuran, toluene, normal hexane and dichloromethane, after 65h treatment, COD is reduced from 113200mg/L to 104mg/L, and the removal rate is up to 99.91%.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (5)
1. The preparation method of the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode is characterized by comprising the following steps of:
adding 2.0-10.0 g polyvinylidene fluoride powder into 50-200 ml N, N-dimethylacetamide, and stirring to obtain polyvinylidene fluoride solution;
step b. 0.01 to 0.1g of H with concentration of 0.01 to 0.1g/mL 2 PtCl 6 Solution and 0.001-0.1 g H with concentration of 0.01-0.1g/mL 2 IrCl 6 Dropwise adding the solution into the polyvinylidene fluoride solution prepared in the step a, and stirring to obtain a yellow solution;
step c, adding alkali liquor into the yellow solution prepared in the step b until the pH value is 8-10, stirring, and then adding 0.001-0.1 g of RuCl with the concentration of 0.01-0.1g/mL 3 Obtaining black emulsion;
step d, centrifuging the black emulsion prepared in the step c for 10-30 min, washing, centrifuging for 10-30 min, and drying at 80-120 ℃ for 5-10 h to obtain nano particles;
step e, mixing and stirring isopropanol and citric acid according to the volume ratio of (1-3) to 1, and heating to obtain colorless transparent solution;
step f, adding the nano particles prepared in the step d into the colorless transparent solution prepared in the step e according to the mass ratio of (10-30), and refluxing for 1-5 h at 80-100 ℃ to obtain black gel;
step g, adding active carbon powder and titanium compound powder into the black gel prepared in the step f, wherein the mass ratio is (10-30): (1-3): 10, and uniformly stirring to obtain a mixture gel;
and h, coating the mixture gel prepared in the step g on a substrate electrode slice, drying for 10-60 min at 100-120 ℃, calcining for 10-60 min at 300-500 ℃, and repeating the coating, drying and calcining for 5-20 times to finally obtain the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode.
2. The method for preparing the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode according to claim 1, wherein the alkali liquor in the step c is any one of ammonia water, KOH and NaOH solution.
3. The method for preparing the ruthenium iridium titanium platinum doped quaternary photoelectrocatalytic carbon-based electrode according to claim 1, wherein the titanium compound in the step g is any one or a combination of any two or more of titanium oxide, titanium nitride, titanium carbide, titanium sulfide and titanium selenide.
4. The method for preparing the ruthenium iridium titanium platinum doped quaternary photoelectrocatalytic carbon-based electrode according to claim 1, wherein the substrate electrode sheet in the step h is any one of titanium-based, niobium-based, carbon-based, stainless steel-based, copper-based and carbon-steel-based.
5. The method for preparing the ruthenium iridium titanium platinum doped quaternary photoelectrocatalysis carbon-based electrode according to claim 1, wherein the substrate electrode sheet in the step h is any one of a substrate and a base net.
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