CN108404994A - A kind of preparation method of the phthalocyanine-sensitized indium sulfide tin composite visible light catalyst of nitro cobalt - Google Patents
A kind of preparation method of the phthalocyanine-sensitized indium sulfide tin composite visible light catalyst of nitro cobalt Download PDFInfo
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- CN108404994A CN108404994A CN201810217994.0A CN201810217994A CN108404994A CN 108404994 A CN108404994 A CN 108404994A CN 201810217994 A CN201810217994 A CN 201810217994A CN 108404994 A CN108404994 A CN 108404994A
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- indium sulfide
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- phthalocyanine
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- GEEGFFDUNIISFE-UHFFFAOYSA-N [O-][N+]([Co])=O Chemical compound [O-][N+]([Co])=O GEEGFFDUNIISFE-UHFFFAOYSA-N 0.000 title claims abstract description 30
- AUPDDIHBWUKWPI-UHFFFAOYSA-N [In]=S.[Sn] Chemical compound [In]=S.[Sn] AUPDDIHBWUKWPI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 title claims description 15
- 239000011941 photocatalyst Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000001007 phthalocyanine dye Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 8
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 4
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 4
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 4
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- JKXCZYCVHPKTPK-UHFFFAOYSA-N hydrate;trihydrochloride Chemical compound O.Cl.Cl.Cl JKXCZYCVHPKTPK-UHFFFAOYSA-N 0.000 claims 1
- 206010070834 Sensitisation Diseases 0.000 abstract description 10
- 230000008313 sensitization Effects 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 8
- 229940107698 malachite green Drugs 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 241000254173 Coleoptera Species 0.000 description 1
- -1 Phthalocyanine compound Chemical class 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000003911 water pollution Methods 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1825—Ligands comprising condensed ring systems, e.g. acridine, carbazole
- B01J31/183—Ligands comprising condensed ring systems, e.g. acridine, carbazole with more than one complexing nitrogen atom, e.g. phenanthroline
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of nitro cobalt phthalocyanine dye (CoTNPc) sensitization indium sulfide tin (SnIn4S8) composite photo-catalyst preparation, wherein preparing material step and including：The synthesis of nitro cobalt phthalocyanine dye, flower-shaped indium sulfide tin (SnIn4S8) the phthalocyanine-sensitized indium sulfide tin (CoTNPc/SnIn of preparation and nitro cobalt4S8) composite material preparation.The beneficial effects of the present invention are the method for preparing composite photocatalyst material is simple, reaction process is easy to control, and photocatalysis performance is improved, it is seen that light utilization ratio improves, and has certain application value.
Description
Technical field
The invention belongs to nano material preparation and applied technical fields, are related to a kind of nitro cobalt phthalocyanine (CoTNPc) sensitization sulphur
Change indium tin (SnIn4S8) composite visible light catalyst preparation method.
Background technology
Industrialized ecology potential must bring problem of environmental pollution, and the processing of wherein water pollution is extremely urgent, and light
Catalysis technique be increasingly becoming curb environmental pollution and the technology of the most critical of energy shortage problem it.So far it more and more grinds
Study carefully scholar to start to join in photocatalysis field.It is well known that directly having proved to be a kind of using solar radiation come drive response
Science, effective green method, the visible optical radiation in solar energy accounts for the 43% of gross energy, therefore efficiently utilizes visible luminous energy
Source becomes the most important thing of photocatalysis research.Indium sulfide tin is the ternary sulfide with visible light catalytic performance of recent report
Semiconductor, band gap 1.81eV, valence band current potential are 1.60eV, and conduction band current potential is -0.21eV.Due to its energy gap compared with
Narrow, indium sulfide tin has strong absorption in visible light region, is the novel photocatalysis material with broad development space.But
Research shows that there are still the high recombination rates of photo-generate electron-hole pair, therefore greatly limits it and be widely applied
Phthalocyanine compound is the very high compound of a kind of chemical stability, since it is with good heat-resisting, sun-proof, resistance to
Acid, alkali resistance and the performances such as bright and lustrous, are initially mainly used for pigment, dyestuff and printing and dyeing industry, and intramolecular has 18 electricity
The big conjugated system of son, structure is more stable, and electron-transport is more convenient.And phthalocyanine has strong inhale in visible light near infrared region
It receives, therefore visible light energy can be more made full use of using phthalocyanine dye sensitization indium sulfide tin, special molecular structure allows light
Raw electronics transfer is rapider, to reduce the compound again of hole-electron pair.This patent mainly uses ultrasonic immersing method sensitization system
The composite visible light catalyst of standby nitro cobalt phthalocyanine/indium sulfide tin.This catalyst can be applied in photocatalysis technology, using too
Positive energy fast and effeciently removes the organic pollution in water.
Invention content
The technical problem to be solved by the present invention is to：Based on the above issues, the present invention provides a kind of nitro cobalt phthalocyanine
(CoTNPc) sensitization indium sulfide tin (SnIn4S8) composite visible light catalyst preparation method.
The present invention solves a technical solution used by its technical problem：A kind of nitro cobalt phthalocyanine (CoTNPc) sensitization
Indium sulfide tin (SnIn4S8) composite visible light catalyst preparation method, include the following steps：
((1) flower-shaped indium sulfide tin (SnIn4S8) preparation：By SnCl4·5H2O and InCl3·4H2O is dissolved in absolute ethyl alcohol
In, it is mixed evenly, thioacetamide is added, continue to be transferred to stainless steel autoclave after stirring 30min, at 160 DEG C
Reaction time 12h.Gained yellow powder water and ethyl alcohol are washed to remove impurity, centrifugal filtration it is dry product.
(2) preparation of nitro cobalt phthalocyanine：A three-necked flask is taken, by 3- nitrophthalonitriles and CoCl2·6H2O is dissolved in
In 100mL n-pentanol solutions and 1mL 1,11 carbon -7- alkene (DBU) of 8- diazabicylos, in the atmosphere of 130 DEG C of nitrogen is added
Heating stirring 6h.Obtained sample distilled water and absolute methanol clean several times, to ensure that DMF dissolvings remove completely, then exist
At 80 DEG C product is obtained after dry 8h；
(3) preparation of the phthalocyanine-sensitized flower-shaped indium sulfide tin composite photo-catalyst of nitro cobalt：It weighs in step (1) after drying
The SnIn of certain mass4S8It is scattered in ethanol solution, nitro cobalt phthalocyanine is dissolved in DMF solution in step (2), waits for it
Phthalocyanine solution is added dropwise in indium sulfide tin after dissolving, is continued after stirring 12h, ultrasonic reaction 4-5h.Obtained sample nothing
Water-ethanol and water washing, centrifugal drying obtain product.
Further, SnCl in the step (1)4·5H2O、InCl3·4H2O, thioacetamide and absolute ethyl alcohol
Molar ratio is 1:4:8:1370, the density of absolute ethyl alcohol is 0.789g/cm3；
Further, 3- nitrophthalonitriles and CoCl in the step (2)2·6H2O molar ratios are 2:1；
Further, CoTNPc in the step (3):SnIn4S8Mass ratio is respectively 5wt%, 10wt%, 25wt%.
Nitro cobalt phthalocyanine (CoTNPc) is sensitized indium sulfide tin (SnIn4S8) composite visible light catalyst application, urged for light
Change degrading malachite green (MG) solution, carries out as steps described below：
It weighs 20mg catalyst to be put into test tube, 50mL 50mg/L MG solution is added, with 420nm optical filters
1000W xenon lamps carry out photocatalytic degradation reaction as light source.Dark reaction time is 30min, and after illumination, time sample is taken per 20min,
It is centrifuged, and then surveys its absorbance.
The beneficial effects of the invention are as follows：The preparation method is simple, and reaction process is easy to control, prepared nitro cobalt phthalocyanine
(CoTNPc) sensitization indium sulfide tin (SnIn4S8) the visible light utilization ratio of composite visible light catalyst is high, photocatalysis performance is carried
Height has certain application value.
Description of the drawings
The following further describes the present invention with reference to the drawings.
Fig. 1 is nitro cobalt phthalocyanine (CoTNPc) the sensitization indium sulfide tin (SnIn that the embodiment of the present invention 1 is prepared4S8) multiple
The scanning electron microscope (SEM) photograph (a) and transmission electron microscope picture (b) of closing light catalyst；
Fig. 2 is nitro cobalt phthalocyanine (CoTNPc) the sensitization indium sulfide tin (SnIn that the embodiment of the present invention 1 is prepared4S8) pure
The X-ray diffractogram of sample and composite photo-catalyst；
Fig. 3 is nitro cobalt phthalocyanine (CoTNPc) the sensitization indium sulfide tin (SnIn that the embodiment of the present invention 1 is prepared4S8) multiple
The activity figure of closing light catalyst degradation malachite green.
Specific implementation mode
Presently in connection with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
(1) floriform cadmium sulfide (SnIn4S8) preparation：By 0.49mmol SnCl4·5H2O (0.1728g) and 1.96mmol
InCl3·4H2O (0.5786g) is added in 40mL ethanol solutions, and after stirring to solution is clarified, it is thio that 3.94mmol is added
Acetamide (0.2962g) seals in persistently stirring half an hour and the 100mL autoclaves that are transferred to, at 160 DEG C, reaction time 12h.
Gained yellow powder water and ethyl alcohol are washed to remove impurity, centrifugal filtration it is dry product；
(2) preparation of nitro cobalt phthalocyanine：Take a three-necked flask, weigh 3- nitrophthalonitriles (1.3850g,
8mmol) and CoCl2·6H2O (0.9517g, 4mmol) is dissolved in 100mL n-pentanol solutions, and 1mL 8- diazas are added
Two rings, 11 carbon -7- alkene (DBU), the heating stirring 6h in the atmosphere of 130 DEG C of nitrogen.Obtained sample distilled water and without water beetle
Alcohol cleans several times, to ensure that DMF dissolvings remove completely, then obtains product after dry 8h at 80 DEG C；
(3) 10wt%-CoTNPc/SnIn4S8The preparation of composite photo-catalyst：By the 100mg's in step (1) after drying
Floriform cadmium sulfide (SnIn4S8) be dissolved in 40mL absolute ethyl alcohols, 10mg CoTNPc are dissolved in DMF (20mL) in step (2), so
Solution is transferred in 100ml autoclaves afterwards, and autoclave is sealed and is heated for 24 hours in 120 DEG C of baking oven.By phthalein after its dissolving
Cyanines solution is added dropwise in indium sulfide tin, continues after stirring 12h, ultrasonic reaction 4-5h.Obtained sample absolute ethyl alcohol and water
Washing, centrifugal drying obtain product.
Scanning electron microscope (SEM) photograph is as shown in Figure 1, as can be seen from Fig., nitro cobalt phthalocyanine (CoTNPc) prepared by present embodiment is quick
Change indium sulfide tin (SnIn4S8) composite photo-catalyst pattern be flower-shaped indium sulfide tin surfaces coat nitro cobalt phthalocyanine (CoTNPc),
And distribution is more uniform.
X ray diffracting spectrum is as shown in Fig. 2, as seen from the figure, the nitro cobalt phthalocyanine (CoTNPc) of preparation is sensitized indium sulfide tin
(SnIn4S8) the feature diffraction for occurring nitro cobalt phthalocyanine (CoTNPc) at 26.7 ° can be seen in the figure in composite photo-catalyst XRD diffraction
Peak, 9.4 °, 18.5 °, 28.2 °, 33.2 °, 47.7 ° are flower-shaped indium sulfide tin (SnIn with 50.0 °4S8) characteristic diffraction peak.Cause
This, can prove nitro cobalt phthalocyanine (CoTNPc) and indium sulfide tin (SnIn4S8) be combined with each other, and do not change itself crystal form,
This is consistent with the result of Electronic Speculum.Application examples：Catalytic degradation malachite green (MG)
20mg different catalysts are weighed respectively to be put into test tube, and 50ml 50mg/L MG solution is added, is filtered with 420nm
The 1000W xenon lamps of mating plate carry out photocatalytic degradation reaction as light source.Dark reaction time is 30min, after illumination, every
20min takes time sample, and high speed centrifugation under the conditions of 4000rpm, takes supernatant liquor about 2mL solution ultraviolet-uisible spectrophotometers
Survey the variation of its concentration.As seen from Figure 3, in 100min malachite green degradation rate to reach 99.2%, it is seen that prepared 10%-
CoTNPc/SnIn4S8Composite photo-catalyst has higher photocatalytic activity.
Claims (4)
1. a kind of preparation method of the phthalocyanine-sensitized indium sulfide tin composite visible light catalyst of nitro cobalt, which is characterized in that including with
Lower step：
(1) flower-shaped indium sulfide tin (SnIn4S8) preparation：By SnCl4·5H2O and InCl3·4H2O is dissolved in absolute ethyl alcohol, is mixed
Conjunction stirs evenly, and thioacetamide is added, and continues to be transferred to stainless steel autoclave after stirring 30min, when reacting at 160 DEG C
Between 12h.Gained yellow powder water and ethyl alcohol are washed to remove impurity, centrifugal filtration it is dry product.
(2) preparation of nitro cobalt phthalocyanine (CoTNPc)：A three-necked flask is taken, by 3- nitrophthalonitriles and CoCl2·6H2O
It is dissolved in 100mL n-pentanol solutions and is added 1mL 1,11 carbon -7- alkene (DBU) of 8- diazabicylos, in the atmosphere of 130 DEG C of nitrogen
Enclose middle heating stirring 6h.Obtained sample distilled water and absolute methanol clean several times, to ensure that DMF dissolvings remove completely, so
Afterwards product is obtained after dry 8h at 80 DEG C；
(3) nitro cobalt phthalocyanine (CoTNPc) is sensitized flower-shaped indium sulfide tin (SnIn4S8) composite photo-catalyst preparation：Weigh step
(1) SnIn of the certain mass in after drying4S8It is scattered in ethanol solution, nitro cobalt phthalocyanine is dissolved in step (2)
In DMF solution, phthalocyanine solution is added dropwise in indium sulfide tin after its dissolving, is continued after stirring 12h, ultrasonic reaction 4-5h.
Obtained sample absolute ethyl alcohol and water washing, centrifugal drying obtain product.
2. a kind of preparation method of nitro cobalt phthalocyanine/indium sulfide tin composite visible light catalyst according to claim 1,
It is characterized in：Tin tetrachloride pentahydrate in the step (1), four trichloride hydrate indiums, thioacetamide and absolute ethyl alcohol rub
You are than being 1:4:8:1370, the density of absolute ethyl alcohol is 0.789g/cm3。
3. a kind of preparation method of nitro cobalt phthalocyanine dye according to claim 1, it is characterized in that：The step (2)
Middle 3- nitrophthalonitriles and CoCl2·6H2O molar ratios are 2:1.
4. the phthalocyanine-sensitized indium sulfide tin (SnIn of a kind of nitro cobalt according to claim 14S8) composite photo-catalyst system
It is standby, it is characterized in that：Flower-shaped indium sulfide tin (SnIn in the step (3)4S8) quality be 100-500mg, and CoTNPc:
SnIn4S8Mass ratio is respectively 5wt%, 10wt%, 25wt%.
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| CN201810217994.0A CN108404994A (en) | 2018-03-16 | 2018-03-16 | A kind of preparation method of the phthalocyanine-sensitized indium sulfide tin composite visible light catalyst of nitro cobalt |
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| CN201810217994.0A CN108404994A (en) | 2018-03-16 | 2018-03-16 | A kind of preparation method of the phthalocyanine-sensitized indium sulfide tin composite visible light catalyst of nitro cobalt |
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| CN111250109A (en) * | 2020-01-19 | 2020-06-09 | 浙江树人学院（浙江树人大学） | Preparation method of indium tin sulfide visible-light-driven photocatalyst and application of visible-light-driven photocatalyst |
| CN115337944A (en) * | 2022-08-18 | 2022-11-15 | 西安建筑科技大学 | Ti 3 C 2 /In 4 SnS 8 Composite material and preparation method and application thereof |
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