CN109675547A - A kind of preparation method and applications of hollow cube type zinc stannate photochemical catalyst - Google Patents
A kind of preparation method and applications of hollow cube type zinc stannate photochemical catalyst Download PDFInfo
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- CN109675547A CN109675547A CN201910008370.2A CN201910008370A CN109675547A CN 109675547 A CN109675547 A CN 109675547A CN 201910008370 A CN201910008370 A CN 201910008370A CN 109675547 A CN109675547 A CN 109675547A
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- photochemical catalyst
- zinc stannate
- hollow cube
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- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 13
- 238000003760 magnetic stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 239000011592 zinc chloride Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 5
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910007694 ZnSnO3 Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910007717 ZnSnO Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-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
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
-
- 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—
-
- B01J35/39—
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
Abstract
The invention discloses a kind of preparation method and applications of hollow cube type zinc stannate photochemical catalyst, there is the zinc stannate photochemical catalyst of hollow cube structure using Co deposited synthesis, the final visible light catalyst for obtaining high activity, the photochemical catalyst has the characteristic of the efficient degradation organic pollutant under simulated solar irradiation irradiation, for expanding the industrial applications range of nano photo catalyzed oxidation degrading waste water pollutant, saving wastewater treatment energy consumption, it is of great immediate significance.
Description
Technical field
The invention belongs to the synthesis technical fields of catalysis material, and in particular to a kind of hollow cube type zinc stannate light is urged
The preparation method and applications of agent.
Background technique
In recent years, the advantages that photocatalysis technology is energy-efficient with its, without secondary pollution, applied widely is in difficult for biological degradation
Good application prospect is shown in treatment of Organic Wastewater.It effectively can convert small point for macromolecular in a mild condition
Son, therefore can be used for purified industrial waste water, it is hydrogen and oxygen to obtain clean renewable energy by water decomposition.TiO2It is to grind
Study carefully most photochemical catalysts, but its quantum yield is low, solar energy utilization ratio is low, and this greatly limits its application ranges.
Therefore, the heat that the novel photocatalyst with the feature of environmental protection and high efficiency and visible light photocatalytic activity has become photocatalysis research is developed
Point.
N-type semiconductor ZnSnO3Due to its high electron mobility and high conductivity, in photocatalysis, photoelectric device and battery
Functional coating etc. has potential application.A large number of studies show that different synthetic methods not only influences ZnSnO3Particle
The Morphologic Characteristics such as size, shape and its crystal form also will affect its optical property and its catalytic activity.ZnSnO3There are many close
At method, such as: thermal evaporation, coprecipitation and hydrothermal synthesis etc..Wherein, it is excellent to have that synthesis is simple, low energy consumption etc. for coprecipitation
Point has great industrial applications prospect.Hollow structure often than the particle of same particle size have bigger specific surface area and
Permeance property, thus there is better absorption property and photocatalytic activity.There is hollow cube knot using Co deposited synthesis
The ZnSnO of structure3It is expected to obtain the visible light catalyst of high activity, for expanding nano photo catalyzed oxidation degrading waste water pollutant
Industrial applications range saves wastewater treatment energy consumption, is of great immediate significance.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple process and low-cost hollow cube type stannic acids
The preparation method of zinc photochemical catalyst, photochemical catalyst made from this method have the organic dirt of efficient degradation under simulated solar irradiation irradiation
Contaminate the characteristic of object.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of hollow cube type zinc stannate photocatalysis
The preparation method of agent, it is characterised in that specific steps are as follows: by 1.363g ZnCl2It is dissolved in 100mL water, on magnetic stirring apparatus
2.941g sodium citrate is added after being uniformly mixed, continues stirring 30min and obtains solution A；3.506g SnCl is weighed again4·
5H2O is dissolved in 50mL ethanol solution, obtains solution B after stirring and dissolving is complete on magnetic stirring apparatus, and solution B is mixed with solution A
It reacts 30min under agitation afterwards, the NaOH solution that 25mL molar concentration is 0.41-1.67mol/L is then added dropwise dropwise, it is molten
Liquid is gradually muddy, and sediment centrifugation, washing are placed in drying box and are dried, then be placed in mortar and grind after reacting 15min
To precursor species, precursor species are placed in tube furnace and obtains hollow cube type zinc stannate light in 300 DEG C of calcining 3h and urges
Agent.
Hollow cube type zinc stannate photochemical catalyst of the present invention efficient degradation organic contamination under sunlight irradiation
Application in object, it is characterised in that detailed process are as follows: by 1.363g ZnCl2It is dissolved in 100mL water, is stirred on magnetic stirring apparatus
Addition 2.941g sodium citrate after mixing is mixed, continues stirring 30min and obtains solution A；3.506g SnCl is weighed again4·5H2O
Be dissolved in 50mL ethanol solution, obtain solution B after stirring and dissolving is complete on magnetic stirring apparatus, after solution B is mixed with solution A
30min is reacted under stirring condition, the NaOH solution that 25mL molar concentration is 0.41mol/L is then added dropwise dropwise, and solution is gradually muddy
It is turbid, sediment centrifugation, washing are placed in drying box and are dried after reacting 15min, then is placed in grinding in mortar and obtains presoma
Precursor species are placed in tube furnace and obtain hollow cube type zinc stannate photochemical catalyst, the tin in 300 DEG C of calcining 3h by substance
Sour zinc photochemical catalyst irradiates 120min by simulated solar irradiation, and the removal rate to the methylene blue waste water of 10mg/L is 98%.
Compared with the prior art, the invention has the following beneficial effects: the present invention is prepared using simple chemical precipitation method
With hollow cube type zinc stannate photochemical catalyst, there is photochemical catalyst obtained the efficient degradation under simulated solar irradiation irradiation to have
The characteristic of machine pollutant.
Detailed description of the invention
Fig. 1 is the XRD diagram of hollow cube type zinc stannate photochemical catalyst made from embodiment 3；
Fig. 2 is the SEM figure of hollow cube type zinc stannate photochemical catalyst made from embodiment 3.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
By 1.363g ZnCl2It is dissolved in 100mL water, 2.941g citric acid is added after being uniformly mixed on magnetic stirring apparatus
Sodium continues stirring 30min and obtains solution A；3.506g SnCl is weighed again4·5H2O is dissolved in 50mL ethanol solution, in magnetic agitation
Solution B is obtained after stirring and dissolving is complete on device, will solution B and solution A mix after react 30min under agitation, then by
The NaOH solution that 25mL molar concentration is 1.67mol/L is added dropwise in drop, and solution is gradually muddy, be centrifuged sediment after reaction 15min,
Washing, which is placed in drying box, dries, then is placed in grinding in mortar and obtains precursor species, and precursor species are placed in tube furnace
In in 300 DEG C of calcining 3h obtain hollow cube type zinc stannate photochemical catalyst, which passes through simulated solar irradiation
120min is irradiated, the removal rate to the methylene blue waste water of 10mg/L is 34.37%.
Embodiment 2
By 1.363g ZnCl2It is dissolved in 100mL water, 2.941g citric acid is added after being uniformly mixed on magnetic stirring apparatus
Sodium continues stirring 30min and obtains solution A；3.506g SnCl is weighed again4·5H2O is dissolved in 50mL ethanol solution, in magnetic agitation
Solution B is obtained after stirring and dissolving is complete on device, will solution B and solution A mix after react 30min under agitation, then by
The NaOH solution that 25mL molar concentration is 1mol/L is added dropwise in drop, and solution is gradually muddy, by sediment centrifugation, water after reaction 15min
It washes to be placed in drying box and dry, then be placed in grinding in mortar and obtain precursor species, precursor species are placed in tube furnace
Hollow cube type zinc stannate photochemical catalyst is obtained in 300 DEG C of calcining 3h, which passes through simulated solar illumination
120min is penetrated, the removal rate to the methylene blue waste water of 10mg/L is 46.28%.
Embodiment 3
By 1.363g ZnCl2It is dissolved in 100mL water, 2.941g citric acid is added after being uniformly mixed on magnetic stirring apparatus
Sodium continues stirring 30min and obtains solution A；3.506g SnCl is weighed again4·5H2O is dissolved in 50mL ethanol solution, in magnetic agitation
Solution B is obtained after stirring and dissolving is complete on device, will solution B and solution A mix after react 30min under agitation, then by
The NaOH solution that 25mL molar concentration is 0.41mol/L is added dropwise in drop, and solution is gradually muddy, be centrifuged sediment after reaction 15min,
Washing, which is placed in drying box, dries, then is placed in grinding in mortar and obtains precursor species, and precursor species are placed in tube furnace
In in 300 DEG C of calcining 3h obtain hollow cube type zinc stannate photochemical catalyst, which passes through simulated solar irradiation
120min is irradiated, the removal rate to the methylene blue waste water of 10mg/L is 98%.
Based on above embodiments, the molar concentration for choosing NaOH solution is the zinc stannate photochemical catalyst of 0.41mol/L preparation
Performance it is more excellent, by further characterizing research, the zinc stannate photochemical catalyst prepared under this condition have hollow cube knot
Structure, compared to traditional catalysis material, zinc stannate photochemical catalyst produced by the present invention is able to respond nature sunlight, and having can
Light-exposed catalytic activity, and preparation method is simple and quick, it is without secondary pollution.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of preparation method of hollow cube type zinc stannate photochemical catalyst, it is characterised in that specific steps are as follows: by 1.363g
ZnCl2It is dissolved in 100mL water, 2.941g sodium citrate is added after being uniformly mixed on magnetic stirring apparatus, continues to stir
30min obtains solution A；3.506g SnCl is weighed again4·5H2O is dissolved in 50mL ethanol solution, the stirring and dissolving on magnetic stirring apparatus
Solution B is obtained after completely, reacts 30min under agitation after solution B is mixed with solution A, 25mL is then added dropwise dropwise and rubs
The NaOH solution that your concentration is 0.41-1.67mol/L, solution is gradually muddy, and sediment is centrifuged, after washing after reacting 15min
It is placed in drying box and dries, then be placed in grinding in mortar and obtain precursor species, precursor species are placed in tube furnace in 300
DEG C calcining 3h obtain hollow cube type zinc stannate photochemical catalyst.
2. hollow cube type zinc stannate photochemical catalyst made from the method according to claim 11 is high under sunlight irradiation
Imitate the application in degradable organic pollutant, it is characterised in that detailed process are as follows: by 1.363g ZnCl2It is dissolved in 100mL water,
2.941g sodium citrate is added after being uniformly mixed on magnetic stirring apparatus, continues stirring 30min and obtains solution A；It weighs again
3.506g SnCl4·5H2O is dissolved in 50mL ethanol solution, obtains solution B after stirring and dissolving is complete on magnetic stirring apparatus, will be molten
Liquid B reacts 30min after mixing with solution A under agitation, and it is 0.41mol/L's that 25mL molar concentration is then added dropwise dropwise
NaOH solution, solution is gradually muddy, and sediment centrifugation, washing are placed in drying box and are dried, then be placed in and grind after reacting 15min
Grinding obtains precursor species in alms bowl, and precursor species are placed in tube furnace and obtain hollow cube type in 300 DEG C of calcining 3h
Zinc stannate photochemical catalyst, the zinc stannate photochemical catalyst irradiate 120min by simulated solar irradiation, useless to the methylene blue of 10mg/L
The removal rate of water is 98%.
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| CN201910008370.2A Pending CN109675547A (en) | 2019-01-04 | 2019-01-04 | A kind of preparation method and applications of hollow cube type zinc stannate photochemical catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110038551A (en) * | 2019-05-28 | 2019-07-23 | 河南师范大学 | Zinc stannate photochemical catalyst and preparation method thereof with hollow polyhedron structure |
| CN110038550A (en) * | 2019-05-28 | 2019-07-23 | 河南师范大学 | A kind of preparation method and applications of visible-light response type Zn2SnO4/ZnO/SnO2 composite photocatalyst material |
| CN110887871A (en) * | 2019-11-27 | 2020-03-17 | 哈尔滨师范大学 | Oxygen-enriched defect zinc stannate material, synthesis method thereof and hydrogen sulfide early warning sensor |
| CN111244423A (en) * | 2020-01-19 | 2020-06-05 | 杭州电子科技大学 | NiO-coated ZnSnO3Preparation method of cubic composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110038551A (en) * | 2019-05-28 | 2019-07-23 | 河南师范大学 | Zinc stannate photochemical catalyst and preparation method thereof with hollow polyhedron structure |
| CN110038550A (en) * | 2019-05-28 | 2019-07-23 | 河南师范大学 | A kind of preparation method and applications of visible-light response type Zn2SnO4/ZnO/SnO2 composite photocatalyst material |
| CN110887871A (en) * | 2019-11-27 | 2020-03-17 | 哈尔滨师范大学 | Oxygen-enriched defect zinc stannate material, synthesis method thereof and hydrogen sulfide early warning sensor |
| CN111244423A (en) * | 2020-01-19 | 2020-06-05 | 杭州电子科技大学 | NiO-coated ZnSnO3Preparation method of cubic composite material |
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Application publication date: 20190426 |