CN110368975A - A kind of construction method of compound semiconductor photocatalytic material - Google Patents
A kind of construction method of compound semiconductor photocatalytic material Download PDFInfo
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- CN110368975A CN110368975A CN201910586990.4A CN201910586990A CN110368975A CN 110368975 A CN110368975 A CN 110368975A CN 201910586990 A CN201910586990 A CN 201910586990A CN 110368975 A CN110368975 A CN 110368975A
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- 239000004065 semiconductor Substances 0.000 title claims abstract description 25
- 150000001875 compounds Chemical class 0.000 title claims abstract description 19
- 238000010276 construction Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- YYKKIWDAYRDHBY-UHFFFAOYSA-N [In]=S.[Zn] Chemical compound [In]=S.[Zn] YYKKIWDAYRDHBY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 238000006555 catalytic reaction Methods 0.000 claims description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 16
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 14
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 claims description 9
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 8
- 239000011592 zinc chloride Substances 0.000 claims description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011941 photocatalyst Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- JKXCZYCVHPKTPK-UHFFFAOYSA-N hydrate;trihydrochloride Chemical compound O.Cl.Cl.Cl JKXCZYCVHPKTPK-UHFFFAOYSA-N 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- NJWNEWQMQCGRDO-UHFFFAOYSA-N indium zinc Chemical compound [Zn].[In] NJWNEWQMQCGRDO-UHFFFAOYSA-N 0.000 claims 1
- 238000004073 vulcanization Methods 0.000 claims 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 16
- 239000008367 deionised water Substances 0.000 abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 abstract description 8
- 235000019441 ethanol Nutrition 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000003321 amplification Effects 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 238000012805 post-processing Methods 0.000 abstract description 2
- 239000013077 target material Substances 0.000 abstract 2
- 239000012429 reaction media Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 30
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- KYCHGXYBBUEKJK-UHFFFAOYSA-K indium(3+);trichloride;hydrate Chemical compound O.Cl[In](Cl)Cl KYCHGXYBBUEKJK-UHFFFAOYSA-K 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- 229910021392 nanocarbon Inorganic materials 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100001234 toxic pollutant Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J35/33—Electric or magnetic properties
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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
-
- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of construction methods of compound semiconductor photocatalytic material.Mesh of the present invention is the γ-Fe by being prepared in situ2O3/ indium sulfide zinc composite material and g-C3N4It is prepared with being stirred under normal temperature and pressure.Advantage of the present invention are as follows: (1) compound semiconductor photocatalytic material has magnetism, is all easily recycled in entire reaction process, simplifies the operational sequence of post-processing；(2) reaction condition of target material building is simple, and low for equipment requirements, preparation method is simple；(3) target material catalytic effect is excellent；(4) reaction is using deionized water, glycerol, ethyl alcohol as reaction medium, environmental-friendly and easy industry amplification.
Description
One technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of construction method of compound semiconductor photocatalytic material.
Two background techniques
Currently, influenced by China's industry fast development and combustion of fossil fuel, bring toxic industrial waste water and
The problem of new energy is supplied is badly in need of solving, and on this basis, toxic pollutant is changed into low toxicity or even nontoxic is discharged
Substance and using a kind of Novel pollution-free the energy replace fossil fuel become primary goal.By continuous research and probe,
Researcher is prepared for a kind of NEW TYPE OF COMPOSITE catalysis material (ZnIn2S4-g-C3N4) for handling organic contamination under visible light
Object and produce at this Novel pollution-free of hydrogen the energy (Liu H, Jin Z, Xu Z, et al.Fabrication of
ZnIn2S4-g-C3N4sheet-on-sheet nanocomposites for efficient visible-light
photocatalytic H2-evolution and degradation of organic pollutants[J].RSC
Advances, 2015,5.).
The composite photocatalyst material significantly can be used to handle organic pollutant and evolving hydrogen reaction, and subsequent also there are many scientific researches
Worker prepares such catalysis material by distinct methods, as microwave synthesizes (Ding N, Zhang L, Zhang H, et
al.Microwave-assisted synthesis of ZnIn2S4/g-C3N4, heterojunction
photocatalysts for efficient visible light photocatalytic hydrogen evolution
[J] .Catalysis Communications, 2017,100:173-177.), hydrothermal synthesis (Shi F, Chen L, Chen M,
et al.A g-C3N4/nanocarbon/ZnIn2S4Nanocomposite:an artificial Z-scheme visible-
light photocatalytic system using nanocarbon as the electron mediator[J]
.Chemical Communications, 2015,51.), physical mixed (Hongcen Y, Ruya C, Pengxiao S, et
al.Constructing electrostatic self-assembled 2D/2D ultra-thin ZnIn2S4/
protonated g-C3N4heterojunctions for excellent photocatalytic performance
Under visible light [J] .Applied Catalysis B:Environmental, 2019:117862.).
However, such catalysis material on the basis of efficient, all has the shortcomings that difficult separation and recovery, therefore, preparation one
Kind effectively segregative compound semiconductor photocatalytic material becomes particularly important.Present invention adds a kind of existing catalytic effects
Magnetic substance (γ-Fe2O3), photocatalysis performance can not only be improved on the original basis, moreover it is possible to divide catalysis material easily
It separates out and, greatly improve the access times of composite photocatalyst material, reduce cost.
Three summary of the invention
It is an object of the invention to propose a kind of preparation method of efficiently segregative compound semiconductor photocatalytic material.
The technical solution for realizing the object of the invention is the γ-Fe by being prepared in situ2O3/ indium sulfide zinc composite material with
g-C3N4It is prepared with being stirred under normal temperature and pressure, the specific steps are as follows::
Step 1) is by a certain amount of Iron trichloride hexahydrate (FeCl3·6H2O it) is dissolved in ethylene glycol and stirs certain time；
A certain amount of sodium hydroxide is added to the water to obtain its aqueous solution by step 2), is added drop-wise in step 1), continues to stir
It mixes spare after a certain period of time；
Mixed liquor obtained by step 2) is transferred in hydrothermal reaction kettle by step 3), and certain time is reacted under certain temperature, is centrifuged
Washing, dry certain time, is made γ-Fe under certain temperature2O3；
Step 4) takes γ-Fe made from different quality containing step 3)2O3With a certain amount of zinc chloride, four trichloride hydrates
In hydrothermal reaction kettle, reaction in-situ obtains γ-Fe for indium and thioacetamide2O3/ indium sulfide zinc composite material；
Step 5) is by the g-C of preparation3N4With the γ-Fe of step 4)2O3/ indium sulfide zinc composite material is stirred by normal temperature and pressure
It mixes to obtain composite semiconductor light-catalyst.
In step 1) of the invention, Iron trichloride hexahydrate quality is 0.2-0.3g, and ethylene glycol volume is 10ml, and mixing time is
30min。
In step 2) of the invention, sodium hydrate aqueous solution 5mol/L, mixing time 30min.
In step 2) of the invention, ethylene glycol: water 1: 1-2: 1.
In step 3) of the invention, the reaction temperature in reaction kettle is 150-180 DEG C, reaction time 8-14h, dry temperature
Degree is 180-200 DEG C, time 10-12h.
In step 4) of the invention, γ-Fe2O3Mass fraction be 5-20wt%, reaction temperature is in hydrothermal reaction kettle
180 DEG C, reaction time 12h.
In step 5) of the invention, by physical agitation by the g-C of instillation3N4Aqueous solution and catalysis material aqueous solution are multiple
It closes, wherein the two aqueous solution mass ratio is 0.2: 1-1: 1.
Compared with prior art, the present invention advantage are as follows: (1) compound semiconductor photocatalytic material has magnetism, entire anti-
It should all be easily recycled in the process, simplify the operational sequence of post-processing；(2) compound semiconductor photocatalytic material constructs
Reaction condition is simple, low for equipment requirements, and preparation method is simple；(3) the more existing public affairs of compound semiconductor photocatalytic material prepared
The catalytic effect for opening other catalysis materials of report is obviously improved；(4) reaction is using deionized water, glycerol, ethyl alcohol as anti-
Medium is answered, process safety is steady, and the flames of anger, smog generate, three-waste free discharge, environmental-friendly and easy industry amplification.
Four specific embodiments
The present invention will be further described for the following examples, and the purpose is to can be best understood from the contents of the present invention.But
It is that embodiment does not limit the scope of the invention in any way.The technical staff of this professional domain is in scope of the invention as claimed
The modifications and adaptations inside made also should belong to right and protection scope of the invention.
Embodiment 1
It weighs 0.25g ferric chloride hexahydrate to be dissolved in 10mL ethylene glycol solution, stirs 30min.By configured 5mol/
The sodium hydrate aqueous solution of L is slowly dropped in above-mentioned solution, and the ratio of ethylene glycol and water is 2: 1, stirs 30min.After will mix
It closes solution to be transferred in hydrothermal reaction kettle, reacts 12h at 160 DEG C.After cooling, washing centrifugation in 200 DEG C of dry 12h, is obtained
γ-Fe2O3.Based on 1mmol indium sulfide zinc, the γ-Fe of different quality is weighed2O3, it is added to 0.2g zinc chloride, 0.6g tetra-
It in trichloride hydrate indium and 0.3g thioacetamide, and is dissolved in 5mL glycerol and 15mL ethyl alcohol, ultrasonic 30min mixes gained
It closes solution to be transferred in hydrothermal reaction kettle, 12h is reacted at 180 DEG C, prepare 5wt%, 10wt%, 15wt%, the light of 20wt%
Catalysis material.And by g-C obtained3N4Aqueous solution (0.5mg/mL) is 1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1 in mass ratio
It is slowly dropped in catalysis material solution (100mg, 200mL deionized water), centrifuge washing obtains composite semiconductor photocatalysis
Material.
Embodiment 2
It weighs 0.25g ferric chloride hexahydrate to be dissolved in 10mL ethylene glycol solution, stirs 30min.By configured 5mol/
The sodium hydrate aqueous solution of L is slowly dropped in above-mentioned solution, and the ratio of ethylene glycol and water is 2: 1, stirs 30min.After will mix
It closes solution to be transferred in hydrothermal reaction kettle, reacts 14h at 150 DEG C.After cooling, washing centrifugation in 200 DEG C of dry 12h, is obtained
γ-Fe2O3.Based on 1mmol indium sulfide zinc, the γ-Fe of different quality is weighed2O3, it is added to 0.2g zinc chloride, 0.6g tetra-
It in trichloride hydrate indium and 0.3g thioacetamide, and is dissolved in 5mL glycerol and 15mL ethyl alcohol, ultrasonic 30min mixes gained
It closes solution to be transferred in hydrothermal reaction kettle, 12h is reacted at 180 DEG C, prepare 5wt%, 10wt%, 15wt%, the light of 20wt%
Catalysis material.And by g-C obtained3N4Aqueous solution (0.5mg/mL) is 1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1 in mass ratio
It is slowly dropped in catalysis material solution (100mg, 200mL deionized water), centrifuge washing obtains composite semiconductor photocatalysis
Material.
Embodiment 3
It weighs 0.25g ferric chloride hexahydrate to be dissolved in 10mL ethylene glycol solution, stirs 30min.By configured 5mol/
The sodium hydrate aqueous solution of L is slowly dropped in above-mentioned solution, and the ratio of ethylene glycol and water is 2: 1, stirs 30min.After will mix
It closes solution to be transferred in hydrothermal reaction kettle, reacts 10h at 170 DEG C.After cooling, washing centrifugation in 200 DEG C of dry 12h, is obtained
γ-Fe2O3.Based on 1mmol indium sulfide zinc, the γ-Fe of different quality is weighed2O3, it is added to 0.2g zinc chloride, 0.6g tetra-
It in trichloride hydrate indium and 0.3g thioacetamide, and is dissolved in 5mL glycerol and 15mL ethyl alcohol, ultrasonic 30min mixes gained
It closes solution to be transferred in hydrothermal reaction kettle, 12h is reacted at 180 DEG C, prepare 5wt%, 10wt%, 15wt%, the light of 20wt%
Catalysis material.And by g-C obtained3N4Aqueous solution (0.5mg/mL) is 1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1 in mass ratio
It is slowly dropped in catalysis material solution (100mg, 200mL deionized water), centrifuge washing obtains composite semiconductor photocatalysis
Material.
Embodiment 4
It weighs 0.25g ferric chloride hexahydrate to be dissolved in 10mL ethylene glycol solution, stirs 30min.By configured 5mol/
The sodium hydrate aqueous solution of L is slowly dropped in above-mentioned solution, and the ratio of ethylene glycol and water is 2: 1, stirs 30min.After will mix
It closes solution to be transferred in hydrothermal reaction kettle, reacts 8h at 180 DEG C.After cooling, washing centrifugation in 200 DEG C of dry 12h, obtains γ-
Fe2O3.Based on 1mmol indium sulfide zinc, the γ-Fe of different quality is weighed2O3, it is added to 0.2g zinc chloride, 0.6g tetra- is hydrated
It in indium trichloride and 0.3g thioacetamide, and is dissolved in 5mL glycerol and 15mL ethyl alcohol, ultrasonic 30min mixes gained molten
Liquid is transferred in hydrothermal reaction kettle, and 12h is reacted at 180 DEG C, prepares 5wt%, 10wt%, 15wt%, the photocatalysis of 20wt%
Material.And by g-C obtained3N4Aqueous solution (0.5mg/mL) is slow for 1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1 in mass ratio
It is added drop-wise in catalysis material solution (100mg, 200mL deionized water), centrifuge washing obtains compound semiconductor photocatalytic material.
Embodiment 5
It weighs 0.25g ferric chloride hexahydrate to be dissolved in 10mL ethylene glycol solution, stirs 30min.By configured 5mol/
The sodium hydrate aqueous solution of L is slowly dropped in above-mentioned solution, and the ratio of ethylene glycol and water is 2: 1, stirs 30min.After will mix
It closes solution to be transferred in hydrothermal reaction kettle, reacts 12h at 160 DEG C.After cooling, washing centrifugation in 180 DEG C of dry 10h, is obtained
γ-Fe2O3.Based on 1mmol indium sulfide zinc, the γ-Fe of different quality is weighed2O3, it is added to 0.2g zinc chloride, 0.6g tetra-
It in trichloride hydrate indium and 0.3g thioacetamide, and is dissolved in 5mL glycerol and 15mL ethyl alcohol, ultrasonic 30min mixes gained
It closes solution to be transferred in hydrothermal reaction kettle, 12h is reacted at 180 DEG C, prepare 5wt%, 10wt%, 15wt%, the light of 20wt%
Catalysis material.And by g-C obtained3N4Aqueous solution (0.5mg/mL) is 1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1 in mass ratio
It is slowly dropped in catalysis material solution (100mg, 200mL deionized water), centrifuge washing obtains composite semiconductor photocatalysis
Material.
Embodiment 6
It weighs 0.25g ferric chloride hexahydrate to be dissolved in 10mL ethylene glycol solution, stirs 30min.By configured 5mol/
The sodium hydrate aqueous solution of L is slowly dropped in above-mentioned solution, and the ratio of ethylene glycol and water is 1: 1, stirs 30min.After will mix
It closes solution to be transferred in hydrothermal reaction kettle, reacts 12h at 160 DEG C.After cooling, washing centrifugation in 200 DEG C of dry 12h, is obtained
γ-Fe2O3.Based on 1mmol indium sulfide zinc, the γ-Fe of different quality is weighed2O3, it is added to 0.2g zinc chloride, 0.6g tetra-
It in trichloride hydrate indium and 0.3g thioacetamide, and is dissolved in 5mL glycerol and 15mL ethyl alcohol, ultrasonic 30min mixes gained
It closes solution to be transferred in hydrothermal reaction kettle, 12h is reacted at 180 DEG C, prepare 5wt%, 10wt%, 15wt%, the light of 20wt%
Catalysis material.And by g-C obtained3N4Aqueous solution (0.5mg/mL) is 1: 0.2,1: 0.4,1: 0.6,1: 0.8,1: 1 in mass ratio
It is slowly dropped in catalysis material solution (100mg, 200mL deionized water), centrifuge washing obtains composite semiconductor photocatalysis
Material.
Claims (7)
1. a kind of construction method of compound semiconductor photocatalytic material, which is characterized in that by the γ-Fe being prepared in situ2O3And vulcanization
Indium zinc composite material and g-C3N4It is prepared with being stirred under normal temperature and pressure, the specific steps are as follows:
Step 1) is by a certain amount of Iron trichloride hexahydrate (FeCl3·6H2O it) is dissolved in ethylene glycol and stirs certain time；
A certain amount of sodium hydroxide is added to the water to obtain its aqueous solution by step 2), is added drop-wise in step 1), continues stirring one
It is spare after fixing time；
Mixed liquor obtained by step 2) is transferred in hydrothermal reaction kettle by step 3), reacts certain time under certain temperature, centrifuge washing,
Dry certain time, is made γ-Fe under certain temperature2O3；
Step 4) takes γ-Fe made from different quality containing step 3)2O3With a certain amount of zinc chloride, four trichloride hydrate indiums and
For thioacetamide in hydrothermal reaction kettle, reaction in-situ obtains γ-Fe2O3/ indium sulfide zinc composite material；
Step 5) is by the g-C of preparation3N4Composite semiconductor light is stirred to get by normal temperature and pressure with the composite photo-catalyst of step 4)
Catalyst.
2. a kind of construction method of compound semiconductor photocatalytic material according to claim 1, it is characterised in that: step 1)
In, Iron trichloride hexahydrate quality is 0.2-0.3g, and ethylene glycol volume is 10ml, mixing time 30min.
3. a kind of construction method of compound semiconductor photocatalytic material according to claim 1, it is characterised in that: step 2)
In, sodium hydrate aqueous solution 5mol/L, mixing time 30min.
4. a kind of construction method of compound semiconductor photocatalytic material according to claim 1, it is characterised in that: step 2)
In, ethylene glycol: water 1: 1-2: 1.
5. a kind of construction method of compound semiconductor photocatalytic material according to claim 1, it is characterised in that: step 3)
In, reaction temperature in reaction kettle is 150-180 DEG C, reaction time 8-14h, and drying temperature is 180-200 DEG C, and the time is
10-12h。
6. a kind of construction method of compound semiconductor photocatalytic material according to claim 1, it is characterised in that: step 4)
In, γ-Fe2O3Mass fraction be 5-20wt%, reaction temperature is 180 DEG C in hydrothermal reaction kettle, reaction time 12h.
7. a kind of construction method of compound semiconductor photocatalytic material according to claim 1, it is characterised in that: step 5)
In, by physical agitation by the g-C of instillation3N4Aqueous solution and catalysis material aqueous solution are compound, wherein the two aqueous solution quality
Than being 0.2: 1-1: 1.
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| CN201910586990.4A CN110368975A (en) | 2019-06-22 | 2019-06-22 | A kind of construction method of compound semiconductor photocatalytic material |
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Application publication date: 20191025 |