CN110368922A - A kind of construction method of indium sesquioxide optic catalytic composite material - Google Patents
A kind of construction method of indium sesquioxide optic catalytic composite material Download PDFInfo
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- CN110368922A CN110368922A CN201910571208.1A CN201910571208A CN110368922A CN 110368922 A CN110368922 A CN 110368922A CN 201910571208 A CN201910571208 A CN 201910571208A CN 110368922 A CN110368922 A CN 110368922A
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- indium sesquioxide
- composite material
- indium
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- catalytic composite
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 19
- 238000010276 construction Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 25
- 239000002243 precursor Substances 0.000 claims description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000013077 target material Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000003321 amplification Effects 0.000 abstract description 2
- 230000002153 concerted effect Effects 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 abstract description 2
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 239000012429 reaction media Substances 0.000 abstract description 2
- 230000005764 inhibitory process Effects 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 description 16
- 238000001816 cooling Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 14
- 238000005406 washing Methods 0.000 description 8
- 229910052738 indium Inorganic materials 0.000 description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 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 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 238000005286 illumination Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 235000014214 soft drink Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/08—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of gallium, indium or thallium
-
- 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
-
- 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
-
- 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
-
- B01J35/39—
-
- 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
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of construction methods of indium sesquioxide optic catalytic composite material.Object of the present invention is to by being doped with nonmetalloid carbon quantum dot and indium sesquioxide composite material be stirred and be prepared under normal temperature and pressure.Advantage of the present invention are as follows: (1) composite photocatalyst material has hexagon tubulose microscopic appearance, specific surface area with higher and more active site；(2) gained indium sesquioxide nanocomposite sufficiently combines the excellent photo-catalysis capability of nanometer indium sesquioxide and the compound action of carbon quantum dot inhibition photo-generate electron-hole, concerted catalysis excellent effect；(3) reaction condition of target material building is simple, and low for equipment requirements, preparation method is simple；(4) target material catalytic effect is excellent；(5) reaction is using deionized water, 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 building side of indium sesquioxide optic catalytic composite material
Method.
Two background techniques
Industrial wastewater containing rhodamine B has harmfulness to human body and animal, and waste water treatment process is led as water process
Research hotspot (Mustafa S, Yunus E U, the Erkan Y et al Determination of rhodamine B in domain
In soft drink, waste water and lipstick samples after solid phase extraction.
[J] .Food and Chemical Toxicology, 2011,49:1796-1799) due to its significant visible absorption and height
Energy conversion efficiency, conductor oxidate based photocatalyst have attracted a large amount of concern (Xiang X, Xie L, Li Z, et
al.Ternary MgO/ZnO/In2O3heterostructured photocatalysts derived from a layered
precursor and visible-light-induced photocatalytic activity[J].Chemical
Engineering Journal, 2013,221:222-229.).Such composite photocatalyst material significantly can be used to handle organic
Pollutant and evolving hydrogen reaction, in environment, the energy, chemical industry, the numerous areas such as biology are had a wide range of applications and outstanding prospect.
However, such catalysis material in respective advantage, all has energy band wider, photo-generate electron-hole pairs are easily compound
The shortcomings that.Therefore, preparing the conductor photocatalysis composite material that one kind effectively inhibits photo-generate electron-hole compound becomes especially to weigh
It wants.Present invention adds a kind of substance (carbon quantum dot for being doped with nonmetalloid) with good electrochemical catalysis performance,
Photocatalysis performance can be greatly improved on the original basis.
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 carbon quantum dot and three oxidations two by being doped with nonmetalloid
Indium composite material is stirred under normal temperature and pressure and is prepared, the specific steps are as follows:
Step 1) is by a certain amount of indium nitrate (In (NO3)3) and spherical urea be dissolved in deionized water and stir one periodically
Between；
Gained mixed liquor in step 1) is transferred in hydrothermal reaction kettle by step 2), reacts certain time under certain temperature, from
Heart washing, dry certain time, is made indium sesquioxide precursor under certain temperature；
Indium sesquioxide precursor obtained by step 2) is put into tube furnace by step 3), calcines certain time under certain temperature,
Indium sesquioxide is made；
A certain amount of citric acid is dissolved in by step 4) respectively at a certain amount of urea, thioacetamide, phosphoric acid and ammonium hydroxide
In ionized water, and stir certain time；
Gained mixed liquor in step 4) is transferred in hydrothermal reaction kettle by step 5), and certain time is reacted under certain temperature, is made
The carbon quantum dot solution of nonmetalloid must be doped with；
Step 6) stirs gained carbon quantum solution in step 5) and the composite photo-catalyst of step 3) by normal temperature and pressure
Composite semiconductor light-catalyst is obtained, every milliliter of carbon quantum solution needs to be added indium sesquioxide 1-2mg.
In step 1) of the invention, indium nitrate quality is 1.6-2.0g, and spherical urea quality is 1.5-1.6g, deionized water
Volume is 40ml, mixing time 30min.
In step 2) of the invention, the reaction temperature in reaction kettle is 120-160 DEG C, reaction time 12-16h, dry
Temperature is 60 DEG C, drying time 12h.
In step 3) of the invention, the calcination temperature in tube furnace is 550-650 DEG C, calcination time 0.5-4h, heating
Rate is 2-5 DEG C/min.
In step 4) of the invention, citric acid quality is 5-7g, and urea quality 6-10g, thioacetamide quality is 12-
15g, phosphoric acid quality 20-22g, ammonium hydroxide quality are 25-27g.
In step 5) of the invention, the reaction temperature in reaction kettle is 160-200 DEG C, reaction time 6-12h.
Compared with prior art, the present invention advantage are as follows: (1) composite photocatalyst material have hexagon tubulose microscopic appearance,
Specific surface area with higher and more active site；(2) gained indium sesquioxide nanocomposite, which sufficiently combines, receives
The excellent photo-catalysis capability and carbon quantum dot of rice indium sesquioxide inhibit the compound action of photo-generate electron-hole, concerted catalysis
Excellent effect；(3) reaction condition of target material building is simple, and low for equipment requirements, preparation method is simple；(4) target material
Catalytic effect is excellent；(5) reaction is using deionized water, ethyl alcohol as reaction medium, 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 1.6g indium nitrate and 1.5g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to water afterwards
In thermal response kettle, 12h is reacted at 120 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.It will
Indium sesquioxide precursor obtained is put into tube furnace, and 0.5h is calcined at 550 DEG C, and 2 DEG C/min of heating rate obtains three oxidations two
Indium.5g citric acid is weighed, is dissolved in 40ml deionized water, 30min is stirred.Mixed solution is transferred in hydrothermal reaction kettle afterwards,
6h is reacted at 160 DEG C.After cooling, 10ml acquired solution is taken, indium sesquioxide made from 10mg is added, 30min is stirred, obtains
Indium sesquioxide optic catalytic composite material.
Embodiment 2
It weighs 1.7g indium nitrate and 1.52g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to afterwards
In hydrothermal reaction kettle, 13h is reacted at 130 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.
Indium sesquioxide precursor obtained is put into tube furnace, 1h is calcined at 580 DEG C, 2 DEG C/min of heating rate obtains three oxidations two
Indium.5.5g citric acid is weighed, 8g urea is dissolved in 40ml deionized water, stirs 30min.It is anti-that mixed solution is transferred to hydro-thermal afterwards
It answers in kettle, reacts 6h at 170 DEG C.After cooling, 10ml acquired solution is taken, indium sesquioxide made from 12mg, stirring is added
30min obtains indium sesquioxide optic catalytic composite material.
Embodiment 3
It weighs 1.8g indium nitrate and 1.54g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to afterwards
In hydrothermal reaction kettle, 14h is reacted at 140 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.
Indium sesquioxide precursor obtained is put into tube furnace, 2h is calcined at 600 DEG C, 3 DEG C/min of heating rate obtains three oxidations two
Indium.6g citric acid is weighed, 26g ammonium hydroxide is dissolved in 40ml deionized water, stirs 30min.It is anti-that mixed solution is transferred to hydro-thermal afterwards
It answers in kettle, reacts 8h at 180 DEG C.After cooling, 10ml acquired solution is taken, indium sesquioxide made from 16mg, stirring is added
30min obtains indium sesquioxide optic catalytic composite material.
Embodiment 4
It weighs 1.9g indium nitrate and 1.56g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to afterwards
In hydrothermal reaction kettle, 15h is reacted at 150 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.
Indium sesquioxide precursor obtained is put into tube furnace, 3h is calcined at 620 DEG C, 4 DEG C/min of heating rate obtains three oxidations two
Indium.6.5g citric acid is weighed, 13g thioacetamide is dissolved in 40ml deionized water, stirs 30min.Mixed solution is shifted afterwards
Into hydrothermal reaction kettle, 10h is reacted at 190 DEG C.After cooling, 10ml acquired solution is taken, three oxidation two made from 18mg is added
Indium stirs 30min, obtains indium sesquioxide optic catalytic composite material.
Embodiment 5
It weighs 2g indium nitrate and 1.6g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to hydro-thermal afterwards
In reaction kettle, 16h is reacted at 160 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.It will system
The indium sesquioxide precursor obtained is put into tube furnace, 4h is calcined at 650 DEG C, 5 DEG C/min of heating rate obtains indium sesquioxide.
7g citric acid, 20g phosphoric acid are weighed, 25g ammonium hydroxide is dissolved in 40ml deionized water, stirs 30min.Mixed solution is transferred to water afterwards
In thermal response kettle, 12h is reacted at 200 DEG C.After cooling, 10ml acquired solution is taken, indium sesquioxide made from 20mg is added, stirs
30min is mixed, indium sesquioxide optic catalytic composite material is obtained.
Embodiment 6
It weighs 2g indium nitrate and 1.6g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to hydro-thermal afterwards
In reaction kettle, 16h is reacted at 160 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.It will system
The indium sesquioxide precursor obtained is put into tube furnace, 4h is calcined at 650 DEG C, 5 DEG C/min of heating rate obtains indium sesquioxide.
7g citric acid, 21g phosphoric acid are weighed, 26g ammonium hydroxide is dissolved in 40ml deionized water, stirs 30min.Mixed solution is transferred to water afterwards
In thermal response kettle, 12h is reacted at 200 DEG C.After cooling, 10ml acquired solution is taken, indium sesquioxide made from 20mg is added, stirs
30min is mixed, indium sesquioxide optic catalytic composite material is obtained.
Embodiment 7
It weighs 2g indium nitrate and 1.6g spherical shape urea is dissolved in 40ml, stir 30min.Mixed solution is transferred to hydro-thermal afterwards
In reaction kettle, 16h is reacted at 160 DEG C.After cooling, washing centrifugation in 60 DEG C of dry 12h, obtains indium sesquioxide precursor.It will system
The indium sesquioxide precursor obtained is put into tube furnace, 4h is calcined at 650 DEG C, 5 DEG C/min of heating rate obtains indium sesquioxide.
7g citric acid, 22g phosphoric acid are weighed, 27g ammonium hydroxide is dissolved in 40ml deionized water, stirs 30min.Mixed solution is transferred to water afterwards
In thermal response kettle, 12h is reacted at 200 DEG C.After cooling, 10ml acquired solution is taken, indium sesquioxide made from 20mg is added, stirs
30min is mixed, indium sesquioxide optic catalytic composite material is obtained.
Embodiment 8
Photocatalysis effect test:
1) blank is eliminated.5 gained composite material of 10ml embodiment and 100ml 20mg/l rhodamine B solution are mixed and are put into
250ml beaker.By the opaque container closing of beaker black, with magnetic stirring apparatus under the conditions of being protected from light agitating solution 1h；
2) light degradation.Solution is put into light degradation instrument progress illumination reaction after the reaction was completed to above-mentioned, using simulation nature
The 500w xenon lamp of illumination condition irradiates.It is sampled since 0min, takes a sample every 10min, each sample takes 3~5ml, then
Use molecular sieve filtration.A sample is taken every 20min after reacting and reaching 50min；One is taken every 30min after reacting and reaching 90min
Secondary sample.Illumination to the end of when reaching 120min wait react carries out ultra-violet analysis to 9 samples got in 120min.Experiment
The result shows that mixed solution color is obviously thin out when reaction proceeds to 30min, mixed solution when reaching 90min
Middle rhodamine B concentration is close to 0mg/l.
Claims (6)
1. a kind of construction method of indium sesquioxide optic catalytic composite material, which is characterized in that by being doped with nonmetalloid
Carbon quantum dot and indium sesquioxide are stirred preparation under normal temperature and pressure and form composite material, the specific steps are as follows:
A certain amount of indium nitrate and spherical urea are dissolved in deionized water and are stirred and obtain mixed liquor after a certain period of time by step 1)
It is spare；
Gained mixed liquor in step 1) is transferred in hydrothermal reaction kettle by step 2), certain time is reacted under certain temperature, centrifugation is washed
It washs, dry certain time, is made indium sesquioxide precursor under certain temperature；
Indium sesquioxide precursor obtained by step 2) is put into tube furnace by step 3), calcines certain time under certain temperature, is made
Indium sesquioxide；
A certain amount of citric acid and a certain amount of compound that mixes are dissolved in deionized water by step 4), and stirring certain time obtains
Mixed liquor is spare；Wherein, mixing compound is urea, thioacetamide, phosphoric acid, any one in ammonium hydroxide；
Gained mixed liquor in step 4) is transferred in hydrothermal reaction kettle by step 5), is reacted certain time under certain temperature, is made and mixes
The miscellaneous carbon quantum dot solution of nonmetalloid；
At normal temperatures and pressures, stirring is mixed for the indium sesquioxide that step 6) prepares gained carbon quantum solution in step 5) and step 3)
Conjunction obtains composite semiconductor light-catalyst, and every milliliter of carbon quantum solution needs to be added indium sesquioxide 1-2mg.
2. a kind of construction method of indium sesquioxide optic catalytic composite material according to claim 1, it is characterised in that: step
It is rapid 1) in, indium nitrate quality is 1.6-2.0g, and spherical urea quality is 1.5-1.6g, and deionized water volume is 40ml, when stirring
Between be 30min.
3. a kind of construction method of indium sesquioxide optic catalytic composite material according to claim 1, it is characterised in that: step
It is rapid 2) in, reaction temperature in reaction kettle is 120-160 DEG C, reaction time 12-16h, and drying temperature is 60 DEG C, drying time
For 12h.
4. a kind of construction method of indium sesquioxide optic catalytic composite material according to claim 1, it is characterised in that: step
It is rapid 3) in, calcination temperature in tube furnace is 550-650 DEG C, calcination time 0.5-4h, and heating rate is 2-5 DEG C/min.
5. a kind of construction method of indium sesquioxide optic catalytic composite material according to claim 1, it is characterised in that: step
It is rapid 4) in, citric acid quality be 5-7g, urea quality 6-10g, thioacetamide quality be 12-15g, phosphoric acid quality 20-
22g, ammonium hydroxide quality are 25-27g.
6. a kind of construction method of indium sesquioxide optic catalytic composite material according to claim 1, it is characterised in that: step
It is rapid 5) in, reaction temperature in reaction kettle is 160-200 DEG C, reaction time 6-12h.
Priority Applications (1)
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