CN108404960B - Preparation method of sulfur-indium-zinc-gold carbon nitride two-dimensional layered composite photocatalyst - Google Patents
Preparation method of sulfur-indium-zinc-gold carbon nitride two-dimensional layered composite photocatalyst Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- AYLZDMCGTKDOGD-UHFFFAOYSA-N [C].[Au].[Zn].[In].[S] Chemical compound [C].[Au].[Zn].[In].[S] AYLZDMCGTKDOGD-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 239000010931 gold Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 29
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 20
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 239000004201 L-cysteine Substances 0.000 claims abstract description 12
- 235000013878 L-cysteine Nutrition 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000011734 sodium Substances 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000007865 diluting Methods 0.000 claims abstract description 4
- 239000001509 sodium citrate Substances 0.000 claims abstract description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 7
- YYKKIWDAYRDHBY-UHFFFAOYSA-N [In]=S.[Zn] Chemical compound [In]=S.[Zn] YYKKIWDAYRDHBY-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 229910052737 gold Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 229910004042 HAuCl4 Inorganic materials 0.000 abstract 1
- 235000011187 glycerol Nutrition 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 2
- 235000018417 cysteine Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- NJWNEWQMQCGRDO-UHFFFAOYSA-N indium zinc Chemical compound [Zn].[In] NJWNEWQMQCGRDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a sulfur-indium-zinc-gold carbon nitride two-dimensional layered composite photocatalyst, and C6H5Na3O7·2H2Dissolving O in deionized water, HAuCl4Diluting and heating to boil, adding the sodium citrate solution, boiling, and cooling to room temperature to obtain a gold colloid mixed solution; g-C3N4Ultrasonic treatment in dissolved ethanol, Zn (NO)3)2·6H20，In(NO3)3·4.5H2Dissolving O, L-Cysteine in the mixture of glycerin and gold colloid, and neutralizing with g-C3N4The solution is mixed and absorbed to obtain ZnIn2S4/Au/g‑C3N4Precursor solution; heating and reacting in a hydrothermal reaction kettle, and carrying out vacuum freeze drying to obtain the powdered sulfur indium zinc/gold/carbon nitride two-dimensional layered composite photocatalyst. The invention has the advantages of easily obtained raw materials, one-kettle synthesis, strong reliability and simple and convenient operation, and the catalyst has stronger photocatalytic activity in a visible light region and has wide application prospect.
Description
Technical Field
The invention relates to a preparation method of a sulfur-indium-zinc-gold carbon nitride two-dimensional layered composite photocatalyst.
Background
In 1972, Fujishima and Honda of the university of Tokyo, Japan were found experimentally in TiO2The photoelectrode can directly decompose water to produce hydrogen, and TiO is utilized to produce hydrogen2The photocatalytic degradation of organic pollutants under the irradiation of ultraviolet light has also made great progress. The semiconductor photocatalysis technology shows huge application prospect. In order to further widen the utilization range of the photocatalytic material and degrade organic matters under the irradiation of visible light, the metal sulfide is widely applied to the photocatalytic reaction of the visible light, because the forbidden band is narrow, the visible light part in sunlight can be absorbed in a larger range, but the sulfide also has the general photo-corrosion phenomenon, so that the service life of the sulfide is greatly shortened.
To solve this problem, ZnIn is a ternary sulfide2S4And g-C3N4The heterojunction formed by compounding can effectively separate photogenerated electrons from holes, and the anti-light corrosion capability of the material is enhanced. Chinese patent application 201510010704.1 discloses a carbon nitride/sulfur indium zinc (ZnIn)2S4/g-C3N4) Composite nano material and its preparation process. Wherein, ZnIn2S4/g-C3N4ZnIn of hexagonal medium phase2S4In the form of large spheres, lamellar g-C3N4The composite surface has limited actual contact area and provides less electron transfer sites.
CN107159288A discloses a preparation method of a carbon nitride-based composite nano material, wherein the carbon nitride-based composite nano material is a zinc indium sulfide/carbon nitride/graphene oxide composite nano material, CdIn2S4Nanocubes and g-C3N4The nano-sheets and the graphene sheets are combined together, and the carbon nitride is prepared by adopting a one-step hydrothermal methodWeighing g-C based composite nano material3N4Dissolving the powder and graphene oxide sheets in deionized water, performing ultrasonic dispersion, and sequentially adding Cd (NO) under stirring3)2·4H2O，In(NO3)3·4.5H2O, after being stirred uniformly, the thioglycollic acid solution (C) is added in turn2H5NS) and Na2And (3) stirring the solution S again, transferring the reaction solution into a reaction kettle with a polytetrafluoroethylene lining, carrying out hydrothermal reaction, washing, centrifuging and drying the obtained product to obtain the zinc indium sulfide/carbon nitride/graphene oxide composite nano material.
To date, ZnIn has not been available2S4/Au/g-C3N4Reports of two-dimensional layered composites.
Disclosure of Invention
The invention aims to provide a preparation method of a sulfur indium zinc gold carbon nitride two-dimensional layered composite photocatalyst, which has the advantages of easily obtained raw materials, one-kettle synthesis, strong reliability and simple and convenient operation, and the prepared catalyst has strong photocatalytic activity in a visible light region and is widely applied.
The invention aims to realize a preparation method of a sulfur indium zinc gold carbon nitride two-dimensional layered composite photocatalyst, which comprises the following specific steps:
1) 7.3525g of C are taken6H5Na3O7·2H2Dissolving O in 50mL of deionized water, and stirring for 30 min;
2) 2.5mL of 0.01M/L HAuCl was taken4Diluting to 100mL, heating to boil, adding 200uL of the sodium citrate solution prepared in the step 1), keeping boiling for 15min, recovering the volume to 100mL, and cooling to room temperature to obtain a stable gold colloid mixed solution;
3) 0.5g g-C3N4Dissolving in 52.5mL ethanol, and ultrasonic treating for 30 min;
ultrasonic conditions are as follows: the ultrasonic frequency is 40kHz, and the ultrasonic power is 150W;
4) 0.0176-0.1232g of Zn (NO)3)2·6H 20，0.0045-0.0315g In(NO3)3·4.5H2O, 0.0572-0.4004g L-Cysteine17.5mL of glycerol and 10mL of the gold colloid mixed solution obtained in the step 2), and then stirring for 15 min;
5) mixing the two solutions obtained in the step 3) and the step 4), and stirring for 30min to obtain g-C3N4Adsorbing free ions and L-Cysteine molecules to obtain ZnIn2S4/Au/g-C3N4The precursor solution of (1);
6) transferring the precursor solution obtained in the step 5) into a 100mL stainless steel hydrothermal reaction kettle containing a polytetrafluoroethylene lining, and reacting at 160-200 ℃ for 20-26h to obtain a powdery sample;
7) taking out the powdery sample obtained in the step 6), respectively washing the powdery sample with alcohol and deionized water for a plurality of times, and carrying out vacuum freeze drying to obtain powdery ZnIn2S4/Au/g-C3N4A two-dimensional layered composite photocatalyst;
vacuum freeze-drying conditions: pre-freezing at-40 ℃ for 4h, vacuum degree of 5Pa, and vacuum drying for 6 h;
the obtained ZnIn2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.05-0.35.
The invention takes L-type cysteine as a sulfur source, and takes abundant functional groups on the surface of the biological molecular cysteine, metal ions, Au colloid and g-C3N4So that ZnIn is present2S4Growing in lamellar form g-C3N4The surface of the metal substrate forms a two-dimensional composite structure, so that the contact area is greatly increased, more electron transfer sites are provided for reaction, and the photocatalytic efficiency can be further increased by using the gold particles as a good electron conductor.
The invention has the advantages of easily obtained raw materials, one-kettle synthesis, strong reliability and simple and convenient operation; ZnIn prepared by the invention2S4/Au/g-C3N4The two-dimensional layered composite catalyst has stronger photocatalytic activity in a visible light area; can be applied to the aspects of environmental pollution treatment, solar energy utilization, hydrogen production by hydrolysis and the like, and has wide application prospect.
Drawings
FIG. 1 is a scanning electron micrograph of the composite photocatalyst of example 1;
FIG. 2 is a scanning electron micrograph of the composite photocatalyst of example 3;
FIG. 3 is a TEM photograph of the composite photocatalyst of example 3;
FIG. 4 is a graph showing the degradation performance of the composite photocatalyst on methyl orange in examples 1-4.
Detailed Description
The present invention is described in detail below with reference to specific examples.
Example 1
1) 7.3525g of C are taken6H5Na3O7·2H2Dissolving O in 50mL of deionized water, and stirring for 30 min;
2) 2.5mL of 0.01M/L HAuCl was taken4Diluting to 100mL, heating to boil, adding 200uL of the sodium citrate solution prepared in the step 1), keeping boiling for 15min, recovering the volume to 100mL, and cooling to room temperature to obtain a stable gold colloid mixed solution;
3) 0.5g g-C3N4Dissolving in 52.5mL ethanol, and ultrasonic treating for 30 min;
ultrasonic conditions are as follows: the ultrasonic frequency is 40kHz, and the ultrasonic power is 150W;
4) 0.0176g of Zn (NO)3)2·6H 20，0.0045g In(NO3)3·4.5H2O, 0.0572g L-Cysteine is dissolved in 17.5mL of glycerol and 10mL of the gold colloid mixed solution obtained in the step 2), and then stirred for 15 min;
5) mixing the two solutions obtained in the step 3) and the step 4), and stirring for 30min to obtain g-C3N4Adsorbing free ions and L-Cysteine molecules to obtain ZnIn2S4/Au/g-C3N4The precursor solution of (1);
6) transferring the precursor solution obtained in the step 5) into a 100ml stainless steel hydrothermal reaction kettle containing a polytetrafluoroethylene lining, and reacting for 24h at 180 ℃ to obtain a powdery sample.
7) Taking out the powdery sample obtained in the step 6)Respectively washing with alcohol and deionized water for several times, and vacuum freeze drying to obtain powdered ZnIn2S4/Au/g-C3N4Two-dimensional layered composite catalyst.
Vacuum freeze-drying conditions: pre-freezing at-40 deg.C for 4h, vacuum degree of 5Pa, and vacuum drying for 6 h.
ZnIn prepared in this example2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.05. ZnIn2S4/Au/g-C3N4The scanning electron micrograph of the two-dimensional layered composite catalyst is shown in FIG. 1.
Example 2, like example 1, except that,
4) 0.0528g Zn (NO)3)2·6H 20，0.0135g In(NO3)3·4.5H2Dissolving O, 0.1716g L-Cysteine in 17.5mL of glycerol and 10mL of the gold colloid mixed solution obtained in the step 2), and then stirring for 15 min;
5) mixing the two solutions obtained in the step 3) and the step 4), and stirring for 30min to obtain g-C3N4Adsorbing free ions and L-Cysteine molecules to obtain ZnIn2S4/Au/g-C3N4The precursor solution of (1);
6) transferring the precursor solution obtained in the step 5) into a 100mL stainless steel hydrothermal reaction kettle containing a polytetrafluoroethylene lining, and reacting for 24h at 180 ℃ to obtain a powdery sample.
ZnIn prepared in example2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.15.
example 3, like example 1, except that,
4) 0.088g Zn (NO)3)2·6H 20，0.0225g In(NO3)3·4.5H2Dissolving 0.286g L-Cysteine in 17.5mL of glycerol and 10mL of the gold colloid mixed solution obtained in the step 2), and then stirring for 15 min;
5) mixing the two solutions obtained in the step 3) and the step 4), and stirring for 30min to obtain g-C3N4Adsorbing free ions and L-Cysteine molecules to obtain ZnIn2S4/Au/g-C3N4The precursor solution of (1);
6) transferring the precursor solution obtained in the step 5) into a 100mL stainless steel hydrothermal reaction kettle containing a polytetrafluoroethylene lining, and reacting for 26h at 160 ℃ to obtain a powdery sample.
ZnIn prepared in this example2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.25. powdered ZnIn2S4/Au/g-C3N4The scanning electron micrograph of the two-dimensional layered composite catalyst is shown in FIG. 2, and the transmission electron micrograph is shown in FIG. 3.
Example 4, like example 1, except that,
4) 0.1232g Zn (NO)3)2·6H 20，0.0315g In(NO3)3·4.5H2Dissolving O, 0.4004g L-Cysteine in 17.5mL of glycerol and 10mL of the gold colloid mixed solution obtained in the step 2), and then stirring for 15 min;
5) mixing the two solutions obtained in the step 3) and the step 4), and stirring for 30min to obtain g-C3N4Adsorbing free ions and L-Cysteine molecules to obtain ZnIn2S4/Au/g-C3N4The precursor solution of (1);
6) transferring the precursor solution obtained in the step 5) into a 100mL stainless steel hydrothermal reaction kettle containing a polytetrafluoroethylene lining, and reacting for 20h at 200 ℃ to obtain a powdery sample.
ZnIn prepared in this example2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.35.
lamellar g-C was observed in the SEM photograph of FIG. 13N4ZnIn of FIG. 22S4/Au/g-C3N4Scanning electron microscope photographIn comparison of the tablet with FIG. 1, g-C is clearly found3N4ZnIn with lamellar formed on surface2S4ZnIn in FIG. 32S4/Au/g-C3N4The presence of gold particles in the layered structure was also observed in the transmission electron micrograph of (a), thus illustrating the successful organization of the layered two-dimensional structure of the invention.
The applicant takes a 300W xenon lamp as a light source, and a 400nm cut-off piece controls the light irradiation in a visible light region to degrade Methyl Orange (MO). The powder ZnIn prepared in the examples 1, 2, 3 and 4 is selected as the catalyst2S4/Au/g-C3N4A composite catalyst sample.
The method comprises the following steps: 100mg of ZnIn prepared in examples 1, 2, 3 and 4 were weighed out separately2S4/Au/g-C3N4The composite catalyst was placed in 100ml of a 10mg/L methyl orange aqueous solution and subjected to an experiment in a photocatalytic reactor. Before illumination, the system is placed in a dark box and stirred for 30min to reach adsorption balance, 2mL of solution is taken, and the concentration of the solution is tested by an ultraviolet-visible spectrophotometer and is used as the initial concentration of the photoreaction. Then the light source was turned on and samples were taken every 5min and detected with an ultraviolet-visible spectrophotometer. The results of the detection are shown in FIG. 4.
As can be seen from FIG. 4, the ZnIn prepared in example 1 was irradiated for 20min after visible light with a wavelength of more than 400nm2S4/Au/g-C3N4The degradation rate of the two-dimensional layered composite catalyst to the methyl orange solution is only 43.3%, and the ZnIn prepared in example 22S4/Au/g-C3N4The degradation rate of the two-dimensional layered composite catalyst was 82.5%, and the ZnIn prepared in example 32S4/Au/g-C3N4The degradation rate of the two-dimensional layered composite catalyst on the methyl orange solution reaches 99.4 percent, and the ZnIn prepared in example 42S4/Au/g-C3N4The degradation rate of the two-dimensional layered composite catalyst on the methyl orange solution is 96.5 percent, which shows that the ZnIn prepared by the invention2S4/Au/g-C3N4The composite catalyst has obvious effect of reducing methyl orangeThe photocatalytic performance is indeed greatly improved by the construction of a two-dimensional layered structure, in which the ZnIn prepared in example 22S4/Au/g-C3N4Samples, i.e. g-C3N4And ZnIn2S4The mass ratio of (1): 0.25 ZnIn2S4/Au/g-C3N4The two-dimensional layered composite catalyst has the best effect.
Claims (2)
1. A preparation method of a sulfur indium zinc gold carbon nitride two-dimensional layered composite photocatalyst is characterized by comprising the following steps: the method comprises the following specific steps:
1) 7.3525g of C are taken6H5Na3O7·2H2Dissolving O in 50mL of deionized water, and stirring for 30 min;
2) 2.5mL of 0.01M/L HAuCl was taken4Diluting to 100mL, heating to boil, adding 200uL of the sodium citrate solution prepared in the step 1), keeping boiling for 15min, recovering the volume to 100mL, and cooling to room temperature to obtain a stable gold colloid mixed solution;
3) 0.5g g-C3N4Dissolving in 52.5mL ethanol, and ultrasonic treating for 30 min;
ultrasonic conditions are as follows: the ultrasonic frequency is 40kHz, and the ultrasonic power is 150W;
4) 0.0176-0.1232g of Zn (NO)3)2·6H2O ，0.0045-0.0315g In(NO3)3·4.5H2O, 0.0572-0.4004g L-Cysteine is dissolved in 17.5mL of glycerol and 10mL of the gold colloid mixed solution obtained in the step 2), and then stirred for 15 min;
5) mixing the two solutions obtained in the step 3) and the step 4), and stirring for 30min to obtain g-C3N4Adsorbing free ions and L-Cysteine molecules to obtain ZnIn2S4/Au/g-C3N4The precursor solution of (1);
6) transferring the precursor solution obtained in the step 5) into a 100mL stainless steel hydrothermal reaction kettle containing a polytetrafluoroethylene lining, and reacting at 160-200 ℃ for 20-26h to obtain a powdery sample;
7) taking out the powdery sample obtained in the step 6), and respectively usingCleaning with alcohol and deionized water for several times, and vacuum freeze drying to obtain powdered ZnIn2S4/Au/g-C3N4A two-dimensional layered composite photocatalyst;
vacuum freeze-drying conditions: pre-freezing at-40 ℃ for 4h, vacuum degree of 5Pa, and vacuum drying for 6 h;
the obtained ZnIn2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.05-0.35.
2. The preparation method of the sulfur indium zinc gold carbon nitride two-dimensional layered composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: ZnIn2S4/Au/g-C3N4g-C in two-dimensional layered composite catalyst3N4And ZnIn2S4The mass ratio of (1): 0.25.
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| CN110624583A (en) * | 2019-09-03 | 2019-12-31 | 沈阳化工大学 | Preparation method of composite graphite phase carbon nitride heterojunction photocatalyst |
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| CN111659271B (en) * | 2020-03-18 | 2022-06-14 | 闽南师范大学 | Dissolving system and dissolving method for dissolving graphite phase carbon nitride |
| CN113996323B (en) * | 2021-11-24 | 2023-11-17 | 新乡学院 | Indium zinc sulfide composite visible light catalyst and preparation method and application thereof |
| CN114894874B (en) * | 2022-04-18 | 2023-02-14 | 湖南大学 | Self-powered double-optical-electrode sensor and preparation method and application thereof |
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