CN109261169A - Visible light-responded high-efficiency composite photocatalyst α-Fe2O3/In2S3Preparation method - Google Patents
Visible light-responded high-efficiency composite photocatalyst α-Fe2O3/In2S3Preparation method Download PDFInfo
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- 229910003145 α-Fe2O3 Inorganic materials 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 38
- 239000007787 solid Substances 0.000 claims abstract description 26
- 239000002105 nanoparticle Substances 0.000 claims abstract description 25
- 239000000725 suspension Substances 0.000 claims abstract description 25
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 17
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 150000002471 indium Chemical class 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 229910000859 α-Fe Inorganic materials 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- 239000012265 solid product Substances 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- 229910052738 indium Inorganic materials 0.000 claims description 9
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000006194 liquid suspension Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000006798 recombination Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 2
- 230000032900 absorption of visible light Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 32
- 238000013019 agitation Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000003483 aging Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- 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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of visible light-responded high-efficiency composite photocatalyst α-Fe2O3/In2S3Preparation method, this method comprises the following steps: 1) by α-Fe2O3Nano particle mixed with trivalent indium salts solution after by ultrasonic disperse, form uniform solid suspension；2) ageing reaction: sodium sulfide solution is added dropwise into the resulting solid suspension of step 1) and reacts completely, then transfers them to be put into baking oven in autoclave and is aged；3) drying grinding: being washed to neutrality for the resulting solid formation of step 2), then successively passes through drying and processing, milled processed.Preparation method of the present invention not only widens the absorption of visible light, but also can effectively inhibit charge recombination, has higher photocatalytic activity, is conducive to the degradation of organic matter.
Description
Technical field
The present invention relates to photocatalyst technology fields, and in particular to a kind of visible light-responded high-efficiency composite photocatalyst α-
Fe2O3/In2S3Preparation method.
Background technique
Bloodstone (α-Fe2O3) it is a kind of visible light-responded semiconductor, band gap 0.28-2.48eV urges agent with other light
It compares, α-Fe2O3Preparation condition it is mild, simple process, at the same have it is cheap, it is nontoxic, the advantages that natural rich reserves.
α-Fe2O3Be a kind of environment-friendly material, therefore also have many applications in environment remediation field, as photocatalytically degradating organic dye,
Organic acid, aldehydes organic matter etc..
However, due to bloodstone (α-Fe2O3) conduction band positions it is too low, be not enough to restore oxygen, so that photo-generated carrier
Recombination probability is very high, and separation is poor, keeps its photocatalytic activity lower.For these reasons, it is relatively simple how to find a kind of technique
It is single, reaction condition is milder, and can carry out different nanoparticles compound, prepare that appearance structure is controllable, photocatalytic activity is high
Composite photo-catalyst, have a very important significance.
Summary of the invention
It is an object of the invention to overcome the shortcomings of above-mentioned background technique, and provide a kind of visible light-responded high efficiency composition
Photochemical catalyst α-Fe2O3/In2S3Preparation method, this method preparation α-Fe2O3/In2S3Charge recombination rate is low again, photocatalysis
It is active high.
To achieve the above object, the present invention provides a kind of visible light-responded high-efficiency composite photocatalyst α-Fe2O3/In2S3
Preparation method, characterized by the following steps:
1) ultrasonic disperse: by α-Fe2O3Nano particle mixed with trivalent indium salts solution after by ultrasonic disperse, formed uniform
Solid suspension；
2) ageing reaction: sodium sulfide solution is added dropwise into the resulting solid suspension of step 1) and reacts completely, then by its turn
It moves in autoclave, then autoclave is put into baking oven and is aged；
3) drying grinding: being washed to neutrality for the resulting solid formation of step 2), then successively by drying and processing, at grinding
Reason.
In above-mentioned technical proposal, in the step 1), trivalent indium salts solution is selected from nitric acid solution of indium, sulfuric acid solution of indium；Institute
The molar concentration for stating trivalent indium salts solution is 0.0067~0.02mol/L；α-the Fe2O3Nano particle and trivalent indium salts solution
The molar ratio of middle solute is (9-19): (2-18).
In above-mentioned technical proposal, in the step 1), α-Fe2O3Nano particle is prepared by the following method:
101) first by Fe (NO3)3·9H2O is completely dissolved in water, then NaOH solution is added dropwise, adjusting pH value to 12~13,
Obtain suspension；
102) the resulting suspension of step 101) is stirred to being uniformly mixed, then carries out hydro-thermal reaction, is cooled to after reaction
Room temperature obtains solid product；
103) it takes the resulting solid product of step 102) to be washed till neutrality, using drying and processing, obtains solid product；
104) the resulting solid product of step 103) is put into progress high-temperature roasting processing in Muffle furnace, then be ground into
It is powdered.
In above-mentioned technical proposal, in the step 101), Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:3.7~7.5)
g/mL。
In above-mentioned technical proposal, in the step 102), the temperature of hydro-thermal reaction is 100~120 DEG C, the reaction time 6
~8h.
In above-mentioned technical proposal, in the step 103), the temperature of drying and processing is 60~80 DEG C, and the time is 5~8h.
In above-mentioned technical proposal, in the step 104), the temperature of high-temperature roasting processing is 400~450 DEG C, the time 2
~3h；After milled processed, resulting α-Fe2O3The partial size of nano particle is 100~1000nm.
In above-mentioned technical proposal, in the step 2), the molar concentration of sodium sulfide solution is 0.042~0.125mol/L；
The molar ratio of solute is 1:(1.5~2.5 in solute and sodium sulfide solution in the trivalent indium salts solution).
In above-mentioned technical proposal, in the step 2), the pH value of the solid suspension after reaction maintains 2~3, ageing
It is 24~26h that temperature, which is 160~180 DEG C of times,.
In above-mentioned technical proposal, in the step 3), drying and processing be specially be 60~80 DEG C in temperature at dry 5~
8h。
Compared with prior art, the present invention has the advantage that
First, α-Fe prepared by preparation method of the present invention2O3/In2S3For α-Fe2O3With In2S3Two kinds of semiconductors form heterogeneous
Structure, it is seen that when light radiation is to composite semiconductor surface, α-Fe2O3With In2S3Photo-generate electron-hole pairs can be generated, due to
In2S3Light induced electron potential ratio α-Fe on semiconductor conduction band2O3More negative, electrons move to α-Fe2O3Conduction band, and α-Fe2O3
The photohole potential ratio In of valence band2S3Corrigendum, hole can move to In2S3Valence band.In this way, the electronics of two kinds of semiconductors is empty
Cave is effectively migrated in heterostructure interface, is reduced charge recombination rate again, is improved photocatalytic activity.
Second, α-Fe prepared by preparation method of the present invention2O3/In2S3Compared to α-Fe2O3Or In2S3Monomer, not only to can
Light-exposed absorption is widened, and can effectively inhibit charge recombination, is had higher photocatalytic activity, is conducive to organic
The degradation of object, α-Fe2O3/In2S3Composite photo-catalyst in visible light illumination 100min, it is reachable to the degradation rate of rhodamine B
To 63.84%.
Third, preparation method of the invention is with other existing visible light response catalyst preparation methods, (a such as secret vanadium is compound
Oxide, calcium plug with molten metal the visible light catalytic materials such as oxide) it compares, it is safe and non-toxic, preparation process is mild, property is stable, raw material is easy
, it can be used for large-scale water body purification engineering, there is good practicability.
Detailed description of the invention
Fig. 1 is photocatalysis test process Contrast on effect schematic diagram of the invention；
Fig. 2 is the α-Fe of the embodiment of the present invention 12O3/In2S3The rhodamine B ultraviolet-visible of composite photo-catalyst scans light
Spectrogram.
Specific embodiment
Below with reference to the embodiment performance that the present invention will be described in detail, but they and do not constitute a limitation of the invention,
It is only for example.Simultaneously by illustrating that advantages of the present invention will become clearer and be readily appreciated that.
Embodiment 1:
Visible light-responded high-efficiency composite photocatalyst α-Fe of the invention2O3/In2S3Preparation method, including walk as follows
It is rapid: to weigh the α-Fe of 0.003mol hydro-thermal method preparation2O3The nitric acid that 10mL molar concentration is 0.0067mol/L is added dropwise in nano particle
Solution of indium (wherein, n (α-Fe2O3):n(In(NO3)3·5H2O)=9:2), ultrasonic 15min is uniformly dispersed, then under stiring slowly
Sodium sulfide solution (wherein, the n (In (NO that 20mL molar concentration is 0.083mol/L is added dropwise3)3·5H2O):n(Na2S)=1:
2.5) into above-mentioned suspension, the pH value of solid suspension maintains 3, then transfers them in autoclave and be put into baking oven
180 DEG C of ageings are for 24 hours.Resulting solid formation is washed to neutrality, and 5h is dried under conditions of 60 DEG C, and grinding is spare, obtains α-
Fe2O3/In2S3Composite photo-catalyst.
Wherein, α-Fe2O3The preparation method of nano particle includes the following steps: to take 16.16g Fe (NO3)3·9H2O, then
Deionized water, which is added, makes volume reach 60mL (Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:3.7) g/mL), in magnetic agitation
Stirring at normal temperature to solid is completely dissolved on device；Then 1molL is added dropwise-1NaOH solution, adjust pH value of solution to 13, obtain
The suspension of rufous, and add water constant volume to 85mL；Again magnetic agitation 30min to be uniformly mixed.Then, it is transferred to polytetrafluoroethyl-ne
In the stainless steel cauldron of alkene liner, after sealing, 100 DEG C of constant temperature 6h.Cooled to room temperature after reaction, after be washed with deionized water
It washs to pH about 7, dries 5h at 60 DEG C.Resulting solid product is put into 400 DEG C of roasting 2h of progress in Muffle furnace, takes out sample grinding
It is spare, α-Fe2O3The partial size of nano particle is 100~1000nm.
Embodiment 2:
Visible light-responded high-efficiency composite photocatalyst α-Fe of the invention2O3/In2S3Preparation method, including walk as follows
It is rapid: to weigh the α-Fe of 0.0032mol hydro-thermal method preparation2O3The nitric acid that 5mL molar concentration is 0.0067mol/L is added dropwise in nano particle
Solution of indium (wherein, n (α-Fe2O3):n(In(NO3)3·5H2O)=19:2), ultrasonic 15min is uniformly dispersed, then delays under stiring
It is slow that sodium sulfide solution (wherein, the n (In (NO that 20mL molar concentration is 0.042mol/L is added dropwise3)3·5H2O):n(Na2S)=1:
2.5) into above-mentioned suspension, the pH value of solid suspension maintains 3, then transfers them in autoclave and be put into baking oven
180 DEG C of ageings are for 24 hours.Resulting solid formation is washed to neutrality, and 5h is dried under conditions of 60 DEG C, and grinding is spare, obtains α-
Fe2O3/In2S3Composite photo-catalyst.
Wherein, α-Fe2O3The preparation method of nano particle includes the following steps: to take 16.16g Fe (NO3)3·9H2O, then
Deionized water, which is added, makes volume reach 60mL (Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:3.7) g/mL), in magnetic agitation
Stirring at normal temperature to solid is completely dissolved on device；Then 1molL is added dropwise-1NaOH solution, adjust pH value of solution to 13, obtain
The suspension of rufous, and add water constant volume to 85mL；Again magnetic agitation 30min to be uniformly mixed.Then, it is transferred to polytetrafluoroethyl-ne
In the stainless steel cauldron of alkene liner, after sealing, 100 DEG C of constant temperature 6h.Cooled to room temperature after reaction, after be washed with deionized water
It washs to pH about 7, dries 5h at 60 DEG C.Resulting solid product is put into 400 DEG C of roasting 2h of progress in Muffle furnace, takes out sample grinding
It is spare, α-Fe2O3The partial size of nano particle is 100~1000nm.
Embodiment 3:
Visible light-responded high-efficiency composite photocatalyst α-Fe of the invention2O3/In2S3Preparation method, including walk as follows
It is rapid: to weigh the α-Fe of 0.0028mol hydro-thermal method preparation2O3The nitre that 15mL molar concentration is 0.0067mol/L is added dropwise in nano particle
Sour solution of indium (wherein, n (α-Fe2O3):n(In(NO3)3·5H2O)=17:6), ultrasonic 15min is uniformly dispersed, then under stiring
Sodium sulfide solution (wherein, the n (In (NO that 20mL molar concentration is 0.125mol/L is slowly added dropwise3)3·5H2O):n(Na2S)=
1:2.5) into above-mentioned suspension, the pH value of solid suspension maintains 3, then transfers them to and be put into baking oven in autoclave
Interior 180 DEG C of ageings are for 24 hours.Resulting solid formation is washed to neutrality, and 5h is dried under conditions of 60 DEG C, and grinding is spare, obtains α-
Fe2O3/In2S3Composite photo-catalyst.
Wherein, α-Fe2O3The preparation method of nano particle includes the following steps: to take 16.16g Fe (NO3)3·9H2O, then
Deionized water, which is added, makes volume reach 60mL (Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:3.7) g/mL), in magnetic agitation
Stirring at normal temperature to solid is completely dissolved on device；Then 1molL is added dropwise-1NaOH solution, adjust pH value of solution to 13, obtain
The suspension of rufous, and add water constant volume to 85mL；Again magnetic agitation 30min to be uniformly mixed.Then, it is transferred to polytetrafluoroethyl-ne
In the stainless steel cauldron of alkene liner, after sealing, 100 DEG C of constant temperature 6h.Cooled to room temperature after reaction, after be washed with deionized water
It washs to pH about 7, dries 5h at 60 DEG C.Resulting solid product is put into 400 DEG C of roasting 2h of progress in Muffle furnace, takes out sample grinding
It is spare, α-Fe2O3The partial size of nano particle is 100~1000nm.
Embodiment 4:
Visible light-responded high-efficiency composite photocatalyst α-Fe of the invention2O3/In2S3Preparation method, including walk as follows
It is rapid: to weigh the α-Fe of 0.0028mol hydro-thermal method preparation2O3The sulfuric acid that 15mL molar concentration is 0.02mol/L is added dropwise in nano particle
Solution of indium (wherein, n (α-Fe2O3):n(In2(SO4)3)=17:18), ultrasonic 15min is uniformly dispersed, then slowly drips under stiring
Adding 20mL molar concentration is sodium sulfide solution (wherein, the n (In of 0.125mol/L2(SO4)3):n(Na2S)=1:1.5) it is extremely above-mentioned
In suspension, the pH value of solid suspension maintains 2, then transfers them in autoclave and be put into 160 DEG C of ageings in baking oven
26h.Resulting solid formation is washed to neutrality, and 8h is dried under conditions of 80 DEG C, and grinding is spare, obtains α-Fe2O3/In2S3It is multiple
Light combination catalyst.
Wherein, α-Fe2O3The preparation method of nano particle includes the following steps: to take 16.16g Fe (NO3)3·9H2O, then
Deionized water, which is added, makes volume reach 121.2mL (Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:7.5) g/mL), in magnetic force
Stirring at normal temperature to solid is completely dissolved on blender；Then 1molL is added dropwise-1NaOH solution, adjust pH value of solution to 12,
The suspension of rufous is obtained, and adds water constant volume to 85mL；Again magnetic agitation 30min to be uniformly mixed.Then, poly- four are transferred to
In the stainless steel cauldron of vinyl fluoride liner, after sealing, 120 DEG C of constant temperature 8h.Cooled to room temperature after reaction, after use deionization
Water washing dries 8h at 80 DEG C to pH about 7.Resulting solid product is put into 450 DEG C of roasting 3h of progress in Muffle furnace, takes out sample
Grind spare, α-Fe2O3The partial size of nano particle is 100~1000nm.
Embodiment 5:
Visible light-responded high-efficiency composite photocatalyst α-Fe of the invention2O3/In2S3Preparation method, including walk as follows
It is rapid: to weigh the α-Fe of 0.003mol hydro-thermal method preparation2O3The sulfuric acid that 15mL molar concentration is 0.0067mol/L is added dropwise in nano particle
Solution of indium (wherein, n (α-Fe2O3):n(In2(SO4)3)=9:2), ultrasonic 15min is uniformly dispersed, then is slowly added dropwise under stiring
20mL molar concentration is sodium sulfide solution (wherein, the n (In of 0.125mol/L2(SO4)3)n(Na2S)=1:2.5) it is hanged to above-mentioned
In supernatant liquid, the pH value of solid suspension maintains 2, then transfers them in autoclave and be put into 160 DEG C of ageings in baking oven
26h.Resulting solid formation is washed to neutrality, and 8h is dried under conditions of 80 DEG C, and grinding is spare, obtains α-Fe2O3/In2S3It is multiple
Light combination catalyst.
Wherein, α-Fe2O3The preparation method of nano particle includes the following steps: to take 16.16g Fe (NO3)3·9H2O, then
Deionized water, which is added, makes volume reach 121.2mL (Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:7.5) g/mL), in magnetic force
Stirring at normal temperature to solid is completely dissolved on blender；Then 1molL is added dropwise-1NaOH solution, adjust pH value of solution to 12,
The suspension of rufous is obtained, and adds water constant volume to 85mL；Again magnetic agitation 30min to be uniformly mixed.Then, poly- four are transferred to
In the stainless steel cauldron of vinyl fluoride liner, after sealing, 120 DEG C of constant temperature 8h.Cooled to room temperature after reaction, after use deionization
Water washing dries 8h at 80 DEG C to pH about 7.Resulting solid product is put into 450 DEG C of roasting 3h of progress in Muffle furnace, takes out sample
Grind spare, α-Fe2O3The partial size of nano particle is 100~1000nm.
Effect example: photocatalytic degradation test
Visible light-responded high-efficiency composite photocatalyst α-Fe prepared by above-described embodiment 1~32O3/In2S3For sieve
The photocatalytic degradation test of red bright B, it is seen that the high-efficiency composite photocatalyst α-Fe of photoresponse2O3/In2S3Photocatalytic activity examination
It tests using rhodamine B aqueous solution as target stains water source, it is living with the photocatalysis of evaluating combined material by the degradation rate of rhodamine
Property.Rhodamine B concentration is 6mgL-1, volume 50ml is placed in the double glazing reactor with ice-water bath, magnetic agitation.It adopts
Light source, illuminance 976500lux, α-Fe are provided with xenon lamp2O3/In2S3Photochemical catalyst 0.05g first inhales in the dark before testing
It is attached, start to sample after reaching adsorption equilibrium, be taken once after illumination every 0min, 30min, 60min, 100min.The sample of acquisition
It is detected using Shimadzu UV2600 ultraviolet-visible spectrophotometer, Detection wavelength 553nm.
Fig. 1 show the photocatalysis test process Contrast on effect schematic diagram of 1-3 of the embodiment of the present invention；Fig. 2 show this hair
α-the Fe of bright embodiment 12O3/In2S3The rhodamine B ultraviolet-visible scanning optical spectrum figure of composite photo-catalyst.As shown in Figure 1, real
Apply the α-Fe of the preparation of example 12O3/In2S3The degradation effect of composite photo-catalyst is best, -60min, 0min, 30min, 60min,
The degradation rate of 100min is respectively 0,23.51%, 33.51%, 47.03%, 61.62%.The composite sample and list of other ratios
The degradation rate of one catalyst is below optimal sample.As shown in Figure 2, rhodamine B is with α-Fe2O3/In2S3The drop of composite catalyst
There is no the movement for generating maximum absorption band, i.e., no sensitization phenomenons for solution.
α-Fe prepared by the present invention2O3/In2S3Visible light-responded composite technology is simple, and reaction condition is mild, leads to
Photocatalysis test is crossed, composite material photocatalyst has visible light photocatalysis active, can efficient degradation dyestuff and organic pollutant.
The content that this specification is not described in detail belongs to the prior art well known to professional and technical personnel in the field.
Claims (10)
1. a kind of visible light-responded high-efficiency composite photocatalyst α-Fe2O3/In2S3Preparation method, it is characterised in that: including such as
Lower step:
1) ultrasonic disperse: by α-Fe2O3Nano particle mixed with trivalent indium salts solution after by ultrasonic disperse, formed uniform solid
Liquid suspension；
2) ageing reaction: sodium sulfide solution is added dropwise into the resulting solid suspension of step 1) and reacts completely, then transfers them to
In autoclave, then autoclave is put into baking oven and is aged；
3) drying grinding: being washed to neutrality for the resulting solid formation of step 2), then successively passes through drying and processing, milled processed, i.e.,
It can.
2. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 12O3/In2S3Preparation method,
Be characterized in that: in the step 1), trivalent indium salts solution is selected from nitric acid solution of indium, sulfuric acid solution of indium；The trivalent indium salts solution
Molar concentration be 0.0067~0.02mol/L；α-the Fe2O3The molar ratio of solute in nano particle and trivalent indium salts solution
For (9-19): (2-18).
3. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 22O3/In2S3Preparation method,
It is characterized in that: in the step 1), α-Fe2O3Nano particle is prepared by the following method:
101) first by Fe (NO3)3·9H2O is completely dissolved in water, then NaOH solution is added dropwise, and is adjusted pH value to 12~13, is obtained
Suspension；
102) the resulting suspension of step 101) is stirred to being uniformly mixed, then carries out hydro-thermal reaction, is cooled to room temperature after reaction,
Obtain solid product；
103) it takes the resulting solid product of step 102) to be washed till neutrality, using drying and processing, obtains solid product；
104) the resulting solid product of step 103) is put into progress high-temperature roasting processing in Muffle furnace, then is ground into powder
Shape.
4. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 32O3/In2S3Preparation method,
It is characterized in that: in the step 101), Fe (NO3)3·9H2The solid-to-liquid ratio of O and water is (1:3.7~7.5) g/mL.
5. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 42O3/In2S3Preparation method,
Be characterized in that: in the step 102), the temperature of hydro-thermal reaction is 100~120 DEG C, and the reaction time is 6~8h.
6. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 52O3/In2S3Preparation method,
Be characterized in that: in the step 103), the temperature of drying and processing is 60~80 DEG C, and the time is 5~8h.
7. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 62O3/In2S3Preparation method,
Be characterized in that: in the step 104), the temperature of high-temperature roasting processing is 400~450 DEG C, and the time is 2~3h；Milled processed
Afterwards, resulting α-Fe2O3The partial size of nano particle is 100~1000nm.
8. described in any item visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 1~72O3/In2S3System
Preparation Method, it is characterised in that: in the step 2), the molar concentration of sodium sulfide solution is 0.042~0.125mol/L；Described three
The molar ratio of solute is 1:(1.5~2.5 in solute and sodium sulfide solution in valence indium salts solution).
9. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 82O3/In2S3Preparation method,
Be characterized in that: in the step 2), the pH value of the solid suspension after reaction maintains 2~3, and the temperature of ageing is 160~180
DEG C time is 24~26h.
10. visible light-responded high-efficiency composite photocatalyst α-Fe according to claim 92O3/In2S3Preparation method,
It is characterized by: in the step 3), dry 5~8h at drying and processing is specially 60~80 DEG C in temperature.
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