CN108607589A - TiN-In2S3The preparation method and applications of nano composite photo-catalyst - Google Patents
TiN-In2S3The preparation method and applications of nano composite photo-catalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 31
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 50
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000011807 nanoball Substances 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 11
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000009833 condensation Methods 0.000 claims abstract description 3
- 230000005494 condensation Effects 0.000 claims abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 239000004408 titanium dioxide Substances 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 239000002077 nanosphere Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 8
- 239000010431 corundum Substances 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910003087 TiOx Inorganic materials 0.000 claims 1
- 229910052738 indium Inorganic materials 0.000 claims 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 12
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 235000014655 lactic acid Nutrition 0.000 description 6
- 239000004310 lactic acid Substances 0.000 description 6
- 238000006303 photolysis reaction Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000015843 photosynthesis, light reaction Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011805 ball Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- 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
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of TiN In2S3The preparation method of nano composite photo-catalyst, includes the following steps：Titanium nitride nano ball is added in absolute ethyl alcohol, cetyl trimethylammonium bromide is added after ultrasonic disperse, stirring, it adds four chloride hydrate indiums and thioacetamide stirs evenly and obtains suspension after 95 DEG C of constant-temperature condensations flow back, the suspension is centrifuged, TiN In are obtained after isolated solid matter is dried2S3Nano composite photo-catalyst；The present invention provides a kind of preparation methods of the regulatable nanometer flower ball-shaped composite photo-catalyst of pattern, nano-scale, have universality.
Description
Technical field
The present invention relates to photocatalysis technology fields, are especially a kind of TiN-In2S3The preparation side of nano composite photo-catalyst
Method and its application.
Background technology
With the violent growth of economic fast development and population, traditional fossil energy exhaustion and corresponding environment are asked
Topic is 21 century chemist and technical specialist's problem encountered.Solar energy is a kind of cleaning, pollution-free and unlimited renewable
Clean energy resource, it disclosure satisfy that demand of the current and following mankind for the energy.Currently, many semiconductors are studied out
Performance with photocatalytic hydrogen production by water decomposition.Hydrogen is a kind of cleaning energy that a kind of combustibility is good, energy conversion efficiency is high
Source is considered as optimal clean energy resource.Therefore, photocatalytic hydrogen production by water decomposition is increasingly closed by researcher in recent years
Note.
Semiconductor indium sulfide gets more and more people's extensive concerning because of physicochemical properties such as its unique optics, electricity.In recent years,
The In of different structure and pattern2S3Nano material is also widely used to the fields such as photocon, dry cell and photovoltaic generator.
Indium sulfide nano-photo catalytic field due to its large specific surface area, reactivity is high, selectivity is strong, have good photocatalytic
Energy.But its photo-generate electron-hole it is quick compound the shortcomings of enable it produce hydrogen activity being restricted, it is therefore necessary to develop one
Kind is effectively promoted the indium sulfide composite material of photo-generate electron-hole separation to promote its photocatalytic activity.
Invention content
The technical problem to be solved by the present invention is to the shortcomings that overcoming the above prior art：It provides a kind of with good
The TiN-In of photodissociation aquatic products hydrogen activity2S3The preparation method of nano composite photo-catalyst.
Technical solution of the invention is as follows：A kind of TiN-In2S3The preparation method of nano composite photo-catalyst, including
Following steps：Titanium nitride nano ball is added in absolute ethyl alcohol, cetyl trimethylammonium bromide is added after ultrasonic disperse, stirs
It mixes, adds four chloride hydrate indiums and thioacetamide stirs evenly and obtains suspension, centrifugation point after 95 DEG C of constant-temperature condensations flow back
From the suspension, TiN-In is obtained after isolated solid matter is dried2S3Nano composite photo-catalyst.
Specifically include following steps：
1）1-10mg titanium nitride nano balls are weighed, 100-300ml absolute ethyl alcohols are added, ultrasonic disperse obtains suspension C；
2）It weighs 10-100mg cetyl trimethylammonium bromides to be added in the suspension C, suspension D is obtained after stirring；
3）The thioacetamide of the four chloride hydrate indiums and 3-8mmol that weigh 2-5mmol is separately added into the suspension D, is stirred
Suspension E is obtained after mixing.
4）The suspension E is obtained into suspension F after 95 DEG C of condensing reflux 2h, centrifuges the suspension F, will
To solid matter be put into 60 DEG C of baking oven it is dry after obtain TiN-In2S3Nano composite photo-catalyst.
The titanium nitride nano ball obtains after heating cooling in ammonia atmosphere by titanium dioxide nano-sphere.
As an optimization, the preparation method of the titanium nitride nano ball is：50-300mg titanium dioxide nano-spheres are taken to be placed in just
In beautiful boat, corundum boat is heated to 600-800 DEG C in ammonia atmosphere, and keep the temperature 3-5h, can be obtained titanium nitride after cooling receives
Rice ball.
The preparation method of the titanium dioxide nano-sphere is：
1）The cetylamine for weighing 5-10mmol is added in 50-200mL absolute ethyl alcohols, 1-3 ml deionized waters is added, with 400-
After the rotating speed stirring 20-60min of 700 r/min, solution A is obtained；
2）It takes 3-5mL isopropyl titanates to be added in solution A, suspension B is obtained after 100-300r/min rotating speeds stirring 1-10min,
And suspension B is positioned over indoor aging 12-24h；
3）The titanium dioxide in suspension B, centrifugal rotational speed 5000-8000r/min, after separation are detached by centrifugal separation
Solid matter be put into 50-80 DEG C of drying in oven after obtain titanium dioxide nano-sphere.
The beneficial effects of the invention are as follows：Composite photo-catalyst prepared by the present invention has good nano-scale, therefore
With larger specific surface area, it is capable of providing more active site, and then improve the photodissociation aquatic products hydrogen activity of catalyst.This hair
A kind of bright preparation method for providing pattern, the regulatable nanometer flower ball-shaped composite photo-catalyst of nano-scale, has pervasive
Property.Easy to operate, equipment needed for the preparation method is simple, and products therefrom is more uniform, and the W-response time is shorter.Blank
The visible light catalytic decomposition aquatic products hydrogen activity of indium sulfide is poor, but it is had with the compound rear hydrogen output of titanium nitride and is significantly carried
Height, activity connect by about one time compared with the promotion of blank indium sulfide.The excellent H2-producing capacity of prepared composite catalyst is fully demonstrated.Nitrogen
It is a kind of transition metal nitride with metal-like properties to change titanium, has the excellent spies such as high, the big, good conductivity of hardness of fusing point
Sign.After titanium nitride is in contact with indium sulfide, light induced electron is transferred to titanium nitride after being excited from the conduction band of indium sulfide, due to two kinds
Difference between the fermi level of material form Schottky barrier to promoted photo-generate electron-hole there are the service life, and then improve
The photochemical catalyzing efficiency of indium sulfide.
Description of the drawings
Fig. 1：For X-ray diffractogram spectrogram in embodiment.
Fig. 2：For titanium nitride nano ball surface shape appearance figure.
Fig. 3：The TiN-In prepared for embodiment 12S3Nano composite photo-catalyst surface topography map.
Fig. 4：The TiN-In prepared for embodiment 22S3Nano composite photo-catalyst surface topography map.
Fig. 5：For the made catalyst of embodiment in lactic acid aqueous solution visible light photolysis water hydrogen rate diagram.
Specific implementation mode
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Apply example.
Embodiment 1：
1）The cetylamine for weighing 8.2mmol is added in 100mL absolute ethyl alcohols, and 1.6 ml deionized waters are added using liquid-transfering gun, with
After the rotating speed stirring 30min of 500 r/min, solution A is obtained.
2）It is pipetted in 4.45mL isopropyl titanates to solution A using liquid-transfering gun, adjustment rotating speed is 300r/min, stirs 3min
After obtain suspension B, suspension B is positioned over indoor aging 18h.
3）The titanium dioxide in suspension B, centrifugal rotational speed 7000r/min, after separation are detached by centrifugal separation
Solid matter be put into 60 DEG C of drying in oven after obtain titanium dioxide nano-sphere.
4）It takes the titanium dioxide nano-sphere of 100mg to be laid in the corundum boat of 75 × 13 × 9mm, corundum boat is placed in high temperature
In tube furnace, in high-purity ammonia of 99.99wt%（Flow is 200 standard milliliters/minute）In be heated to 700 DEG C, and keep the temperature 4h,
Titanium nitride nano ball is obtained after furnace cooling.
5）It weighs 1.4mg titanium nitride nano balls to be placed in round-bottomed flask, 100ml absolute ethyl alcohols, ultrasonic disperse 10min is added
Obtain suspension C.It weighs in the suspension C after ultrasonic disperse is added in 50mg cetyl trimethylammonium bromides, after stirring 15min
Obtain suspension D.The thioacetamide of the four chloride hydrate indiums and 4.8mmol that weigh 2.4mmol is separately added into suspension D,
Suspension E is obtained after stirring 30min.
6）Round-bottomed flask equipped with suspension E is put into constant temperature oil bath, suspension F is obtained after 95 DEG C of condensing reflux 2h,
Suspension F is centrifuged, obtained solid matter is put into 60 DEG C of baking oven after drying and obtains TiN-In2S3Nanometer flower ball-shaped
Nucleocapsid composite photo-catalyst.
Photochemical catalyzing H2-producing capacity test is carried out at room temperature：It is added into the lactic acid aqueous solution of 80ml 10wt%
20mg TiN-In2S3The catalyst of nano composite photo-catalyst moves into quartz glass reactor after ultrasonic 30min, uses 5 DEG C
Recirculated water keep temperature of reactor constant.It is online using gas-chromatography using the radiation of visible light quartz reactor more than 420nm
Analysis obtains light and urges the curve for decomposing water with amounts of hydrogen caused by light application time.
Embodiment 2：
1）The cetylamine for weighing 8.2mmol is added in 100mL absolute ethyl alcohols, and 1.6 ml deionized waters are added using liquid-transfering gun, with
After the rotating speed stirring 30min of 500 r/min, solution A is obtained.
2）It is pipetted in 4.45mL isopropyl titanates to solution A using liquid-transfering gun, adjustment rotating speed is 300r/min, stirs 3min
After obtain suspension B, suspension B is positioned over indoor aging 18h.
3）The titanium dioxide in suspension B, centrifugal rotational speed 7000r/min, after separation are detached by centrifugal separation
Solid matter be put into 60 DEG C of drying in oven after obtain titanium dioxide nano-sphere.
4）It takes the titanium dioxide nano-sphere of 100mg to be laid in the corundum boat of 75 × 13 × 9mm, corundum boat is placed in high temperature
In tube furnace, in 99.99% high-purity ammonia（Flow is 200 standard milliliters/minute）In be heated to 700 DEG C of range, and keep the temperature
4h obtains titanium nitride nano ball after furnace cooling.
5）4.2mg titanium nitride nano balls are weighed in round-bottomed flask, 100ml absolute ethyl alcohols are added, ultrasonic disperse 10min is obtained
To suspension C.It weighs in the suspension C after ultrasonic disperse is added in 50mg cetyl trimethylammonium bromides, is obtained after stirring 15min
To suspension D.The thioacetamide of the four chloride hydrate indiums and 4.8mmol that weigh 2.4mmol is separately added into suspension D, is stirred
Suspension E is obtained after mixing 30min.
6）Round-bottomed flask equipped with suspension E is put into constant temperature oil bath, suspension F is obtained after 95 DEG C of condensing reflux 2h,
Suspension F is centrifuged, obtained solid matter is put into 60 DEG C of baking oven after drying and obtains TiN-In2S3Nanometer flower ball-shaped
Nucleocapsid composite photo-catalyst.
Photochemical catalyzing H2-producing capacity test is carried out at room temperature：It is added into the lactic acid aqueous solution of 80ml 10wt%
20mg TiN-In2S3The catalyst of nano composite photo-catalyst moves into quartz glass reactor after ultrasonic 30min, uses 5 DEG C
Recirculated water keep temperature of reactor constant.It is online using gas-chromatography using the radiation of visible light quartz reactor more than 420nm
Analysis obtains light and urges the curve for decomposing water with amounts of hydrogen caused by light application time.
As shown in Figs. 1-5, Fig. 1：For X-ray diffractogram spectrogram, the curve 1 in Fig. 1 is the TiN- prepared in embodiment 2
In2S3The X-ray diffractogram spectrogram of nano composite photo-catalyst.Curve 2 is the TiN-In prepared in embodiment 12S3It is nano combined
The X-ray diffractogram spectrogram of photochemical catalyst.Curve 3 is the X-ray diffractogram spectrogram of blank indium sulfide.Curve 4 is received for titanium nitride
The X-ray diffractogram spectrogram of rice ball.
Curve 1 in Fig. 5 is blank indium sulfide visible light photolysis water hydrogen rate diagram in lactic acid aqueous solution.Curve 2 is
TiN-In described in embodiment 22S3Nano composite photo-catalyst visible light photolysis water hydrogen rate diagram in lactic acid aqueous solution.Curve 3
For TiN-In described in embodiment 12S3Nano composite photo-catalyst visible light photolysis water hydrogen rate diagram in lactic acid aqueous solution.
By Fig. 1-5 it is found that the composite photo-catalyst of this method preparation is different with the quality of the titanium nitride of addition, can make
For the different photochemical catalyst of pattern is gone out, there is morphology controllable and universality.While two hours of blank indium sulfide hydrogen output are only
Hydrogen output maximum for 11.73 micromoles per grams, the composite photo-catalyst of this method preparation can reach 21.17 micromoles per grams.
Activity, which improves, to be connect by about one time, it will be apparent that improves production hydrogen activity, has extensive research and application prospect.
The feature implementation example that the above is only the present invention, is not limited in any way the scope of the present invention.It is all to use together
The technical solution formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (6)
1. a kind of TiN-In2S3The preparation method of nano composite photo-catalyst, it is characterised in that：Include the following steps：By titanium nitride
Nanosphere is added in absolute ethyl alcohol, and cetyl trimethylammonium bromide is added after ultrasonic disperse, stirs, adds four chloride hydrates
Indium and thioacetamide stir evenly and obtain suspension after 95 DEG C of constant-temperature condensations flow back, and centrifuge the suspension, will detach
TiN-In is obtained after obtained solid matter drying2S3Nano composite photo-catalyst.
2. TiN-according to claim 12S3The preparation method of nano composite photo-catalyst, it is characterised in that：Specific packet
Include following steps：
1）1-10mg titanium nitride nano balls are weighed, 100-300ml absolute ethyl alcohols are added, ultrasonic disperse obtains suspension C；
2）It weighs 10-100mg cetyl trimethylammonium bromides to be added in the suspension C, suspension D is obtained after stirring；
3）The thioacetamide of the four chloride hydrate indiums and 3-8mmol that weigh 2-5mmol is separately added into the suspension D, is stirred
Suspension E is obtained after mixing；
4）The suspension E is obtained into suspension F after 95 DEG C of condensing reflux 2h, the suspension F is centrifuged, by what is obtained
Solid matter is put into 60 DEG C of baking oven and obtains TiN-In after drying2S3Nano composite photo-catalyst.
3. TiN-according to claim 1 or 22S3The preparation method of nano composite photo-catalyst, it is characterised in that：Institute
It states after titanium nitride nano ball heats cooling by titanium dioxide nano-sphere in ammonia atmosphere and obtains.
4. TiN-according to claim 32S3The preparation method of nano composite photo-catalyst, it is characterised in that：The nitrogen
Change titanium nanosphere preparation method be：50-300mg titanium dioxide nano-spheres are taken to be placed in corundum boat, by corundum boat in ammonia atmosphere
It is heated to 600-800 DEG C in enclosing, and keeps the temperature 3-5h, can be obtained titanium nitride nano ball after cooling.
5. TiN-according to claim 42S3The preparation method of nano composite photo-catalyst, it is characterised in that：Described two
The preparation method of TiOx nano ball is：
1）The cetylamine for weighing 5-10mmol is added in 50-200mL absolute ethyl alcohols, 1-3 ml deionized waters is added, with 400-
After the rotating speed stirring 20-60min of 700 r/min, solution A is obtained；
2）It takes 3-5mL isopropyl titanates to be added in solution A, suspension B is obtained after 100-300r/min rotating speeds stirring 1-10min,
And suspension B is positioned over indoor aging 12-24h；
3）The titanium dioxide in suspension B, centrifugal rotational speed 5000-8000r/min, after separation are detached by centrifugal separation
Solid matter be put into 50-80 DEG C of drying in oven after obtain titanium dioxide nano-sphere.
6. a kind of TiN-In described in claim 12S3The application of nano composite photo-catalyst, it is characterised in that：It is urged applied to light
Change hydrogen production by water decomposition.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810289924.6A CN108607589B (en) | 2018-04-03 | 2018-04-03 | TiN-In2S3Preparation method and application of nano composite photocatalyst |
Applications Claiming Priority (1)
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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 |
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