CN115709079A - Mo-modified sulfur-indium-zinc photocatalyst, and synthesis method and application thereof - Google Patents
Mo-modified sulfur-indium-zinc photocatalyst, and synthesis method and application thereof Download PDFInfo
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- CN115709079A CN115709079A CN202211191797.9A CN202211191797A CN115709079A CN 115709079 A CN115709079 A CN 115709079A CN 202211191797 A CN202211191797 A CN 202211191797A CN 115709079 A CN115709079 A CN 115709079A
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- YYKKIWDAYRDHBY-UHFFFAOYSA-N [In]=S.[Zn] Chemical class [In]=S.[Zn] YYKKIWDAYRDHBY-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 238000001308 synthesis method Methods 0.000 title abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 45
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000011701 zinc Substances 0.000 claims description 12
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 6
- 238000006303 photolysis reaction Methods 0.000 claims description 6
- 230000015843 photosynthesis, light reaction Effects 0.000 claims description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 7
- 230000002194 synthesizing effect Effects 0.000 claims 3
- 238000010189 synthetic method Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 150000002500 ions Chemical class 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 230000005684 electric field Effects 0.000 abstract description 3
- 230000000737 periodic effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 150000002431 hydrogen Chemical class 0.000 abstract description 2
- 238000011056 performance test Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 6
- 239000002803 fossil fuel Substances 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- UDWJTDBVEGNWAB-UHFFFAOYSA-N zinc indium(3+) sulfide Chemical compound [S-2].[Zn+2].[In+3] UDWJTDBVEGNWAB-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a Mo modified sulfur indium zinc photocatalyst, a synthesis method and an application thereof, wherein the Mo modified sulfur indium zinc photocatalyst is a hexagonal ZnIn photocatalyst 2 S 4 Single crystal phase, mo element entering ZnIn 2 S 4 Unit cell, partially replacing In position In unit cell. The invention has the beneficial effects that: the activity of the photocatalyst reaches 1mmol/g/h, is 10 times of that of a pure sulfur indium zinc catalyst, and the photocatalyst has stable catalytic performance, and can still keep more than 90% of the activity of a fresh sample in a 5-cycle performance test; mo is doped into the sulfur indium zinc crystal lattice to generate unit cell dipoles, and the unit cell dipoles are superposed in the positive direction to form a built-in electric field by utilizing the characteristic of periodic arrangement of the unit cells, so that the carrier recombination rate is reduced, the probability of S-2 ions being oxidized is inhibited, and the hydrogen production activity and the catalytic life of the catalyst are improved; the catalyst prepared by the invention has good performance of photolyzing water to produce hydrogen, has stable property and is not easy to generate lightAnd (6) corrosion.
Description
Technical Field
The invention relates to a Mo modified sulfur indium zinc photocatalyst, a synthesis method and application thereof, and belongs to the technical field of nano material preparation and photocatalysis.
Background
The development of modern industry is based on fossil fuel consumption. The fossil fuel is used as a non-renewable energy source, and the large use of the fossil fuel causes problems of air pollution, energy shortage and the like. Therefore, the search for a clean energy source to replace fossil fuel is urgent. The combustion of H2 produces only water, which is an excellent clean energy source. The hydrogen production technology by photolysis comes from solar energy, the reactant is water, and the hydrogen production technology is an ideal technology for replacing fossil fuel.
Among many photocatalytic materials, ternary sulfide indium zinc sulfide (ZnIn 2S 4) shows great potential due to visible light response characteristics, a simple preparation method, and excellent stability. However, the higher carrier recombination rate limits its photocatalytic performance. In addition, sulfur element in the indium zinc sulfide catalyst has a valence of-2, so that the sulfur element is easily oxidized by holes generated by illumination, and the catalyst is deactivated. This is one of the reasons that the widespread use of sulfur indium zinc photocatalysts is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a Mo modified sulfur indium zinc photocatalyst and a synthesis method and application thereof, wherein Mo is doped into a sulfur indium zinc crystal lattice to generate unit cell dipoles, and the unit cell dipoles are superposed in a positive direction to form a built-in electric field by utilizing the characteristic of periodic arrangement of the unit cells, so that the carrier recombination rate is reduced, the probability of S-2 ions being oxidized is inhibited, and the hydrogen production activity and the catalytic life of the catalyst are improved.
The invention is realized by the following scheme: mo modified S-in-Zn photocatalyst which is hexagonal ZnIn 2 S 4 Single crystal phase, mo element entering ZnIn 2 S 4 Unit cell, partial substitution of In position In unit cell。
Mo modification proportion range: mo and ZnIn 2 S 4 The molar ratio is 1-10%.
A synthesis method of a Mo modified sulfur indium zinc photocatalyst comprises the following steps:
step one, dissolving 0.1g of Mo powder in a solution (20 mL) of H2O2 with the concentration of 10 percent to obtain a coordinated Mo solution A;
dissolving indium nitrate, zinc nitrate (the molar ratio is 2:1) and thioacetamide in water (70 mL) to obtain a reaction liquid B;
step three, mixing the coordinated Mo solution A with the reaction solution B (controlling the addition amount of A and controlling the mol ratio of Mo to Zn to be 1-10%), mechanically stirring for 30 minutes, and then transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours;
step four, naturally cooling to room temperature, centrifugally separating solid powder obtained by the hydrothermal reaction, washing with ethanol and water for 3 times respectively, and drying overnight;
and fifthly, calcining the dried solid powder for 3 hours at 300 ℃ by using a muffle furnace to prepare the Mo modified sulfur indium zinc photocatalyst.
The amount of the h2o2 solution to be used in the first step is 20mL by 10%.
In the second step, the mol ratio of the indium nitrate to the zinc nitrate is 2:1, thioacetamide was dissolved in 70mL of water.
And in the third step, the adding amount of A is controlled so that Mo: the Zn mol ratio is controlled between 1 and 10 percent.
An application of Mo modified S-in-Zn photocatalyst in hydrogen production by photolysis of water.
An application of a Mo modified sulfur indium zinc photocatalyst in water photolysis hydrogen production is that a 300W xenon lamp is used for simulating solar light irradiation; 0.1g of catalyst was dissolved in 100mL of water and charged into a quartz reactor; the distance between the quartz reactor and the central position of the light source is 15cm, and the reaction process is carried out under the protection of N2; the H2 produced was detected by chromatography.
The invention has the beneficial effects that:
1. the activity of the photocatalyst reaches 1mmol/g/h, is 10 times of that of a pure sulfur indium zinc catalyst, the catalytic performance is stable, and more than 90% of the activity of a fresh sample can be still maintained in a 5-cycle performance test;
2. according to the invention, mo is doped into the crystal lattice of the sulfur-indium-zinc to generate unit cell dipoles, and the unit cell dipoles are positively superposed to form a built-in electric field by utilizing the characteristic of periodic arrangement of the unit cells, so that the recombination rate of current carriers is reduced, the probability of S-2 ions being oxidized is inhibited, and the hydrogen production activity and the catalytic life of the catalyst are improved;
3. the catalyst prepared by the invention has good performance of photolyzing water to produce hydrogen, has stable property and is not easy to generate light corrosion.
Drawings
FIG. 1 is a graph comparing the hydrogen production performance of a Mo-modified sulfur indium zinc catalyst at 1%.
FIG. 2 is a graph comparing the hydrogen production performance of a 10% Mo modified sulfur indium zinc catalyst with a pure sulfur indium zinc catalyst.
Fig. 3 is a XRD result pattern for Mo modified sulphur indium zinc catalyst and pure sulphur indium zinc catalyst.
FIG. 4 is a diagram showing the result of the photolysis water-hydrogen production cycle of the Mo modified sulfur-indium-zinc catalyst.
Detailed Description
The invention is further described below with reference to fig. 1-4, without limiting the scope of the invention.
In the following description, for purposes of clarity, not all features of an actual implementation are described, well-known functions or constructions are not described in detail since they would obscure the invention with unnecessary detail, it being understood that in the development of any actual embodiment, numerous implementation details must be set forth in order to achieve the developer's specific goals, such as compliance with system-related and business-related constraints, changing from one implementation to another, and it being recognized that such development effort might be complex and time consuming, but would nevertheless be a routine undertaking for those of ordinary skill in the art.
Example 1 preparation and Properties of Mo-modified Sulfur indium Zinc catalyst 1%.
Dissolving 0.1g of Mo powder in a 10% H2O2 solution (20 mL) to obtain a coordinated Mo solution A; indium nitrate (0.75 g), zinc nitrate (0.30 g) and thioacetamide were dissolved in water (80 mL) to obtain a reaction solution B; adding 0.1mL of the solution A into the solution B, mechanically stirring for 30 minutes, and then transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours; naturally cooling to room temperature, centrifugally separating solid powder obtained by the hydrothermal reaction, washing with ethanol and water for 3 times respectively, and drying overnight; the dried solid powder was calcined at 300 ℃ for 3 hours in a muffle furnace to prepare a 1-% mo-modified sulfur indium zinc photocatalyst. The preparation method of the pure sulfur indium zinc catalyst used for comparison is similar, and solution A does not need to be added in the reaction. Simulating sunlight irradiation by a 300W xenon lamp; 0.1g of catalyst is dissolved in 100mL of water and is filled into a quartz reactor; the distance between the quartz reactor and the central position of the light source is 15cm, and the reaction process is carried out under the protection of N2; the H2 produced was detected by chromatography. The hydrogen production efficiency of the catalyst is shown in figure 1, the hydrogen production amount of the Mo-modified sulfur indium zinc catalyst with the percentage of 1 percent is stably increased within 2 hours, and the hydrogen production rate is 2.5mmol/g/h, which is ten times that of the pure sulfur indium zinc catalyst.
Example 2 preparation and performance of mo-modified sulphur indium zinc catalyst was calculated 10%.
Dissolving 0.1g of Mo powder in a 10% H2O2 solution (20 mL) to obtain a coordinated Mo solution A; indium nitrate (0.75 g), zinc nitrate (0.30 g) and thioacetamide were dissolved in water (80 mL) to obtain a reaction solution B; adding 1mL of the solution A into the solution B, mechanically stirring for 30 minutes, and then transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours; naturally cooling to room temperature, centrifugally separating solid powder obtained by the hydrothermal reaction, washing with ethanol and water for 3 times respectively, and drying overnight; the dried solid powder was calcined at 300 ℃ for 3 hours in a muffle furnace to prepare a 1-% mo-modified sulfur indium zinc photocatalyst. The preparation method of the pure sulfur indium zinc catalyst used for comparison is similar, and solution A does not need to be added in the reaction. Simulating sunlight irradiation by a 300W xenon lamp; 0.1g of catalyst was dissolved in 100mL of water and charged into a quartz reactor; the distance between the quartz reactor and the central position of the light source is 15cm, and the reaction process is carried out under the protection of N2; the H2 produced was detected by chromatography. The hydrogen production efficiency of the catalyst is shown in figure 2, the hydrogen production of the Mo modified sulfur indium zinc catalyst is stably increased within 2 hours by 10 percent, and the hydrogen production rate is 0.3mmol/g/h which is 3 times that of the pure sulfur indium zinc catalyst.
Example 3%/10% structural analysis of Mo-modified Sulfur indium Zinc catalyst.
Characterization of the 1%/10% mo-modified zinc indium sulfide catalysts prepared in examples 1 and 2 by XRD. As shown in FIG. 3, XRD results of 1% Mo modified sulfur indium zinc catalyst and 10% Mo modified sulfur indium zinc catalyst detected only one crystal phase of hexagonal sulfur indium zinc. This indicates that the Mo-modified sulfur indium zinc catalyst is a hexagonal sulfur indium zinc single crystal phase. It is noteworthy that the XRD diffraction peaks of both the Mo-modified sulfur indium zinc catalyst 1% and the 10% Mo-modified sulfur indium zinc catalyst were shifted to the high angle direction compared to the pure sulfur indium zinc catalyst, which indicates that Mo incorporation into the sulfur indium zinc unit cell results in lattice shrinkage. Since the radius of Mo ion is smaller than that of In ion and larger than that of Zn ion, it can be judged that Mo element partially replaces In ion In S-In-Zn unit cell.
Example 4% 10% photocatalytic hydrogen production cycle testing of mo-modified sulphur indium zinc catalyst.
Simulating sunlight irradiation by a 300W xenon lamp; 0.1g of catalyst is dissolved in 100mL of water and is filled into a quartz reactor; the distance between the quartz reactor and the central position of the light source is 15cm, and the reaction process is carried out under the protection of N2; the H2 produced was detected by chromatography. After 4 hours of reaction, the light was stopped, the H2 in the reactor was removed by introducing N2 for half an hour, the light reaction was continued for 4 hours, and the produced H2 was detected by chromatography. The test was repeated 5 times. The results of the photolytic hydrohydrogenesis cycle of 1-percent Mo-modified S-in-Zn catalyst and 10-percent Mo-modified S-in-Zn catalyst are shown in FIG. 4. 1% Mo modified Sulfur indium Zinc catalyst the catalyst hydrogen production rate after 5 cycles of testing was 2.25mmol/g/h, 90% of the fresh sample. 10% Mo modified Sulfur indium Zinc catalyst the catalyst hydrogen production rate after 5 cycles of testing was 0.26mmol/g/h, 87% of fresh sample.
Although the invention has been described and illustrated in some detail, it should be understood that various modifications may be made to the described embodiments or equivalents may be substituted, as will be apparent to those skilled in the art, without departing from the spirit of the invention.
Claims (8)
1. A Mo modified sulfur indium zinc photocatalyst is characterized in that: the Mo modified S-in-Zn photocatalyst is hexagonal ZnIn 2 S 4 Single crystal phase, mo element entering ZnIn 2 S 4 Unit cell, partially replacing In position In unit cell.
2. The Mo-modified sulfur indium zinc photocatalyst of claim 1, wherein: mo modification ratio example Range: mo and ZnIn 2 S 4 The molar ratio is 1-10%.
3. A synthetic method of a Mo modified sulfur indium zinc photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
step one, dissolving 0.1g of Mo powder in a solution (20 mL) of H2O2 with the concentration of 10 percent to obtain a coordinated Mo solution A;
dissolving indium nitrate, zinc nitrate (the molar ratio is 2:1) and thioacetamide in water (70 mL) to obtain a reaction liquid B;
thirdly, mixing the coordinated Mo solution A with the reaction solution B (controlling the addition amount of A and controlling the molar ratio of Mo to Zn to be 1-10%), mechanically stirring for 30 minutes, and then transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction at 180 ℃ for 12 hours;
step four, naturally cooling to room temperature, centrifugally separating solid powder obtained by the hydrothermal reaction, respectively washing with ethanol and water for 3 times, and drying overnight;
and fifthly, calcining the dried solid powder for 3 hours at 300 ℃ by using a muffle furnace to prepare the Mo modified sulfur indium zinc photocatalyst.
4. The method for synthesizing a Mo modified sulfur indium zinc photocatalyst as claimed in claim 3, wherein the method comprises the following steps: the amount of the h2o2 solution to be used in the first step is 20mL by 10%.
5. The method for synthesizing a Mo-modified sulfur indium zinc photocatalyst according to claim 3, wherein the method comprises the following steps: in the second step, the mol ratio of the indium nitrate to the zinc nitrate is 2:1, thioacetamide was dissolved in 70mL of water.
6. The method for synthesizing a Mo-modified sulfur indium zinc photocatalyst according to claim 3, wherein the method comprises the following steps: and in the third step, the adding amount of A is controlled so that Mo: the Zn molar ratio is controlled to be 1-10%.
7. An application of Mo modified S-in-Zn photocatalyst in hydrogen production by photolysis of water.
8. The application of the Mo modified sulfur indium zinc photocatalyst in hydrogen production by photolysis of water according to claim 7, wherein the Mo modified sulfur indium zinc photocatalyst is prepared by the following steps: simulating sunlight irradiation by a 300W xenon lamp; 0.1g of catalyst was dissolved in 100mL of water and charged into a quartz reactor; the distance between the quartz reactor and the central position of the light source is 15cm, and the reaction process is carried out under the protection of N2; the H2 produced was detected by chromatography.
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- 2022-09-28 CN CN202211191797.9A patent/CN115709079A/en active Pending
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