CN108355684B - Nanorod-shaped BiOI photocatalyst and preparation method thereof - Google Patents
Nanorod-shaped BiOI photocatalyst and preparation method thereof Download PDFInfo
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- CN108355684B CN108355684B CN201810177484.5A CN201810177484A CN108355684B CN 108355684 B CN108355684 B CN 108355684B CN 201810177484 A CN201810177484 A CN 201810177484A CN 108355684 B CN108355684 B CN 108355684B
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- oleic acid
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 18
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 18
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005642 Oleic acid Substances 0.000 claims abstract description 18
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 10
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000000593 degrading effect Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
-
- 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 preparation method of a nanorod-shaped BiOI photocatalyst, which comprises the following steps: adding Bi (NO)3)3Completely dissolving in oleic acid, adding KI, stirring for 7-13 days, adding water, hydrolyzing to generate BiOI, centrifuging, taking precipitate, washing and drying to obtain the nano rod-shaped BiOI photocatalyst; the Bi (NO)3)3: oleic acid: KI: water (1.0 to 2.0) g: (35-65) mL: (0.35-0.65) g: (7-13) mL, wherein Bi (NO)3)3And KI by weight, oleic acid and water by volume. The invention uses Bi (NO)3)3And KI as a raw material, fully stirring in oleic acid, and hydrolyzing at normal temperature and normal pressure to prepare the nano-rod-shaped BiOI photocatalyst. The preparation method has the advantages of high operation safety, low energy consumption, simple requirements on reaction equipment, low preparation cost and capability of observing the reaction process at any time; the nano-rod-shaped BiOI photocatalyst prepared by the preparation method has high surface area and excellent catalytic performance.
Description
Technical Field
The invention relates to a photocatalyst, in particular to a nanorod-shaped BiOI photocatalyst and a preparation method thereof.
Background
Today, environmental pollution and energy shortage are two major challenges facing human sustainable development. The semiconductor photocatalyst can store and convert cheap, clean and renewable solar energy, and is widely applied to hydrogen production by photolysis of water and CO photo-reduction2Production of renewable Fuel (CH)3OH、CH4And CO) and photolysis of organic pollutants.
In recent years, bismuth oxyhalide (BiOX, X ═ Cl, Br, I) photocatalysts have been developed because of their high photocatalytic activityPeople have a wide attention. Which consists of two X－Ion layer and Bi2O2The layered structure formed by the alternate arrangement of the layers can generate an internal electric field, which is beneficial to the effective separation of photo-generated electron-hole pairs, separated electrons and holes can be compounded only by some gaps of the structure, the recombination rate is greatly reduced, and the photocatalytic activity is higher. The BiOX of the laminated structure can provide enough large space polarization related atoms and orbitals; the induced dipole can effectively separate electron hole pairs and improve the photocatalytic activity. The layered tetragonal lead fluorochloride ore type BiOX compound has good optical, electrical and magnetic properties, and has been widely used in catalysis, ion conductors, photochromic devices, ferroelectric materials, dyes and solar cells. BiOX is a promising photocatalyst because it has good photocatalytic activity under both ultraviolet and visible light irradiation.
At present, there are many reports on different methods for preparing pure BiOX samples to improve photocatalytic activity, but there is still a need to further improve photocatalytic efficiency thereof for practical use. Until now, although a variety of different BiOI layered nanostructures have been synthesized and applied to photocatalytic processes under UV or UV-visible radiation, it has been a challenge to synthesize BiOI layered nanostructures with controllable morphology and high photocatalytic activity of visible light by a simple and efficient method. In the prior art, a hydrothermal reaction is generally required when the nano BiOI photocatalyst is prepared. The hydrothermal reaction is a high-temperature reaction, so that the method has the disadvantages of high danger, high energy consumption and high preparation cost, and is difficult to realize large-scale industrial production. And the theoretical simulation and analysis of the BiOX prepared by the hydrothermal method are difficult, the reproducibility is poor, the requirements on reaction equipment are high, the BiOX is difficult to observe from time to time, and the parameter adjustment is difficult.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a nanorod-like BiOI photocatalyst and a preparation method thereof.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows: a preparation method of a nano-rod-shaped BiOI photocatalyst comprises the following steps: adding Bi (NO)3)3Completely dissolving in oleic acid, adding KI, stirring for 7-13 days, adding water, hydrolyzing to generate BiOI, centrifuging, taking precipitate, washing and drying to obtain the nano rod-shaped BiOI photocatalyst; the Bi (NO)3)3: oleic acid: KI: water (1.0 to 2.0) g: (35-65) mL: (0.35-0.65) g: (7-13) mL, wherein Bi (NO)3)3And KI by weight, oleic acid and water by volume.
Preferably, the washing is performed for 3-5 times by using ethanol and n-hexane respectively.
Preferably, the drying temperature is 60 ℃, and the drying time is 10-15 h.
Preferably, the Bi (NO)3)3: oleic acid: KI: water ═ 1.5 g: 50mL of: 0.5 g: 10mL of a solution of Bi (NO)3)3And KI by weight, oleic acid and water by volume.
The invention also provides a nano-rod-shaped BiOI photocatalyst, which is prepared by the preparation method of the nano-rod-shaped BiOI photocatalyst.
Compared with the prior art, the invention has the beneficial effects that: the invention uses Bi (NO)3)3And KI as a raw material, fully stirring in oleic acid, and hydrolyzing at normal temperature and normal pressure to prepare the nano-rod-shaped BiOI photocatalyst. The preparation method has the advantages of high operation safety, low energy consumption, simple requirements on reaction equipment, low preparation cost and capability of observing the reaction process at any time; the nano-rod-shaped BiOI photocatalyst prepared by the preparation method has high surface area and excellent catalytic performance.
Drawings
FIG. 1 is a scanning electron micrograph of a nanorod-shaped BiOI photocatalyst according to example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a nanorod-shaped BiOI photocatalyst according to example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of a nanorod-shaped BiOI photocatalyst according to example 1 of the present invention;
fig. 4 is a graph of the catalytic activity of the nanorod-shaped BiOI photocatalyst of example 1 of the present invention in degrading methyl orange under visible light.
Detailed Description
Example 1
This example 1 provides a method for preparing a nanorod-shaped BiOI photocatalyst, which includes the following steps: 1.5gBi (NO)3)3Dissolving in 50mL of oleic acid, adding 0.5g of KI after complete dissolution, stirring for 10 days, then adding 10mL of water, hydrolyzing to generate BiOI, centrifuging, taking the precipitate, sequentially washing with ethanol and n-hexane for 3 times respectively, and then drying in an oven at 60 ℃ for 12 hours to obtain the nano rod-shaped BiOI photocatalyst.
Example 2
This example 2 provides a method for preparing a nanorod-shaped BiOI photocatalyst, including the following steps: 1.0gBi (NO)3)3Dissolving in 35mL of oleic acid, adding 0.35g of KI after complete dissolution, stirring for 7 days, then adding 7mL of water, hydrolyzing to generate BiOI, centrifuging, taking precipitate, sequentially washing with ethanol and n-hexane for 3 times respectively, and drying in an oven at 60 ℃ for 10 hours to obtain the nano rod-shaped BiOI photocatalyst.
Example 3
This embodiment 3 provides a method for preparing a nanorod-shaped BiOI photocatalyst, which includes the following steps: 2.0gBi (NO)3)3Dissolving the mixture in 65mL of oleic acid, adding 0.65g of KI after complete dissolution, stirring for 13 days, then adding 13mL of water, hydrolyzing to generate BiOI, centrifuging, taking precipitate, sequentially washing with ethanol and n-hexane for 5 times respectively, and then drying in an oven at 60 ℃ for 15 hours to obtain the nano rod-shaped BiOI photocatalyst.
The performance of the nanorod-shaped BiOI photocatalyst prepared in the example was tested:
1. surface topography
Fig. 1 to 3 are scanning electron micrographs of the nanorod-shaped BiOI photocatalyst of example 1 at different magnification, and it can be seen from fig. 1 to 3 that the nanorod-shaped BiOI photocatalyst of example 1 has a rod-shaped appearance, a high surface area, and good dispersibility.
2. Photocatalytic activity
The catalytic activity of the nanorod-shaped BiOI photocatalyst of examples 1-3 in degrading methyl orange under visible light was tested. The results show that the nanorod-shaped BiOI photocatalysts of examples 1-3 all have better catalytic performance than the nanosheet-shaped BiOI photocatalyst.
Wherein, fig. 4 is a graph of the catalytic activity of the nanorod-shaped BiOI photocatalyst of example 1 in degrading methyl orange under visible light, and it can be seen from fig. 4 that the nanorod-shaped BiOI photocatalyst of the present invention has good catalytic activity.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (5)
1. A preparation method of a nano-rod-shaped BiOI photocatalyst is characterized by comprising the following steps: adding Bi (NO)3)3Completely dissolving in oleic acid, adding KI, stirring for 7-13 days, adding water, hydrolyzing to generate BiOI, centrifuging, taking precipitate, washing and drying to obtain the nano rod-shaped BiOI photocatalyst; the Bi (NO)3)3: oleic acid: KI: water (1.0 to 2.0) g: (35-65) mL: (0.35-0.65) g: (7-13) mL, wherein Bi (NO)3)3And KI by weight, oleic acid and water by volume.
2. The method for preparing the nanorod-shaped BiOI photocatalyst of claim 1, wherein the washing is performed 3-5 times by using ethanol and n-hexane respectively.
3. The method for preparing the nanorod-shaped BiOI photocatalyst according to claim 1, wherein the drying temperature is 60 ℃ and the drying time is 10-15 hours.
4. The method of preparing the nanorod-shaped BiOI photocatalyst as in any one of claims 1 to 3, wherein the Bi (NO) is3)3: oleic acid: KI: water ═ water1.5 g: 50mL of: 0.5 g: 10mL of a solution of Bi (NO)3)3And KI by weight, oleic acid and water by volume.
5. A nanorod-shaped BiOI photocatalyst is prepared by the preparation method of any one of claims 1 to 4.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112895A (en) * | 2013-02-22 | 2013-05-22 | 厦门大学 | Method for preparing ring-shaped bismuth oxyiodide (BiOI) microspheres |
| CN104368362A (en) * | 2014-09-18 | 2015-02-25 | 太原理工大学 | Microemulsion-like photocatalyst, preparation method and applications thereof |
| CN104475132A (en) * | 2014-11-26 | 2015-04-01 | 安徽工业大学 | Preparation method of flower-like BiOBr and application of flower-like BiOBr in rhodamine degradation reaction |
| CN105562040A (en) * | 2016-01-11 | 2016-05-11 | 安徽工业大学 | Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst |
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2018
- 2018-03-02 CN CN201810177484.5A patent/CN108355684B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112895A (en) * | 2013-02-22 | 2013-05-22 | 厦门大学 | Method for preparing ring-shaped bismuth oxyiodide (BiOI) microspheres |
| CN104368362A (en) * | 2014-09-18 | 2015-02-25 | 太原理工大学 | Microemulsion-like photocatalyst, preparation method and applications thereof |
| CN104475132A (en) * | 2014-11-26 | 2015-04-01 | 安徽工业大学 | Preparation method of flower-like BiOBr and application of flower-like BiOBr in rhodamine degradation reaction |
| CN105562040A (en) * | 2016-01-11 | 2016-05-11 | 安徽工业大学 | Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| BiOI光催化剂的稳定性及BiOBr (Cl)的性能强化研究;朵芳芳;《中国优秀博士学位论文全文数据库 工程科技I辑》;20160715(第7期);摘要、第35页第3.2.1部分 * |
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