CN108607589B - TiN-In2S3Preparation method and application of nano composite photocatalyst - Google Patents
TiN-In2S3Preparation method and application of nano composite photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims description 11
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000002077 nanosphere Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- UKCIUOYPDVLQFW-UHFFFAOYSA-K indium(3+);trichloride;tetrahydrate Chemical compound O.O.O.O.Cl[In](Cl)Cl UKCIUOYPDVLQFW-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 8
- 238000000354 decomposition reaction Methods 0.000 claims description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 230000002431 foraging effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 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 4
- 239000002131 composite material Substances 0.000 abstract description 10
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 description 11
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000004310 lactic acid Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000006303 photolysis reaction Methods 0.000 description 5
- 230000015843 photosynthesis, light reaction Effects 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 235000014655 lactic acid Nutrition 0.000 description 4
- 238000012876 topography Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000003421 catalytic decomposition reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
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- 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
- B01J27/24—Nitrogen compounds
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a TiN-In2S3The preparation method of the nano composite photocatalyst comprises the following steps: adding titanium nitride nanospheres into absolute ethyl alcohol, adding hexadecyl trimethyl ammonium bromide after ultrasonic dispersion, stirring, adding indium chloride tetrahydrate and thioacetamide, stirring uniformly, condensing and refluxing at constant temperature of 95 ℃ to obtain turbid liquid, centrifugally separating the turbid liquid, and drying the separated solid matter to obtain TiN-In2S3A nano composite photocatalyst; the invention provides a preparation method of a nanometer flower-shaped spherical composite photocatalyst with adjustable morphology and nanometer size, and the preparation method has universality.
Description
Technical Field
The invention relates to the technical field of photocatalysis, In particular to TiN-In2S3Preparation method of nano composite photocatalyst and nano composite photocatalystThe application thereof.
Background
With the rapid development of economy and the dramatic increase of population, the conventional exhaustion of fossil energy and the corresponding environmental problems are the problems faced by chemists and technical experts in the 21 st century. Solar energy is a clean, pollution-free and infinitely renewable energy source that can meet the present and future human needs for energy. Currently, many semiconductors have been developed to have the ability to produce hydrogen by photocatalytic decomposition of water. Hydrogen is a clean energy with good combustion performance and high energy conversion efficiency, and is considered as the most ideal clean energy. Therefore, in recent years, hydrogen production by photocatalytic decomposition of water has received increasing attention from researchers.
The semiconductor indium sulfide has attracted much attention because of its unique physical and chemical properties such as optical and electrical properties. In of different structures and morphologies In recent years2S3Nanomaterials have also been widely used in the fields of optical waveguides, dry cells, photovoltaic generators, and the like. The indium sulfide has good photocatalytic performance in the field of nano photocatalysis due to large specific surface area, high reaction activity and strong selectivity. However, the hydrogen production activity is limited due to the defects of rapid recombination of photo-generated electron holes and the like, so that an indium sulfide composite material for effectively promoting the separation of the photo-generated electron holes is required to be developed so as to improve the photocatalytic activity.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art: provides TiN-In with good photolysis water hydrogen production activity2S3A method for preparing a nano composite photocatalyst.
The technical solution of the invention is as follows: TiN-In2S3The preparation method of the nano composite photocatalyst comprises the following steps: adding titanium nitride nanospheres into absolute ethyl alcohol, adding hexadecyl trimethyl ammonium bromide after ultrasonic dispersion, stirring, adding indium chloride tetrahydrate and thioacetamide, stirring uniformly, condensing and refluxing at constant temperature of 95 ℃ to obtain turbid liquid, centrifugally separating the turbid liquid, and drying the separated solid matter to obtain TiN-In2S3A nano composite photocatalyst.
The method specifically comprises the following steps:
1) weighing 1-10mg of titanium nitride nanospheres, adding 100ml of absolute ethanol, and performing ultrasonic dispersion to obtain a suspension C;
2) weighing 10-100mg of hexadecyl trimethyl ammonium bromide, adding into the suspension C, and stirring to obtain a suspension D;
3) and weighing 2-5mmol of indium chloride tetrahydrate and 3-8mmol of thioacetamide, respectively adding into the suspension D, and stirring to obtain a suspension E.
4) Condensing and refluxing the suspension E at 95 ℃ for 2h to obtain suspension F, centrifugally separating the suspension F, and drying the obtained solid substance In a 60 ℃ oven to obtain TiN-In2S3A nano composite photocatalyst.
The titanium nitride nanospheres are obtained by heating and cooling titanium dioxide nanospheres in an ammonia atmosphere.
As optimization, the preparation method of the titanium nitride nanosphere comprises the following steps: and (3) placing 50-300mg of titanium dioxide nanospheres in a corundum boat, heating the corundum boat to 600-800 ℃ in an ammonia atmosphere, preserving heat for 3-5h, and cooling to obtain the titanium nitride nanospheres.
The preparation method of the titanium dioxide nanosphere comprises the following steps:
1) weighing 5-10mmol of hexadecylamine, adding the hexadecylamine into 50-200mL of absolute ethanol, adding 1-3 mL of deionized water, and stirring at the rotating speed of 400-700 r/min for 20-60min to obtain a solution A;
2) adding 3-5mL of isopropyl titanate into the solution A, stirring at the rotating speed of 300r/min for 1-10min to obtain a suspension B, and placing the suspension B in a room for aging for 12-24 h;
3) separating the titanium dioxide in the suspension B by a centrifugal separation method, wherein the centrifugal rotation speed is 5000-.
The invention has the beneficial effects that: the composite photocatalyst prepared by the invention has good nano size, so that the composite photocatalyst has larger specific surface area, can provide more active sites, and further improves the activity of the catalyst for photolyzing water to produce hydrogen. The invention provides a preparation method of a nanometer flower-shaped spherical composite photocatalyst with adjustable morphology and nanometer size, and the preparation method has universality. The preparation method has the advantages of simple operation, simple equipment, more uniform product and shorter overall reaction time. The hydrogen production activity of the blank visible light catalytic decomposition water of indium sulfide is poor, but the hydrogen production amount is obviously improved after the blank visible light catalytic decomposition water is compounded with titanium nitride, and the activity is improved by nearly one time compared with that of the blank indium sulfide. Fully embodies the excellent hydrogen production performance of the prepared composite catalyst. Titanium nitride is a transition metal nitride having metalloid properties, and has excellent characteristics such as high melting point, high hardness, and good conductivity. After the titanium nitride is contacted with the indium sulfide, photoproduction electrons are transferred to the titanium nitride after being excited from a conduction band of the indium sulfide, and a Schottky barrier is formed due to the difference between Fermi energy levels of the two materials, so that the service life of photoproduction electron holes is prolonged, and the photocatalytic water decomposition efficiency of the indium sulfide is improved.
Drawings
FIG. 1: the X-ray diffraction pattern of the example is shown.
FIG. 2: the surface topography of the titanium nitride nanosphere is shown.
FIG. 3: TiN-In prepared for example 12S3The surface topography of the nano composite photocatalyst.
FIG. 4: TiN-In prepared for example 22S3The surface topography of the nano composite photocatalyst.
FIG. 5: the hydrogen production rate diagram of visible light photolysis of water in lactic acid aqueous solution is shown by the catalyst prepared in the example.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1:
1) weighing 8.2mmol of hexadecylamine, adding the hexadecylamine into 100mL of absolute ethyl alcohol, adding 1.6 mL of deionized water by using a pipette gun, and stirring at the rotating speed of 500 r/min for 30min to obtain a solution A.
2) And (3) transferring 4.45mL of isopropyl titanate into the solution A by using a liquid transfer gun, adjusting the rotating speed to 300r/min, stirring for 3min to obtain a suspension B, and placing the suspension B in a room for aging for 18 h.
3) Separating the titanium dioxide in the suspension B by a centrifugal separation method, wherein the centrifugal rotation speed is 7000r/min, and drying the separated solid substance in a drying oven at 60 ℃ to obtain the titanium dioxide nanospheres.
4) 100mg of titanium dioxide nanospheres are spread in a corundum boat with the diameter of 75 multiplied by 13 multiplied by 9mm, the corundum boat is placed in a high-temperature tube furnace, the corundum boat is heated to 700 ℃ in high-purity ammonia gas with the flow rate of 200 standard milliliters per minute by 99.99 weight percent, the temperature is kept for 4 hours, and the titanium nitride nanospheres are obtained after furnace cooling.
5) Weighing 1.4mg of titanium nitride nanospheres, placing the titanium nitride nanospheres in a round-bottom flask, adding 100ml of absolute ethyl alcohol, and performing ultrasonic dispersion for 10min to obtain suspension C. And weighing 50mg of hexadecyl trimethyl ammonium bromide, adding into the suspension C subjected to ultrasonic dispersion, and stirring for 15min to obtain a suspension D. 2.4mmol of indium chloride tetrahydrate and 4.8mmol of thioacetamide are weighed and respectively added into the suspension D, and the suspension E is obtained after stirring for 30 min.
6) Putting the round-bottom flask containing the suspension E into a constant-temperature oil bath, carrying out condensation reflux at 95 ℃ for 2h to obtain a suspension F, carrying out centrifugal separation on the suspension F, putting the obtained solid substance into a 60 ℃ oven, and drying to obtain TiN-In2S3The nanometer flower spherical core-shell structure composite photocatalyst.
The performance test of hydrogen produced by photocatalytic decomposition at room temperature: adding 20mg of TiN-In into 80ml of 10wt% aqueous solution of lactic acid2S3The catalyst of the nano composite photocatalyst is moved into a quartz glass reactor after being subjected to ultrasonic treatment for 30min, and circulating water at the temperature of 5 ℃ is used for keeping the temperature of the reactor constant. And irradiating the quartz reactor with visible light of more than 420nm, and performing gas chromatography on-line analysis to obtain a curve of the amount of hydrogen generated by photocatalytic water decomposition along with the irradiation time.
Example 2:
1) weighing 8.2mmol of hexadecylamine, adding the hexadecylamine into 100mL of absolute ethyl alcohol, adding 1.6 mL of deionized water by using a pipette gun, and stirring at the rotating speed of 500 r/min for 30min to obtain a solution A.
2) And (3) transferring 4.45mL of isopropyl titanate into the solution A by using a liquid transfer gun, adjusting the rotating speed to 300r/min, stirring for 3min to obtain a suspension B, and placing the suspension B in a room for aging for 18 h.
3) Separating the titanium dioxide in the suspension B by a centrifugal separation method, wherein the centrifugal rotation speed is 7000r/min, and drying the separated solid substance in a drying oven at 60 ℃ to obtain the titanium dioxide nanospheres.
4) 100mg of titanium dioxide nanospheres are spread in a corundum boat with the diameter of 75 multiplied by 13 multiplied by 9mm, the corundum boat is placed in a high-temperature tube furnace, the corundum boat is heated to the range of 700 ℃ in 99.99% high-purity ammonia gas (the flow is 200 standard milliliters per minute), heat preservation is carried out for 4 hours, and the titanium nitride nanospheres are obtained after furnace cooling.
5) Weighing 4.2mg of titanium nitride nanospheres into a round-bottom flask, adding 100ml of absolute ethyl alcohol, and performing ultrasonic dispersion for 10min to obtain suspension C. And weighing 50mg of hexadecyl trimethyl ammonium bromide, adding into the suspension C subjected to ultrasonic dispersion, and stirring for 15min to obtain a suspension D. 2.4mmol of indium chloride tetrahydrate and 4.8mmol of thioacetamide are weighed and respectively added into the suspension D, and the suspension E is obtained after stirring for 30 min.
6) Putting the round-bottom flask containing the suspension E into a constant-temperature oil bath, carrying out condensation reflux at 95 ℃ for 2h to obtain a suspension F, carrying out centrifugal separation on the suspension F, putting the obtained solid substance into a 60 ℃ oven, and drying to obtain TiN-In2S3The nanometer flower spherical core-shell structure composite photocatalyst.
The performance test of hydrogen produced by photocatalytic decomposition at room temperature: adding 20mg of TiN-In into 80ml of 10wt% aqueous solution of lactic acid2S3The catalyst of the nano composite photocatalyst is moved into a quartz glass reactor after being subjected to ultrasonic treatment for 30min, and circulating water at the temperature of 5 ℃ is used for keeping the temperature of the reactor constant. And irradiating the quartz reactor with visible light of more than 420nm, and performing gas chromatography on-line analysis to obtain a curve of the amount of hydrogen generated by photocatalytic water decomposition along with the irradiation time.
As shown in fig. 1-5, fig. 1: curve 1 In FIG. 1 is the TiN-In prepared In example 2 for the X-ray diffraction pattern2S3Nano composite photocatalystThe X-ray diffraction pattern of (a). Curve 2 is the TiN-In prepared In example 12S3X-ray diffraction pattern spectrogram of the nano composite photocatalyst. Curve 3 is an X-ray diffraction pattern of blank indium sulfide. Curve 4 is the X-ray diffraction pattern of the titanium nitride nanospheres.
As can be seen from FIGS. 1 to 5, the composite photocatalyst prepared by the method can be used for preparing photocatalysts with different shapes and shapes according to different qualities of the added titanium nitride, and has shape controllability and universality. Meanwhile, the hydrogen production of the blank indium sulfide is only 11.73 micromoles/gram in two hours, and the maximum hydrogen production of the composite photocatalyst prepared by the method can reach 21.17 micromoles/gram. The activity is improved by nearly one time, the hydrogen production activity is obviously improved, and the method has wide research and application prospects.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.
Claims (5)
1. TiN-In2S3The preparation method of the nano composite photocatalyst is characterized by comprising the following steps: the method comprises the following steps: adding titanium nitride nanospheres into absolute ethyl alcohol, adding hexadecyl trimethyl ammonium bromide after ultrasonic dispersion, stirring, adding indium chloride tetrahydrate and thioacetamide, stirring uniformly, condensing and refluxing at constant temperature of 95 ℃ to obtain turbid liquid, centrifugally separating the turbid liquid, and drying the separated solid matter to obtain TiN-In2S3A nano composite photocatalyst;
the method specifically comprises the following steps:
1) weighing 1-10mg of titanium nitride nanospheres, adding 100ml of absolute ethanol, and performing ultrasonic dispersion to obtain a suspension C;
2) weighing 10-100mg of hexadecyl trimethyl ammonium bromide, adding into the suspension C, and stirring to obtain a suspension D;
3) weighing 2-5mmol of indium chloride tetrahydrate and 3-8mmol of thioacetamide, respectively adding into the suspension D, and stirring to obtain a suspension E;
4) condensing and refluxing the suspension E at 95 ℃ for 2h to obtain suspension F, centrifugally separating the suspension F, and drying the obtained solid substance In a 60 ℃ oven to obtain TiN-In2S3A nano composite photocatalyst.
2. The TiN-In of claim 12S3The preparation method of the nano composite photocatalyst is characterized by comprising the following steps: the titanium nitride nanospheres are obtained by heating and cooling titanium dioxide nanospheres in an ammonia atmosphere.
3. The TiN-In of claim 22S3The preparation method of the nano composite photocatalyst is characterized by comprising the following steps: the preparation method of the titanium nitride nanosphere comprises the following steps: and (3) placing 50-300mg of titanium dioxide nanospheres in a corundum boat, heating the corundum boat to 600-800 ℃ in an ammonia atmosphere, preserving heat for 3-5h, and cooling to obtain the titanium nitride nanospheres.
4. The TiN-In of claim 32S3The preparation method of the nano composite photocatalyst is characterized by comprising the following steps: the preparation method of the titanium dioxide nanosphere comprises the following steps:
1) weighing 5-10mmol of hexadecylamine, adding the hexadecylamine into 50-200mL of absolute ethanol, adding 1-3 mL of deionized water, and stirring at the rotating speed of 400-700 r/min for 20-60min to obtain a solution A;
2) adding 3-5mL of isopropyl titanate into the solution A, stirring at the rotating speed of 300r/min for 1-10min to obtain a suspension B, and placing the suspension B in a room for aging for 12-24 h;
3) separating the titanium dioxide in the suspension B by a centrifugal separation method, wherein the centrifugal rotation speed is 5000-.
5. TiN-In prepared by the method of claim 12S3The application of the nano composite photocatalyst is characterized in that: the method is applied to photocatalytic water decomposition for hydrogen production.
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| CN115367785A (en) * | 2022-08-23 | 2022-11-22 | 安徽工程大学 | High-efficiency photocatalyst micro/nano-thorn spherical indium sulfide and preparation method and application thereof, indium sulfide composite membrane and preparation method and application thereof |
Citations (5)
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