CN113797937A - Preparation method and application of sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst - Google Patents
Preparation method and application of sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst Download PDFInfo
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- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 66
- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 title claims abstract description 48
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- QOYRNHQSZSCVOW-UHFFFAOYSA-N cadmium nitrate tetrahydrate Chemical compound O.O.O.O.[Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QOYRNHQSZSCVOW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
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- 238000007146 photocatalysis Methods 0.000 claims abstract description 7
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- 238000006731 degradation reaction Methods 0.000 claims description 11
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- 229910003765 Ni2O5 Inorganic materials 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 239000010955 niobium Substances 0.000 claims description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 2
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 13
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- HXSJLKZLIDKETF-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].O.O.O.O.O.[Nb+5].[Nb+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].O.O.O.O.O.[Nb+5].[Nb+5] HXSJLKZLIDKETF-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
-
- B01J35/23—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a preparation method and application of a sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst. For the sodium niobate/cadmium sulfide composite catalyst, the sodium niobate, the cadmium nitrate tetrahydrate and the thioacetamide are dissolved in an organic solvent according to the stoichiometric ratio, and after the sodium niobate, the cadmium nitrate tetrahydrate and the thioacetamide are fully stirred and uniformly mixed, the sodium niobate, the cadmium nitrate tetrahydrate and the thioacetamide are both prepared by a hydrothermal synthesis method. In the preparation process, the process parameters such as the concentration of sodium hydroxide, the mixture ratio of raw materials, the hydrothermal synthesis temperature and the like are changed to prepare the composite pyroelectric catalysts with different proportions. The preparation method has the advantages of simple process and flow, easy operation, strong repeatability, low cost and high product recycling rate, and has wide application prospects in the aspects of degrading organic pollutants, catalyzing and sterilizing, enhancing photocatalysis and the like.
Description
Technical Field
The invention belongs to the technical field of novel functional materials, and particularly relates to a preparation method and application of a sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst.
Background
The photocatalytic method is an advanced oxidation technology that has been widely studied. It is prepared through the respective excitation of electrons and holes with dissolved oxygen and OH in solution-Reacting to generate active free radicals with strong oxidation property. The active free radicals can effectively carry out oxidation-reduction reaction with organic pollutants to successfully decompose the organic pollutants into water, carbon dioxide and other harmless substances, and although the photocatalysis method has the advantages of high efficiency, safety, environmental friendliness and the like, the photocatalysis method also has some defects, for example, the narrow ultraviolet light absorption range causes the light energy utilization rate not to be too high.
The transformation of heat energy (such as day and night temperature difference) by temperature difference of room temperature is a clean energy which is ubiquitous in nature. The pyroelectric material has excellent thermoelectric conversion capability, and can realize the conversion from heat energy to electric energy by utilizing the change of environmental temperature. Unlike thermoelectric materials which have been widely studied. Thermoelectric materials mainly utilize the temperature difference between two ends of the material to realize the conversion of heat energy to electric energy. On the nano scale, it is very difficult to maintain a temperature difference between the two ends of the nano material, and it is difficult to perform the micro/nano thermoelectric conversion only by using the thermoelectric effect. Therefore, on a micrometer/nanometer scale, the utilization of the pyroelectric material to realize the conversion of thermal energy into electric energy has great advantages.
NaNbO3One of the lead-free piezoelectric materials which has been widely studied also has excellent pyroelectric properties, NaNbO3The pyroelectric coefficient is about 10Cm-2K-1. It is important to emphasize that the pyroelectric effect occurs below the ferroelectric curie temperature (Tc). When the temperature T is>At Tc, the ferroelectric spontaneous polarization is zero, which results in the disappearance of the pyroelectric effect. NaNbO3Up to 370 ℃, hence NaNbO3Materials are suitable candidates for room temperature thermocatalysis. But the current NaNbO3As a pyroelectric catalytic sterilization and degradation organic dye in dye wastewater and an enhancement of photocatalysis application, a system complete and reasonable process is not available, and the sterilization and degradation efficiency is low, so that the requirements in the actual treatment process are difficult to meet.
Disclosure of Invention
The invention aims to provide a preparation method and application of a sodium niobate/cadmium sulfide rod-shaped pyroelectric catalyst aiming at the problems in the prior art.
The technical scheme adopted by the invention is as follows:
a rod-shaped pyroelectric sodium niobate/cadmium sulfide catalyst is prepared from NaNbO prepared by hydrothermal synthesis3And loading CdS particles to the surface of the rod-shaped sodium niobate by using the CdS particles as carriers. The loading capacity of cadmium sulfide is 30-50%, preferably 50%; the sodium niobate is rod-shaped, and the ratio of the diameter of cadmium sulfide particles to the diameter of cadmium sulfide rods is (1:3) - (1: 4.5); the preparation method is that the single sodium niobate (NaNbO) is prepared by a hydrothermal synthesis method3) And (3) taking the cadmium sulfide (CdS) particles as a carrier, and loading the cadmium sulfide (CdS) particles on the surface of the sodium niobate with the rod-shaped structure by hydrothermal synthesis, wherein the preparation steps are as follows:
a. preparing a sodium niobate monomer: niobium (Ni) oxide pentahydrate2O5·5H2O) is dissolved in sodium hydroxide solution, dilute hydrochloric acid (HCl) is dripped into the solution to adjust the pH value, then the solution is mechanically stirred for 2 to 4 hours at room temperature, put into a reaction kettle for hydro-thermal synthesis, centrifugally washed and put into a drying oven, and dried to obtain NaNbO3A monomer;
b. preparation of sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst, namely preparing the niobate prepared in the step aSodium (NaNbO)3) Dissolving a monomer, cadmium nitrate tetrahydrate and thioacetamide in a glycol organic solvent according to a stoichiometric ratio, mechanically stirring the mixture for 2-4 hours at room temperature, fully and uniformly mixing the mixture, putting the mixture into a reaction kettle for hydrothermal synthesis, washing and drying to obtain NaNbO3A CdS composite catalyst.
Ni described in step a2O5·5H2O0.3-0.5 g, Ni2O5·5H2The mass ratio of the O to the NaOH particles is 0.25-0.42; the concentration of the sodium hydroxide is 10mol/L or 12mol/L or 14 mol/L.
And b, adding dilute hydrochloric acid to adjust the pH of the solution to 7-8.
The parameters of the reaction kettle in the step a are as follows: the reaction time is 360min, and the reaction temperature is 160-180 ℃.
And (c) the mass ratio of the sodium niobate to the cadmium nitrate tetrahydrate and the thioacetamide in the step b is 1:1: 1.
And in the step b, the ethylene glycol organic solvent is 60-70 mL.
The parameters of the reaction kettle in the step b are as follows: the reaction time is 720min, and the reaction temperature is 160-180 ℃.
And c, loading the CdS in the step b to be 30-50 wt%.
Application of sodium niobate/cadmium sulfide rod-shaped composite pyroelectric catalyst, namely NaNbO3The application of the/CdS rod-shaped composite pyroelectric catalyst in catalytic degradation of organic dye wastewater, wherein rhodamine B is selected in a wastewater treatment experiment.
NaNbO3The application of the/CdS rod-shaped composite pyroelectric catalyst is characterized in that the temperature of cold water in cold-hot circulation is 20-25 ℃, and the temperature of hot water is 60-65 ℃ in the pyroelectric catalysis application process of the sodium niobate/cadmium sulfide rod-shaped composite catalyst.
NaNbO3the/CdS rod-shaped composite pyroelectric catalyst is applied to a water body, and is used for degrading a rhodamine B water solution under the condition of cold and hot circulation, wherein the concentration of the rhodamine B water solution is 5 mg/L.
The specific method of pyroelectric catalysis is as follows: the solution is placed in a cold water and hot water bath environment in a circulating mode, circulation is carried out once every 10min, and light-shielding treatment is carried out in the experimental process. After 10 cycles per interval, 3mL of the supernatant was measured and centrifuged, and the absorbance was measured by UV spectroscopy at 554 nm.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention takes sodium niobate as a carrier, prepares the sodium niobate/cadmium sulfide composite pyroelectric catalyst by modifying the sodium niobate, provides a larger specific surface area and an active site for the sodium niobate carrier, promotes the separation of a photoproduction electron pair, reduces the recombination of the photoproduction electron and a hole, and improves the degradation effect on organic dye.
(2) The invention adopts niobium oxide pentahydrate, cadmium nitrate tetrahydrate and thioacetyl as main raw materials, and has the advantages of simple raw materials and low cost. Preparing NaNbO by adopting hydrothermal synthesis method3The CdS rod-shaped composite pyroelectric catalyst has the advantages of simple process and flow, easy reaction control and strong repeatability.
(3) NaNbO prepared by the invention3The preparation method of the CdS rod-shaped composite pyroelectric catalyst is reasonably designed on process parameters and product structures, has higher pyroelectric catalytic performance, and has obvious effects on pyroelectric catalytic sterilization, organic pollutant degradation and photocatalysis enhancement. The degradation of rhodamine B aqueous solution is obviously higher than that of NaNbO3A monomer.
(4) NaNbO prepared by the invention3The CdS rod-shaped composite pyroelectric catalyst can excite the pyroelectric effect by means of day and night temperature difference in industrial application, realize pyroelectric catalysis, and is easy to operate.
Drawings
FIG. 1 is a drawing showing that NaNbO is prepared by the present invention3XRD pattern of/CdS composite pyroelectric catalyst.
FIG. 2 is a drawing showing that NaNbO is prepared by the present invention3SEM image of/CdS composite pyroelectric catalyst.
FIG. 3 is a drawing showing that NaNbO is prepared by the present invention3The degradation diagram of the/CdS composite pyroelectric catalyst to a rhodamine B water solution.
Detailed Description
The invention aims to provide a preparation method and application of a sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst.
The sodium niobate/cadmium sulfide rod-shaped composite pyroelectric catalyst is prepared by a hydrothermal synthesis method, sodium niobate is used as a carrier, cadmium sulfide particles are loaded on the surface of the sodium niobate, and the cadmium sulfide particles provide a larger specific surface area and active sites for the sodium niobate carrier, so that the separation of photo-generated electron pairs is promoted, the recombination of photo-generated electrons and holes is reduced, and the degradation of organic dyes is improved. The method has simple preparation process and low raw material cost, and the sodium niobate/cadmium sulfide rod-shaped composite pyroelectric catalyst is applied to photocatalysis, and can obviously improve the catalytic performance by utilizing the temperature change of day and night, thereby showing good application prospect in the aspects of treating organic pollutants and the like.
Example 1:
preparation of NaNbO by hydrothermal synthesis method3Monomer (b):
mixing Ni2O5·5H2Dissolving O and 1.2g of NaOH particles in 30mL of deionized water, dropwise adding dilute hydrochloric acid into the solution to adjust the pH value of the solution to 7, and then mechanically stirring the solution at room temperature for 2 hours; after the solutions are fully mixed, putting the mixed solution into a reaction kettle for hydrothermal synthesis, and setting the reaction temperature to be 160 ℃ and the reaction time to be 360 min; and after the reaction is finished, cooling to room temperature, centrifugally washing, and putting into a 70 ℃ oven to obtain the sodium niobate monomer.
Example 2:
preparation of NaNbO by hydrothermal synthesis method3A CdS rod-shaped composite pyroelectric catalyst:
the NaNbO prepared in example 1 was added3Dissolving a monomer, cadmium nitrate tetrahydrate and thioacetamide in a glycol organic solvent of 70mL according to the mass ratio of 1:1:1, and mechanically stirring the monomer at room temperature for about 2 hours; after fully and uniformly mixing, putting the mixture into a reaction kettle for hydrothermal synthesis, and setting the reaction temperature to be 160 ℃ and the reaction time to be 720 min; cooling to room temperature after the reaction is finished, centrifugally washing, and putting into a 70 ℃ oven to obtain NaNbO3A CdS composite catalyst.
FIG. 1 shows NaNbO3XRD pattern of/CdS rod-like pyroelectric catalyst, as can be seen from FIG. 1, at diffraction angle 2 theta22.75 degrees, 32.39 degrees, 46.46 degrees, 52.33 degrees, 57.77 degrees and 67.80 degrees, and the position of each diffraction peak is compared with the PDF #75-2102 standard card to respectively find that the standard card is compared with NaNbO3The characteristic peaks of the (100), (110), (200), (210), (211) and (220) crystal planes of (A) and (B) are matched. And at the diffraction angle 2 theta of 26.50 degrees, 30.70 degrees, 43.97 degrees, 52.10 degrees, 54.58 degrees and 63.93 degrees, the diffraction peak positions are compared with a PDF #75-1546 standard card, and are respectively matched with characteristic peaks of (111), (200), (220), (311), (222) and (400) crystal faces of CdS, so that NaNbO can be determined3The XRD pattern of the/CdS composite pyroelectric catalyst does not have any other impurity peaks.
FIG. 2 shows NaNbO obtained after hydrothermal synthesis3SEM image of/CdS rod-shaped composite pyroelectric catalyst, and rod-shaped NaNbO can be found from the SEM image3Are distributed in a straight staggered way and have the diameter of about 200 nm. While CdS particles are tightly attached to rod-shaped NaNbO3The surface, but the alignment was disordered and the particle diameter was about 50 nm.
Application example 1:
NaNbO obtained as described above3The rod-shaped pyroelectric catalyst is applied to treating organic pollutants in wastewater and degrading rhodamine B aqueous solution.
50mL of 5mg/L rhodamine B solution is taken, and 0.05g of NaNbO is added into the rhodamine B solution3The rod-shaped pyroelectric catalyst is prepared by circularly placing the solution in an environment with cold water at 25 ℃ and hot water at 65 ℃, circulating once every 10min, and carrying out light-shielding treatment in the whole experiment process. The supernatant of the solution was taken after every 10 cycles, and after centrifuging the supernatant at 8000r/min for 3min, the absorbance was measured by UV spectrometer at 554 nm.
Comparative application example 1:
NaNbO obtained as described above3The rod-shaped pyroelectric catalyst is applied to treating organic pollutants in wastewater and degrading rhodamine B aqueous solution.
Three portions of 50mL of 5mg/L rhodamine B solution are respectively added with 0.05g of NaNbO with the load of 30, 40 and 50wt percent3The solution is circularly placed in an environment with cold water at 25 ℃ and hot water at 65 ℃, the circulation is carried out once every 10min, and the whole experiment process is carried out in a dark place. Every 10 timesAfter the circulation, a supernatant of the solution was collected once, and after the supernatant was centrifuged at 8000r/min for 3min, the absorbance was measured at 554nm by an ultraviolet spectrometer.
FIG. 3 is NaNbO3A curve diagram of degrading rhodamine B water solution by using a CdS rod-shaped pyroelectric catalyst. As can be seen from FIG. 3, under the condition of pyroelectric catalysis, the degradation of the composite thermoelectric catalyst to rhodamine B aqueous solution is obviously higher than that of NaNbO in application 13Monomer, and 50% NaNbO3The degradation rate of the/CdS composite pyroelectric catalyst to a rhodamine B water solution can reach 81%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (8)
1. A preparation method of a sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst is characterized in that the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst takes sodium niobate as a carrier, cadmium sulfide particles are loaded on the surface of the sodium niobate, and the loading capacity of cadmium sulfide is 30-50%, preferably 50%; the sodium niobate is rod-shaped, and the ratio of the diameter of cadmium sulfide particles to the diameter of cadmium sulfide rods is (1:3) - (1: 4.5);
the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst is respectively matched with NaNbO at diffraction angles of 2 theta 22.75 degrees, 32.39 degrees, 46.46 degrees, 52.33 degrees, 57.77 degrees and 67.80 degrees3The characteristic peaks of the (100), (110), (200), (210), (211) and (220) crystal planes of the CdS are matched with the characteristic peaks of the (111), (200), (220), (311), (222) and (400) crystal planes of the CdS respectively at diffraction angles 2 theta of 26.50 degrees, 30.70 degrees, 43.97 degrees, 52.10 degrees, 54.58 degrees and 63.93 degrees;
the preparation method is that the single sodium niobate (NaNbO) is prepared by a hydrothermal synthesis method3) And (3) taking the cadmium sulfide (CdS) particles as a carrier, and loading the cadmium sulfide (CdS) particles on the surface of the sodium niobate with the rod-shaped structure by hydrothermal synthesis, wherein the preparation steps are as follows:
a. preparing a sodium niobate monomer: mixing niobium (N) oxide pentahydratei2O5·5H2O) and sodium hydroxide particles are dissolved in deionized water, dilute hydrochloric acid (HCl) is dripped into the solution to adjust the pH value, then the solution is mechanically stirred for 2 to 4 hours at room temperature, the solution is put into a reaction kettle for hydro-thermal synthesis, and NaNbO is obtained after washing and drying3A monomer; the Ni2O5·5H2The mass ratio of the O to the NaOH particles is 0.25-0.42; the concentration of the sodium hydroxide is 10mol/L or 12mol/L or 14 mol/L;
b. preparing a sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst, namely preparing the sodium niobate (NaNbO) prepared in the step a3) Dissolving a monomer, cadmium nitrate tetrahydrate and thioacetamide in a glycol organic solvent according to a stoichiometric ratio, mechanically stirring the mixture for 2-4 hours at room temperature, fully and uniformly mixing the mixture, putting the mixture into a reaction kettle for hydrothermal synthesis, washing and drying to obtain NaNbO3A CdS composite catalyst.
2. The preparation method and application of the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst according to claim 1, wherein dilute hydrochloric acid is added in the step a to adjust the pH of the solution to 7-8.
3. The method and the application of the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst as claimed in claim 1, wherein the parameters of the reaction kettle in the step a are as follows: the reaction time is 360min, and the reaction temperature is 160-180 ℃.
4. The method and the application of the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst as claimed in claim 1, wherein the parameters of the reaction kettle in the step b are; the reaction time is 720min, and the reaction temperature is 160-180 ℃.
5. The preparation method and the application of the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst as claimed in claim 1, wherein the mass ratio of the sodium niobate to the cadmium nitrate tetrahydrate and the thioacetamide in the step b is 1:1: 1.
6. The application of the sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst prepared by the preparation method of any one of claims 1 to 5 is characterized in that the composite rod-shaped catalyst is applied to pyroelectric catalytic sterilization and degradation of organic dyes in dye wastewater and enhanced photocatalysis.
7. The use of claim 6, wherein the composite rod catalyst is used for realizing pyroelectric catalysis by means of day-night temperature difference to excite pyroelectric effect.
8. The sodium niobate/cadmium sulfide composite rod-shaped pyroelectric catalyst prepared by the method of any one of claims 1 to 7.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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