CN111921525A - Preparation method of palladium-doped tin dioxide spherical nano material - Google Patents
Preparation method of palladium-doped tin dioxide spherical nano material Download PDFInfo
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- CN111921525A CN111921525A CN202010698432.XA CN202010698432A CN111921525A CN 111921525 A CN111921525 A CN 111921525A CN 202010698432 A CN202010698432 A CN 202010698432A CN 111921525 A CN111921525 A CN 111921525A
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- palladium
- tin dioxide
- mixed solution
- doped tin
- dioxide spherical
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000011259 mixed solution Substances 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 11
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 3
- 229910000510 noble metal Inorganic materials 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 7
- 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 4
- 229940107698 malachite green Drugs 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005286 illumination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910003445 palladium oxide Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910021509 tin(II) hydroxide Inorganic materials 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
- B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
- B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
-
- B01J35/39—
-
- B01J35/40—
-
- B01J35/51—
-
- 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
-
- 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 preparation method of a palladium-doped tin dioxide spherical nano material, which comprises the following steps: mixing stannous sulfate, citric acid and polyvinylpyrrolidone, adding the mixture into deionized water, stirring to obtain a mixed solution, adding palladium chloride into the mixed solution, and stirring to obtain a mixed solution; placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, cooling, and then carrying out centrifugal separation on a reaction kettle bottom product to obtain a sample; and washing the sample by sequentially adopting deionized water and ethanol to obtain the palladium-doped tin dioxide spherical nano material. The noble metal ions are doped and modified to prepare the semiconductor tin dioxide with wider band gap, so that the recombination of electrons and holes in a semiconductor structure can be effectively controlled, and the response range scale to light can be widened, thereby maximally utilizing the light energy.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and relates to a preparation method of a palladium-doped tin dioxide spherical nano material.
Background
The research of the photocatalysis technology is being carried out in a large range, and the research in the field of wastewater treatment is greatly advanced. Compared with the traditional oxidant, the semiconductor serving as the photocatalyst has many advantages, pollutants can be completely mineralized at room temperature by using sunlight or near ultraviolet irradiation, and secondary pollution cannot be caused.
Existing tin dioxide (SnO)2) The photocatalytic material has the defects of wide band gap, low light energy utilization rate, easy recombination of photon-generated carriers and the like, so the photocatalytic performance of the material is improved by doping modification.
Disclosure of Invention
The invention aims to provide a preparation method of a palladium-doped tin dioxide spherical nano material, which solves the problem that a photon-generated carrier is easy to compound in the prior art.
The technical scheme adopted by the invention is that the preparation method of the palladium-doped tin dioxide spherical nano material comprises the following steps:
step 2, placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, cooling, and then carrying out centrifugal separation on a reaction kettle bottom product to obtain a sample;
and 3, washing the sample by sequentially adopting deionized water and ethanol to obtain the palladium-doped tin dioxide spherical nano material.
The invention is also characterized in that:
the ratio of stannous sulfate to citric acid to polyvinylpyrrolidone to palladium chloride is 1:6:2: 0.01-1: 6:2: 0.04.
The centrifugal separation process in the step 2 comprises the following steps: and (3) rinsing the kettle bottom product by using deionized water, transferring the kettle bottom product to a centrifugal tube, centrifuging for 1min at the rotating speed of 5000r/min, pouring out the upper-layer waste liquid, and obtaining a sample in the centrifugal tube.
The hydrothermal reaction temperature in the step 2 is 160-180 ℃.
The hydrothermal reaction time in the step 2 is 15-20 h.
The invention has the beneficial effects that:
the preparation method of the palladium-doped tin dioxide spherical nano material can enable a coupling system to be formed between metal palladium and tin dioxide better; the noble metal ions are doped and modified to prepare the semiconductor tin dioxide with wider band gap, so that the recombination of electrons and holes in a semiconductor structure can be effectively controlled, and the response range scale to light can be widened, thereby maximally utilizing the light energy. The preparation process is simple, and the photocatalyst has good photocatalytic activity on the malachite green solution under the condition of illumination for 3 hours.
Drawings
FIG. 1 is an SEM image of a palladium-doped tin dioxide spherical nanomaterial obtained by the preparation method of the present invention;
FIG. 2 is a high-power SEM image of a palladium-doped tin dioxide spherical nanomaterial obtained by the preparation method of the present invention;
FIG. 3 is an EDS diagram of the palladium-doped tin dioxide spherical nano-material obtained by the preparation method of the invention;
FIG. 4 is a diagram of the photocatalytic performance of the palladium-doped tin dioxide spherical nanomaterial obtained by the preparation method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a palladium-doped tin dioxide spherical nano material, which comprises the following steps:
SnO2Can be obtained by hydrolyzing tin salt, and the specific reaction is as follows:
Sn 2++2H2O→Sn(OH)2+2H+
Sn(OH)4+2OH-→Sn(OH)6 2-
Sn(OH)6 2-→SnO2+2OH-+2H2O
wherein, the citric acid and the polyvinylpyrrolidone can play a role in regulating and controlling the appearance. Polyvinylpyrrolidone in SnO2The formation process of the structure plays an important role. Polyvinylpyrrolidone has a long chain structure with a large amount of hydrophilicity "-CH" along its long chain2-CH2The existence of the group can be used as a soft template to control the morphology, and the palladium chloride can provide palladium elements required by doping.
Step 2, placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the temperature of 160-180 ℃ for 15-20 h, cooling, and then performing centrifugal separation on a reaction kettle bottom product to obtain a sample;
and 3, washing the sample by sequentially adopting deionized water and ethanol to obtain the palladium-doped tin dioxide spherical nano material.
Through the mode, the preparation method of the palladium-doped tin dioxide spherical nano material can enable a coupling system to be formed between metal palladium and tin dioxide better; the noble metal ions are doped and modified to prepare the semiconductor tin dioxide with wider band gap, so that the recombination of electrons and holes in a semiconductor structure can be effectively controlled, and the response range scale to light can be widened, thereby maximally utilizing the light energy. The preparation process is simple, and the photocatalyst has good photocatalytic activity on the malachite green solution under the condition of illumination for 3 hours.
Example 1
step 2, placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the reaction temperature of 180 ℃ for 15 hours, cooling, then wetting and washing a kettle bottom product with deionized water, transferring the kettle bottom product to a centrifugal tube, centrifuging for 1min at 5000r/min, pouring out the upper-layer waste liquid after centrifugation, and obtaining a sample in the centrifugal tube;
step 3, adding deionized water into the centrifugal tube for washing, and repeating for four times; and then the steps are repeated by ethanol for four times to obtain the palladium-doped tin dioxide spherical nano material.
Example 2
step 2, placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the temperature of 160 ℃ for 18 hours, and cooling and then carrying out centrifugal separation on a reaction kettle bottom product to obtain a sample;
and 3, washing the sample by sequentially adopting deionized water and ethanol to obtain the palladium-doped tin dioxide spherical nano material. The SEM image of the product is shown in FIG. 1, the high power SEM image is shown in FIG. 2, and the EDS image is shown in FIG. 3. As can be seen from FIG. 1 and FIG. 2, the product produced consisted of a large number of hollow spherical masses, SnO produced in example 22The diameter of the sphere is 450-650nm, the hollow number of the sphere is more, and the appearance is good; from fig. 3, it can be seen that trace Pd element is doped in the nanomaterial. Other elements such as C, O appear in the element list due to the use of conductive gel during the analysis. The photocatalytic performance of the palladium-doped tin dioxide spherical nano material prepared by the embodiment on the malachite green solution is tested,as shown in FIG. 4, the results show that the nanomaterial prepared by the embodiment has good photocatalytic activity on a malachite green solution, and the degradation rate reaches 80% after illumination for 3 hours.
Example 3
step 2, placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction at the reaction temperature of 170 ℃ for 20 hours, and cooling and then carrying out centrifugal separation on a reaction kettle bottom product to obtain a sample;
and 3, washing the sample by sequentially adopting deionized water and ethanol to obtain the palladium-doped tin dioxide spherical nano material.
Claims (5)
1. A preparation method of a palladium-doped tin dioxide spherical nano material is characterized by comprising the following steps:
step 1, mixing stannous sulfate, citric acid and polyvinylpyrrolidone, adding the mixture into deionized water, stirring to obtain a mixed solution, adding palladium chloride into the mixed solution, and stirring to obtain a mixed solution;
step 2, placing the mixed solution in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, cooling, and then carrying out centrifugal separation on a reaction kettle bottom product to obtain a sample;
and 3, washing the sample by sequentially adopting deionized water and ethanol to obtain the palladium-doped tin dioxide spherical nano material.
2. The preparation method of the palladium-doped tin dioxide spherical nanomaterial according to claim 1, wherein the ratio of stannous sulfate to citric acid to polyvinylpyrrolidone to palladium chloride is 1:6:2: 0.01-1: 6:2: 0.04.
3. The method for preparing the palladium-doped tin dioxide spherical nanomaterial according to claim 1, wherein the centrifugal separation process in the step 2 is as follows: and (3) rinsing the kettle bottom product by using deionized water, transferring the kettle bottom product to a centrifugal tube, centrifuging for 1min at the rotating speed of 5000r/min, pouring out the upper-layer waste liquid, and obtaining a sample in the centrifugal tube.
4. The method for preparing the palladium-doped tin dioxide spherical nanomaterial according to claim 1, wherein the hydrothermal reaction temperature in the step 2 is 160-180 ℃.
5. The method for preparing the palladium-doped tin dioxide spherical nanomaterial according to claim 1, wherein the hydrothermal reaction time in the step 2 is 15-20 h.
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| CN202010698432.XA CN111921525A (en) | 2020-07-20 | 2020-07-20 | Preparation method of palladium-doped tin dioxide spherical nano material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116510719A (en) * | 2023-04-16 | 2023-08-01 | 大连理工大学 | Core-shell material ZnO/SnO 2 Preparation method and application of (C) |
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