CN117482964A - TiO (titanium dioxide) 2 Preparation method of NiS composite photocatalytic material - Google Patents
TiO (titanium dioxide) 2 Preparation method of NiS composite photocatalytic material Download PDFInfo
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- CN117482964A CN117482964A CN202311460061.1A CN202311460061A CN117482964A CN 117482964 A CN117482964 A CN 117482964A CN 202311460061 A CN202311460061 A CN 202311460061A CN 117482964 A CN117482964 A CN 117482964A
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 20
- 239000004408 titanium dioxide Substances 0.000 title claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 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
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 238000005286 illumination Methods 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 230000001112 coagulating effect Effects 0.000 claims description 3
- 239000000084 colloidal system Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 23
- 239000001257 hydrogen Substances 0.000 abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 23
- 238000004519 manufacturing process Methods 0.000 abstract description 20
- 239000003054 catalyst Substances 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 5
- 230000006798 recombination Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 5
- 230000004913 activation Effects 0.000 abstract description 3
- 239000002800 charge carrier Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000002256 photodeposition Methods 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000006163 transport media Substances 0.000 description 1
Classifications
-
- 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
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
Abstract
The invention discloses a TiO 2 The invention relates to a preparation method of a NiS composite photocatalytic material, belonging to the technical field of photocatalytic material preparation. The invention solves the problems of TiO 2 The light utilization rate is low, the photo-generated carrier recombination rate is high, and the technical problem of poor photo-catalytic hydrogen production performance is caused. The invention prepares TiO by sol-gel method 2 Photocatalytic material, preparing NiS photocatalytic material by alcohol thermal method, and finally preparing TiO by photo-deposition method 2 A NiS composite photocatalytic material. The invention is characterized in that TiO 2 The catalyst is loaded on the catalyst to enhance the active site, reduce the activation energy, capture charge carriers and inhibit the recombination of photo-generated electrons and holes to promote oxygenAnd (3) carrying out chemical reduction reaction. NiS is a transition metal oxide and can replace expensive noble metal cocatalysts. NiS can reduce TiO 2 The charge recombination rate of the catalyst is improved, the photocatalytic activity is improved, and the hydrogen production performance is greatly improved. The photocatalytic material prepared by the invention has uniform microstructure, good photocatalytic hydrogen production activity, the hydrogen production amount of one hour with the highest performance is 83.55mmoL/g, the hydrogen production amount of 4 hours is 260.97mmoL/g, and the hydrogen production rate is 64.24mmoL/g/h.
Description
Technical Field
The invention belongs to the field of photocatalytic material preparation, and in particular relates to TiO 2 Preparation of NiS composite photocatalytic material and test of photocatalytic hydrogen production performance.
Background
Development of high-efficiency photocatalytic hydrogen-generating materials requires realization of rapid electron transfer and efficient interfacial catalytic reaction to promote hydrogen generation. In addition to expensive noble metals, lower cost and abundant non-noble metals are also widely considered for use as electron transport media to improve the performance of the photocatalyst. However, this limits the improvement of photocatalytic performance due to the lack of almost all non-noble metals with the necessary interfacial catalytically active sites to support the hydrogen evolution reaction. Therefore, the development of new interfacial active sites on metal modified photocatalysts is of great importance.
By forming a metal oxide layer on TiO 2 The NiS nano particles are compounded on the basis of the nano particles, so that the active site can be enhanced, and meanwhile, the activation energy is reduced, the charge carriers are captured, and the combination of photo-generated electrons and holes is inhibited to promote the oxidation-reduction reaction, so that the photo-catalytic activity is improved, and the hydrogen production performance is greatly improved.
Disclosure of Invention
The invention mainly solves the problem of TiO under the prior art condition 2 The method has low sunlight utilization rate and high photo-generated carrier recombination rate, so that the problem of poor photo-catalytic hydrogen production performance is solved. The invention prepares TiO by sol-gel method 2 Photocatalytic material, preparing NiS photocatalytic material by alcohol thermal method, and finally preparing TiO by photo-deposition method 2 A NiS composite photocatalytic material. The composite material forms a heterostructure, which is beneficial to improving the photocatalytic performance.
TiO (titanium dioxide) 2 The preparation method of the NiS composite photocatalytic material is characterized by comprising the following specific steps:
1. TiO (titanium dioxide) 2 Photocatalytic material:
in-situ generation of TiO by taking titanium isopropoxide as precursor 2 Mixing 10mL of titanium isopropoxide with 10-30 mL of absolute ethyl alcohol, marking the obtained solution as A solution, marking the mixed solution of 3mL of deionized water and 10mL of absolute ethyl alcohol as B solution, and separatingStirring for 30min, dropwise adding 2mL glacial acetic acid into solution A to promote gel formation, continuously stirring, dropwise and slowly adding solution B into solution A, slowly changing the solution from transparent clear to white turbid colloid, mixing sol solution with pH of about 6.5 to form weak acidity, completely coagulating sol within 5min after dropwise adding, aging gel at room temperature for 6h, collecting 40g aged gel, loading into 100mL reaction kettle, reacting at 100-140deg.C for 20-24 h, naturally cooling, washing for several times, vacuum drying, grinding into powder with agate mortar to obtain TiO 2 Sample powder.
2. NiS photocatalytic material:
nickel nitrate and thiourea are used as precursors, and a one-step alcohol heating method is adopted to prepare the nickel sulfide photocatalytic material: adding 0.58g of nickel nitrate and 0.3g of thiourea into a solution containing 70ml of glycol, stirring for 30min at room temperature, transferring the solution into a 100ml hydrothermal reaction kettle, carrying out alcohol heating at 160-200 ℃ for 12h, cooling, filtering, washing, and then carrying out vacuum drying at 60 ℃ for 12h to obtain powder, namely the NiS photocatalytic material.
3. TiO (titanium dioxide) 2 NiS photocatalytic material:
100mg of TiO to be prepared 2 Mixing the photocatalytic material with 10-40 mg of NiS photocatalytic material in 40ml of glycol solution, stirring under illumination under 400W xenon lamp for 2-4 h, centrifuging, washing with water and absolute ethanol for 3 times respectively, and vacuum drying at 60deg.C to obtain powder of TiO 2 /NiS photocatalytic material.
Preparation of TiO in step one 2 The added absolute ethyl alcohol is 10-30 mL.
Preparation of TiO in step one 2 The heat preservation temperature of the steel is 100-140 ℃.
Preparation of TiO in step one 2 The heat preservation time of the steel is 20-24 h.
The temperature of the heat preservation of the NiS prepared in the second step is 160-200 ℃.
Preparing TiO in the third step 2 The NiS content of the NiS composite material is 10-40 mg.
Preparing TiO in the third step 2 The illumination time of the/NiS composite material is 2-4 h.
The beneficial effects of the invention are as follows:
the invention is characterized in that TiO 2 The loading of the cocatalyst can enhance the active site, reduce the activation energy, capture charge carriers and inhibit the recombination of photo-generated electrons and holes to promote the oxidation-reduction reaction. NiS is a transition metal oxide and can replace expensive noble metal cocatalysts. NiS can reduce TiO 2 Thereby improving the photocatalytic activity and greatly improving the hydrogen production performance.
TiO prepared by the invention 2 The NiS photocatalytic material has higher photocatalytic hydrogen production performance. The light source was a 300W xenon lamp and 3mg of catalyst was suspended in aqueous lactic acid (50 mL,20 vol%) for hydrogen generation (H) 2 ) Gas, 3wt% of H was added to the reactant solution 2 PtCl 6 And (3) irradiating the aqueous solution for 30min under a xenon lamp to enable platinum to be deposited on the surface of the catalyst, and carrying out a hydrogen production experiment on the catalyst in a photocatalytic hydrogen production system, wherein data are collected every 1 hour.
The photocatalytic material prepared by the invention has uniform microstructure, good photocatalytic hydrogen production activity, the hydrogen production amount of one hour with the highest performance is 83.55mmoL/g, the hydrogen production amount of 4 hours is 260.97mmoL/g, and the hydrogen production rate is 64.24mmoL/g/h. Thus the TiO prepared by the invention 2 The NiS composite photocatalytic material has higher hydrogen production performance.
Description of the drawings:
FIG. 1 is an XRD pattern of the photocatalytic material synthesized in the examples;
FIG. 2 is an ultraviolet-visible absorption spectrum of the photocatalytic material synthesized in the examples;
FIG. 3 is a photo-catalytic hydrogen production diagram of the photo-catalytic material synthesized in the example;
FIG. 4 is a photocatalytic hydrogen production cycle test chart of the photocatalytic material synthesized in the example;
fig. 5 is an SEM image of the photocatalytic material synthesized in the example.
Detailed Description
The invention will be described in further detail with reference to specific examples.
Example 1:
1. TiO (titanium dioxide) 2 Photocatalytic material:
in-situ generation of TiO by taking titanium isopropoxide as precursor 2 Mixing 10mL of titanium isopropoxide with 20mL of absolute ethyl alcohol, marking the obtained solution as solution A, marking the mixed solution of 3mL of deionized water and 10mL of absolute ethyl alcohol as solution B, separately stirring for 30min, dropwise adding 2mL of glacial acetic acid into the solution A to promote gel formation, continuously stirring, slowly dropwise adding the solution B into the solution A, slowly changing the solution from transparent clear to white turbid colloid, mixing the sol solution with pH of about 6.5 to be weak acidity, completely coagulating the sol within 5min after the dropwise adding, and aging the gel for 6h at room temperature. Taking 40g of aged gel, placing the gel into a 100ml reaction kettle, reacting for 18 hours at 120 ℃, naturally cooling a sample, washing for multiple times, vacuum drying, and grinding into powder by an agate mortar to obtain TiO 2 Sample powder.
2. NiS photocatalytic material:
nickel nitrate and thiourea are used as precursors, and a one-step alcohol heating method is adopted to prepare the nickel sulfide photocatalytic material: 0.58g of nickel nitrate and 0.3g of thiourea were added to a solution containing 70ml of ethylene glycol. Stirring at room temperature for 30min, transferring to a 100ml hydrothermal reaction kettle, heating with alcohol at 180 ℃ for 12h, cooling, filtering, washing, and vacuum drying at 60 ℃ for 12h to obtain powder which is the NiS photocatalytic material.
3. TiO (titanium dioxide) 2 NiS photocatalytic material:
100mg of TiO to be prepared 2 Mixing the photocatalytic material with 30mg of NiS photocatalytic material in 40ml of glycol solution, stirring under light under 400W xenon lamp for 3 hr, centrifuging, washing with water and absolute ethanol for 3 times, and vacuum drying at 60deg.C to obtain powder of TiO 2 /NiS photocatalytic material.
Example 2:
100mg of TiO as described above 2 The photocatalytic material was mixed with 10mg of the NiS photocatalytic material in a solution containing 40ml of ethylene glycol, the other being the same. Named TiO 2 NiS-10 was used as a comparative experiment.
Claims (7)
1. TiO (titanium dioxide) 2 The preparation method of the NiS composite photocatalytic material is characterized by comprising the following specific steps:
1. TiO (titanium dioxide) 2 Photocatalytic material:
in-situ generation of TiO by taking titanium isopropoxide as precursor 2 Mixing 10mL of titanium isopropoxide with 10-30 mL of absolute ethyl alcohol, marking the obtained solution as A solution, marking 3mL of deionized water and 10mL of absolute ethyl alcohol as B solution, separately stirring for 30min, dropwise adding 2mL of glacial acetic acid into the A solution to promote gel formation, continuously stirring, gradually dropwise adding the B solution into the A solution, slowly changing the solution into white turbid colloid from transparent clear solution, mixing the sol solution to have pH of about 6.5 and weak acidity, completely coagulating the sol within 5min after dropwise adding, aging the gel at room temperature for 6h, filling 40g of aged gel into a 100mL reaction kettle, reacting for 20-24 h at 100-140 ℃, naturally cooling a sample, repeatedly washing, vacuum drying, grinding into powder by an agate mortar to obtain TiO 2 Sample powder.
2. NiS photocatalytic material:
nickel nitrate and thiourea are used as precursors, and a one-step alcohol heating method is adopted to prepare the nickel sulfide photocatalytic material: adding 0.58g of nickel nitrate and 0.3g of thiourea into a solution containing 70ml of glycol, stirring for 30min at room temperature, transferring the solution into a 100ml hydrothermal reaction kettle, carrying out alcohol heating at 160-200 ℃ for 12h, cooling, filtering, washing, and then carrying out vacuum drying at 60 ℃ for 12h to obtain powder, namely the NiS photocatalytic material.
3. TiO (titanium dioxide) 2 NiS photocatalytic material:
100mg of TiO to be prepared 2 Mixing the photocatalytic material with 10-40 mg of NiS photocatalytic material in 40ml of glycol solution, stirring under illumination under 400W xenon lamp for 2-4 h, centrifuging, washing with water and absolute ethanol for 3 times respectively, and vacuum drying at 60deg.C to obtain powder of TiO 2 /NiS photocatalytic material.
2. The TiO according to claim 1 2 Preparation of NiS composite photocatalytic materialThe method is characterized in that TiO is prepared in the first step 2 The added absolute ethyl alcohol is 10-30 mL.
3. The TiO according to claim 1 2 The preparation method of the NiS composite photocatalytic material is characterized in that TiO is prepared in the first step 2 The heat preservation temperature of the steel is 100-140 ℃.
4. The TiO according to claim 1 2 The preparation method of the NiS composite photocatalytic material is characterized in that TiO is prepared in the first step 2 The heat preservation time of the steel is 20-24 h.
5. The TiO according to claim 1 2 The preparation method of the NiS composite photocatalytic material is characterized in that the heat preservation temperature of the NiS prepared in the second step is 160-200 ℃.
6. The TiO according to claim 1 2 The preparation method of the NiS composite photocatalytic material is characterized by preparing TiO in the third step 2 The NiS content of the NiS composite material is 10-40 mg.
7. The TiO according to claim 1 2 The preparation method of the NiS composite photocatalytic material is characterized by preparing TiO in the third step 2 The illumination time of the/NiS composite material is 2-4 h.
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