CN107866235B - Method for preparing heterojunction photocatalyst - Google Patents
Method for preparing heterojunction photocatalyst Download PDFInfo
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- CN107866235B CN107866235B CN201711013003.9A CN201711013003A CN107866235B CN 107866235 B CN107866235 B CN 107866235B CN 201711013003 A CN201711013003 A CN 201711013003A CN 107866235 B CN107866235 B CN 107866235B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000011943 nanocatalyst Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- 239000002105 nanoparticle Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 19
- 229910052753 mercury Inorganic materials 0.000 abstract description 17
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 10
- 239000003546 flue gas Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000001132 ultrasonic dispersion Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000011068 loading method Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 33
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Substances [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 4
- -1 cadmium sulfide modified bismuth oxyiodide Chemical class 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000004686 pentahydrates Chemical class 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 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
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/39—
-
- 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
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The invention provides a method for preparing a heterojunction photocatalyst, which comprises the steps of preparing CdS and BiOI nano-catalysts respectively, then uniformly loading CdS on the surface of BiOI through ultrasonic dispersion, and then forming the CdS/BiOI heterojunction photocatalyst through a calcination process. The heterojunction can effectively separate photo-generated electron hole pairs, the defect of low BiOI quantum efficiency is overcome, the prepared CdS/BiOI heterojunction photocatalytic material has good catalytic performance under the condition of visible light, the elemental mercury in flue gas of a power plant can be effectively subjected to photocatalytic oxidation, the mercury removal efficiency under the irradiation of an LED lamp reaches more than 80%, and the problem of mercury emission is solved. In addition, the preparation process is simple and the manufacturing cost is low.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to an inorganic catalyst, in particular to a method for preparing a nano CdS/BiOI heterojunction photocatalyst for high-performance photocatalytic oxidation of flue gas mercury in an electric power plant.
Background
As a highly toxic substance, mercury has the properties of high volatility, easy permanent enrichment in organisms and food chains and the like, causes great harm to the environment and human health, and has attracted wide attention to emission control. Coal combustion is a main artificial mercury emission source, and mercury emitted by coal in China accounts for about 40% of artificial emission every year, wherein a power plant accounts for about 35%. The adoption of the photocatalytic oxidation technology is the prior mercury removal technology. In recent years, BiOI has been widely studied as a visible light-induced, narrow bandgap semiconductor. However, the low quantum efficiency of the BiOI limits its further industrial applications. Therefore, there is a strong need to develop a photocatalyst having high quantum efficiency.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a method for preparing a heterojunction photocatalyst, and the method for preparing the heterojunction photocatalyst aims to solve the technical problems in the prior art that the heterojunction photocatalyst is low in catalytic efficiency, complex in preparation process and high in preparation cost.
The invention provides a method for preparing a heterojunction photocatalyst, which comprises the following steps:
1) weighing Cd (CH) according to the molar ratio of 1:53COO)2·2H2O and CH4N2S, mixing Cd (CH)3COO)2·2H2O and CH4N2Dissolving S in deionized water, continuously stirring to obtain a clear solution, pouring the solution into a hydrothermal reaction kettle, preserving heat for 18-30 h at the temperature of 130-160 ℃, naturally cooling to room temperature, centrifugally cleaning with deionized water, and transferring to an oven for drying to obtain CdS nanoparticles;
2) weighing Bi (NO)3)3·5H2O is dissolved in (CH)2OH)2Forming a solution A of Bi (NO)3)3·5H2O and (CH)2OH)2The material ratio is 1-2 g: 20-50 ml; weighing KI and dissolving in (CH)2OH)2Forming a solution B, said KI and (CH)2OH)2The material ratio of (A) is 0.50 g: 20-50 ml; adding the solution A into the solution B according to the volume ratio of 1:1 to obtain a uniform solution C, pouring the solution C into a hydrothermal reaction kettle, preserving the heat for 18-30 h at the temperature of 130-160 ℃, and naturally cooling to room temperatureThen respectively centrifugally cleaning with deionized water and ethanol, and then transferring to an oven for drying to obtain the BiOI nano catalyst;
3) dissolving the obtained BiOI nano catalyst and CdS into deionized water, wherein the mass ratio of the BiOI nano catalyst to the CdS is 1: 0.2-0.4, ultrasonically dispersing for 20-120 min to form CdS/BiOI suspension, centrifugally cleaning and drying, and finally calcining at 200-350 ℃ for 60-180 min to obtain the CdS/BiOI heterojunction photocatalyst.
The invention provides a synthesis method of a cadmium sulfide modified bismuth oxyiodide photocatalyst, which is simple in process and low in cost, and the cadmium sulfide modified bismuth oxyiodide photocatalyst is synthesized into a CdS/BiOI heterojunction photocatalyst by adopting an ultrasonic-assisted calcination method. Firstly, preparing CdS and BiOI nano-catalysts respectively and independently. Dissolving the obtained BiOI nano catalyst and a certain amount of CdS into deionized water, uniformly loading the CdS on the surface of the BiOI through ultrasonic dispersion, centrifugally cleaning a target solution for a plurality of times, and finally, calcining at high temperature and naturally cooling to obtain the CdS/BiOI heterojunction photocatalyst.
The heterojunction can effectively separate photo-generated electron hole pairs, the defect of low BiOI quantum efficiency is overcome, the prepared CdS/BiOI heterojunction photocatalytic material has good catalytic performance under the condition of visible light, the elemental mercury in flue gas of a power plant can be effectively subjected to photocatalytic oxidation, the mercury removal efficiency under the irradiation of an LED lamp reaches more than 80%, and the problem of mercury emission is solved. In addition, the preparation process is simple and the manufacturing cost is low.
The cadmium sulfide modified bismuth oxyiodide (CdS/BiOI) photocatalyst prepared by the invention can be used as a power plant flue gas photocatalytic oxidation catalyst. In the experimental process, the content of the element mercury in the simulated flue gas (nitrogen and air) carrying the element mercury is obviously reduced after the simulated flue gas passes through the photocatalytic reactor.
Compared with the prior art, the invention has remarkable technical progress. The invention has simple process and low cost. The photocatalyst prepared by the method has the advantages that trace cadmium sulfide is loaded on the surface of bismuth oxyiodide, the quantum efficiency of the bismuth oxyiodide is obviously improved, and flue gas mercury can be well oxidized by photocatalysis under the condition of visible light.
Drawings
FIG. 1: SEM image of example 1 sample.
FIG. 2: PL profile of example 2 sample.
FIG. 3: example 3 sample mercury removal efficiency plot under simulated flue gas carrier gas.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
The cadmium acetate, the dihydrate (not less than 98.5%), the thiourea (not less than 99.0%), the bismuth nitrate, the pentahydrate (not less than 99.0%), the potassium iodide (not less than 99.0%) and the glycol (not less than 99.0%) are used in the invention. The above medicines are purchased from chemical reagents of national medicine group, Inc., and no further treatment is carried out on the test medicines.
The SEM (scanning electron microscope) used in the invention adopts a Philips XL30 type electron microscope.
The PL spectrum used in the present invention was a fluorescence spectrum measuring instrument of SHIMADZU RF5301 model, manufactured by Japan, and the excitation wavelength was 320 nm.
The on-line mercury tester used in the invention is a LUMEX portable Zeeman effect mercury analyzer RA-915M with zero signal standard deviation<0.2ng/m3。
Example 1
1) 0.85g of Cd (CH) was weighed3COO)2·2H2O and 1.21g of CH4N2S, dissolving the CdS nanoparticles in 40ml of deionized water, continuously stirring to obtain a clear solution, pouring the target solution into a 50ml hydrothermal reaction kettle, keeping the temperature at 150 ℃ for 20h, naturally cooling to room temperature, centrifugally cleaning the target solution for a plurality of times by using the deionized water, and then transferring the target solution into an oven to dry the target solution to obtain the CdS nanoparticles.
2) 1.46g of Bi (NO)3)3·5H2O dissolved in 20ml of (CH)2OH)2Forming solution a. 0.50g of KI was dissolved in 20ml of (CH)2OH)2Forming solution B. Slowly dripping the solution A into the solution B according to the volume ratio of 1:1 to obtain a uniform solution C. Pouring the solution C into a 50ml hydrothermal reaction kettle, keeping the temperature at 160 ℃ for 18h, naturally cooling to room temperature, respectively centrifugally cleaning with deionized water and ethanol for a plurality of times, and then transferring to an oven for dryingAnd obtaining the BiOI nano catalyst.
3) Dissolving 1g of BiOI and 0.2g of CdS in deionized water, performing ultrasonic dispersion for 30min to obtain a CdS/BiOI suspension, performing centrifugal cleaning and drying, and finally maintaining the temperature in a muffle furnace at 350 ℃ for 60min to obtain the CdS/BiOI heterojunction photocatalyst.
Example 2
1) 3.19mmol of Cd (CH) were weighed3COO)2·2H2O and 15.95mmol of CH4N2S, dissolving the CdS nanoparticles in 40ml of deionized water, continuously stirring to obtain a clear solution, pouring the target solution into a 50ml hydrothermal reaction kettle, keeping the temperature at 130 ℃ for 30h, naturally cooling to room temperature, centrifugally cleaning the target solution for a plurality of times by using the deionized water, and then transferring the target solution into an oven to dry the target solution to obtain the CdS nanoparticles.
2) 1.46g of Bi (NO)3)3·5H2O dissolved in 20ml of (CH)2OH)2Forming solution a. 0.50g of KI was dissolved in 20ml of (CH)2OH)2Forming solution B. Slowly dripping the solution A into the solution B according to the volume ratio of 1:1 to obtain a uniform solution C. And pouring the solution C into a 50ml hydrothermal reaction kettle, keeping the temperature at 150 ℃ for 20h, naturally cooling to room temperature, respectively centrifugally cleaning the solution C for a plurality of times by using deionized water and ethanol, and then transferring the solution C into an oven for drying to obtain the BiOI nano catalyst.
3) Dissolving 1g of BiOI and 0.4g of CdS in deionized water, performing ultrasonic dispersion for 60min to obtain a CdS/BiOI suspension, performing centrifugal cleaning and drying, and finally maintaining the temperature in a muffle furnace at 300 ℃ for 90min to obtain the CdS/BiOI heterojunction photocatalyst.
Example 3
1) 3.19mmol of Cd (CH) were weighed3COO)2·2H2O and 1.21g of CH4N2S, dissolving the CdS nanoparticles in 40ml of deionized water, continuously stirring to obtain a clear solution, pouring the target solution into a 50ml hydrothermal reaction kettle, keeping the temperature at 160 ℃ for 18h, naturally cooling to room temperature, centrifugally cleaning the target solution for a plurality of times by using the deionized water, and then transferring the target solution into an oven to dry the target solution to obtain the CdS nanoparticles.
2) 1.46g of Bi (NO)3)3·5H2O dissolved in 20ml of (CH)2OH)2Forming solution a. 0.50g of KI was dissolved in 20ml of (CH)2OH)2Forming solution B. Slowly dripping the solution A into the solution B according to the volume ratio of 1:1 to obtain a uniform solution C. And pouring the solution C into a 50ml hydrothermal reaction kettle, keeping the temperature at 140 ℃ for 24h, naturally cooling to room temperature, respectively centrifugally cleaning the solution C for a plurality of times by using deionized water and ethanol, and then transferring the solution C into an oven for drying to obtain the BiOI nano catalyst.
3) Dissolving 1g of BiOI and 0.2g of CdS in deionized water, performing ultrasonic dispersion for 30min to obtain a CdS/BiOI suspension, performing centrifugal cleaning and drying, and finally maintaining the temperature of 250 ℃ in a muffle furnace for 120min to obtain the CdS/BiOI heterojunction photocatalyst.
FIG. 1 is an SEM image of a sample of example 1, from which it can be seen that the catalyst is uniformly distributed and no agglomeration occurs. FIG. 2 is a PL diagram of sample 2 of the embodiment, and it can be seen from the PL diagram that the CdS/BiOI heterojunction photocatalyst of the present invention has a significantly reduced photo-generated electron-hole recombination rate and an improved quantum efficiency compared to a pure phase BiOI. Fig. 3 is a graph of the mercury removal efficiency of the sample of the embodiment 3 under the simulated flue gas carrier gas, and it can be known that the mercury removal efficiency of the catalyst of the invention under the simulated flue gas carrier gas condition is greatly improved (about 80%) compared with that of the BiOI (about 16%).
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (1)
1. A method of preparing a heterojunction photocatalyst, comprising the steps of:
1) weighing Cd (CH) according to the molar ratio of 1:53COO)2·2H2O and CH4N2S, mixing Cd (CH)3COO)2·2H2O and CH4N2Dissolving S in deionized water, continuously stirring to obtain a clear solution, pouring the solution into a hydrothermal reaction kettle, preserving heat for 18-30 h at the temperature of 130-160 ℃, naturally cooling to room temperature, centrifugally cleaning with deionized water, and transferring to an oven for drying to obtain CdS nanoparticles;
2) weighing Bi (NO)3)3•5H2O is dissolved in (CH)2OH)2Forming a solution A of Bi (NO)3)3•5H2O and (CH)2OH)2The material ratio is 1-2 g: 20-50 ml; weighing KI and dissolving in (CH)2OH)2Forming a solution B, said KI and (CH)2OH)2The material ratio of (A) is 0.50 g: 20-50 ml; adding the solution A into the solution B according to the volume ratio of 1:1 to obtain a uniform solution C, pouring the solution C into a hydrothermal reaction kettle, preserving the heat for 18-30 h at the temperature of 130-160 ℃, naturally cooling to room temperature, respectively centrifugally cleaning with deionized water and ethanol, and then transferring to an oven for drying to obtain the BiOI nano catalyst;
3) dissolving the obtained BiOI nano catalyst and CdS into deionized water, wherein the mass ratio of the BiOI nano catalyst to the CdS is 1: 0.2-0.4, ultrasonically dispersing for 20-120 min to form CdS/BiOI suspension, centrifugally cleaning and drying, and finally calcining at 200-350 ℃ for 60-180 min to obtain the CdS/BiOI heterojunction photocatalyst.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| CN105879888A (en) * | 2016-01-22 | 2016-08-24 | 江苏大学 | Method for preparing CdS/BiOI heterojunction complex photocatalyst |
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| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
| CN105879888A (en) * | 2016-01-22 | 2016-08-24 | 江苏大学 | Method for preparing CdS/BiOI heterojunction complex photocatalyst |
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| Title |
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| 超声分散法制备 WS2/TiO2复合光催化剂及其光催化性能;杜意恩 等;《四川大学学报（自然科学版）》;20100731;第829-834页 * |
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