CN110773206A - Fe with high catalytic degradation activity 2O 3BiOCl composite photocatalyst and preparation method and application thereof - Google Patents
Fe with high catalytic degradation activity 2O 3BiOCl composite photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 18
- 230000015556 catabolic process Effects 0.000 title claims abstract description 17
- 230000000694 effects Effects 0.000 title claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 9
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 117
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000002135 nanosheet Substances 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 16
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000001179 sorption measurement Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052797 bismuth Inorganic materials 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 238000000634 powder X-ray diffraction Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 8
- 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 5
- 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 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 239000000979 synthetic dye Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000000870 ultraviolet spectroscopy 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
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- 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
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
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- B01J35/40—
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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
- C02F1/00—Treatment of water, waste water, or sewage
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- 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
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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
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- C02F2101/38—Organic compounds containing nitrogen
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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
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Abstract
Fe with high catalytic degradation activity
2O
3A/BiOCl composite photocatalyst, a preparation method and an application thereof belong to the technical field of nano material photocatalysis. Aiming at the problems of complex preparation process, high cost and the like of the existing catalyst for degrading dye, the invention takes bismuth nitrate as a bismuth source and ferric chloride as a chlorine source and an iron source, and prepares Fe in one step under hydrothermal condition
2O
3/BiOCl nano composite photocatalyst, Fe in the catalyst
2O
3The molar ratio of the BiOCl to the BiOCl is 1-3: 1; fe
2O
3Is of a nanoparticle structure, BiOCl is of a square nanosheet structure, Fe
2O
3The nanoparticles are loaded on the BiOCl nanosheets. Compared with pure phase BiOCl, the Fe prepared by the invention
2O
3The BiOCl composite photocatalyst has higher catalytic activity, the preparation method is simple, the reaction time is short, and a surfactant is not required to be added.
Description
Technical Field
The invention belongs to the technical field of nano material photocatalysis, and particularly relates to Fe with high catalytic degradation activity
2O
3/BiOCl composite photocatalyst and preparation method and application thereof.
Background
Currently, water and soil environmental pollution is more concerned than ever before. Especially in the textile industry, the release of toxic organic dyes has become a serious environmental problem. Because the chemical structure of the synthetic dye is highly stable, the synthetic dye can not be degraded by adopting the traditional treatment methods such as adsorption, chemical coagulation, extraction, membrane separation and the like. Therefore, the wastewater discharged from the textile industry cannot meet more stringent international environmental standards. In recent years, a photocatalytic technology has attracted much attention as a green technology for efficiently decomposing organic dyes using solar energy. However, it remains a significant challenge to develop a low-cost, high-efficiency, practical photocatalyst.
In recent years, BiOCl has been widely studied as an efficient and inexpensive photocatalyst in the degradation of organic pollutants. The layered structure of BiOCl is beneficial to the separation of photoelectrons and holes, and has higher activity. BiOCl, however, absorbs only UV light due to its wide band gap (3.19-3.60 eV). Up to now, the photocatalytic activity has been improved by complexing BiOCl with other semiconductors, such as BiOI/BiOCl, Ag/AgCl/BiOCl, BiOCl/Ag
3PO
4And the like. However, BiOI, Ag, AgCl and Ag were used
3PO
4The modified BiOCl heterojunction is expensive, and practical application of the modified BiOCl heterojunction is limited. Furthermore, some of the preparation methods of these heterojunctions are cumbersome, e.g. requiring toxic solvents, expensive surfactants or finely controlled pH values.
In conclusion, although the BiOCl-based nano composite material has higher degradation activity, the industrial application of the BiOCl-based nano composite material is limited due to the reasons of complex preparation, high cost and the like. Therefore, there is a need for a simple, economical, and environmentally friendly method for preparing BiOCl-based heterojunctions.
Disclosure of Invention
Aiming at the problems of complex preparation process, high cost and the like of the existing catalyst for degrading dye, the invention provides Fe with high catalytic degradation activity
2O
3/BiOCl composite photocatalyst, said Fe
2O
3Fe in/BiOCl composite photocatalyst
2O
3The molar ratio of BiOCl to BiOCl is 1-3: 1.
Further defined, the Fe
2O
3Is in a nano-particle structure, and the particle size is 10-50 nm; BiOCl is a square nanosheet structure, the side length is 200-600nnm, and the thickness is 10-50 nm; fe
2O
3The nanoparticles are loaded on the BiOCl nanosheets.
The invention also provides the Fe with high catalytic degradation activity
2O
3The preparation method of the/BiOCl composite photocatalyst comprises the following steps: dissolving bismuth nitrate pentahydrate in organic alcohol, stirring until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding an iron trichloride aqueous solution into the organic alcohol, and stirring for 1-2 hours to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining for reaction at the temperature of 140-200 ℃ for 8-24h, and after the reaction is finished, sequentially filtering, washing and drying to obtain Fe
2O
3/BiOCl composite photocatalyst.
Further, the organic alcohol is one or more of methanol, ethanol, propanol, isopropanol and ethylene glycol.
Further defined, the dosage ratio of the bismuth nitrate pentahydrate to the organic alcohol is 1 mmol: 2-8 mL.
Further limiting, the molar ratio of the bismuth nitrate pentahydrate to the ferric trichloride is 1: 2-6.
Further limiting, the volume ratio of the organic alcohol to the ferric trichloride aqueous solution is 1: 1-4.
Further limiting, the washing refers to washing for 3 times by using water and absolute ethyl alcohol respectively; and drying at 40-80 ℃.
The invention also provides the Fe
2O
3Application of the BiOCl composite photocatalyst in degradation of organic dye.
Further limited, the application is to use the Fe
2O
3the/BiOCl composite photocatalyst is dispersed in the dye to be degraded, stirred in the dark for adsorption, and after the adsorption reaches the balance, the dye is degraded under the irradiation of visible light.
Advantageous effects
Selection of Fe in the invention
2O
3As a coupling element with BiOCl, the advantage is that, firstly, Fe
2O
3The nano-silver-doped nano-silver nano-particles are chemical substances with rich reserves, low cost and environmental friendliness, and are widely applied to the fields of magnetism, sensors, biological materials, photocatalysis and the like. Secondly, its band energy is well matched to BiOCl, facilitating the transfer of optical energy charges from one material to another. III is n-type Fe
2O
3And stable hybridization is easily formed between the p-type BiOCl semiconductor, so that separation of photoelectrons and holes is facilitated, and recombination of the photoelectrons and the holes is effectively prevented. Fe synthesized by the invention
2O
3the/BiOCl is used as a photocatalyst and has the following beneficial effects:
(1) firstly proposes a one-step hydrothermal method for preparing Fe
2O
3Compared with the traditional two-step preparation technology, the BiOCl composite photocatalyst has the advantages of simple synthesis process, low cost and easy expanded production.
(2) Fe prepared by the method
2O
3the/BiOCl composite nano material has ultrahigh separation efficiency of photoproduction electrons and holes and excellent performance of visible light catalytic degradation of industrial dyes.
Drawings
FIG. 1 is Fe
2O
3The X-ray powder diffraction test chart of/BiOCl, wherein the abscissa is diffraction angle 2 theta (DEG), and the ordinate is diffraction peak intensity; wherein BiOCl 85-0861 represents BiOCl standard peak, Fe
2O
373-0603 for Fe
2O
3A standard peak;
FIG. 2 is Fe
2O
3A scanning electron micrograph of/BiOCl;
FIG. 3 is Fe
2O
3Degradation performance of/BiOCl on rhodamine BCharacterizing, wherein the abscissa is degradation time (minutes), and the ordinate is the removal rate (%) of the dye rhodamine B;
FIG. 4 is Fe
2O
3The degradation performance of the/BiOCl on methyl orange is characterized, the abscissa represents the degradation time (minutes), and the ordinate represents the removal rate (%) of the dye methyl orange.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific examples, but the present invention is not limited to the examples. Those skilled in the art, having the benefit of this disclosure, may effect numerous modifications thereto without departing from the scope and spirit of the invention as set forth in the claims.
Example 1.Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol of bismuth nitrate pentahydrate in 20mL of ethylene glycol, fully stirring for 1h until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding 20mL of aqueous solution containing 10mmol of ferric chloride, continuously stirring for 1h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 12h at 200 ℃, filtering after the reaction is finished, washing for three times by using water and absolute ethyl alcohol respectively, and drying in an oven at 60 ℃ to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3The molar ratio to BiOCl was 1: 1.
FIG. 1 is Fe
2O
3X-ray powder diffraction test pattern of/BiOCl. From the figure, it can be seen that the prepared solid powder X-ray derived peaks are similar to those of BiOCl standard card JCPDS: 85-0861 and Fe
2O
3Standard card JCPDS: 73-0603 correspond completely to each other, indicating that the obtained solid powder is Fe
2O
3a/BiOCl composite material; FIG. 2 is Fe
2O
3the/BiOCl scanning electron microscope picture shows that the obtained Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 400 nm; thickness of about 25nm, Fe
2O
3The nanoparticle size is about 30 nm.
Example 2.Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol of bismuth nitrate pentahydrate in 10mL of ethylene glycol, fully stirring for 1h until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding 40mL of aqueous solution containing 15mmol of ferric chloride, continuously stirring for 1h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 24h at 140 ℃, filtering after the reaction is finished, washing for three times by using water and absolute ethyl alcohol respectively, and drying in an oven at 80 ℃ to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3Molar ratio to BiOCl 1.5: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; fe
2O
3Fe loaded on BiOCl square nano sheet in shape of BiOCl
2O
3Nanoparticles, BiOCl square nanosheets 300nm in size, about 40nm in thickness, Fe
2O
3The nanoparticle size was 25nm (not shown).
Example 3.Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol bismuth nitrate pentahydrate in 40mL ethanol, stirring for 2h to dissolve completely, dripping 80mL aqueous solution containing 30mmol ferric chloride, stirring for 1h, transferring the mixed solution to a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 8h at 160 ℃, filtering after the reaction is finished, washing with water and absolute ethyl alcohol for three times respectively, and drying in a 40 ℃ oven to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3The molar ratio to BiOCl was 3: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; the resulting Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 300 nm; thickness of about 35nm, Fe
2O
3The nanoparticle size was about 50nm (not shown).
Example 4.Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol bismuth nitrate pentahydrate in 15mL ethanol, stirring for 1.5h to dissolve completely, dripping 45mL aqueous solution containing 20mmol ferric chloride, stirring for 1h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 10h at 170 ℃, filtering after the reaction is finished, washing with water and absolute ethyl alcohol for three times respectively, and drying in a 50 ℃ oven to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3The molar ratio to BiOCl was 2: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; the resulting Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 200 nm; thickness of about 10nm, Fe
2O
3The nanoparticle size was about 10nm (not shown).
Example 5 Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol of bismuth nitrate pentahydrate in 25mL of propanol, fully stirring for 1h until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding 50mL of aqueous solution containing 25mmol of ferric chloride, continuously stirring for 1.5h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 16h at 190 ℃, filtering after the reaction is finished, washing for three times by using water and absolute ethyl alcohol respectively, and drying in a 70 ℃ oven to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3Molar ratio to BiOCl 2.5: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; the resulting Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 600 nm; thickness of about 40nm, Fe
2O
3The nanoparticle size was about 20nm (not shown).
Example 6.Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol of bismuth nitrate pentahydrate in 20mL of isopropanol, fully stirring for 2h until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding 30mL of aqueous solution containing 10mmol of ferric chloride, continuously stirring for 2h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 14h at 150 ℃, filtering after the reaction is finished, washing for three times by using water and absolute ethyl alcohol respectively, and drying in an oven at 60 ℃ to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3The molar ratio to BiOCl was 1: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; the resulting Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 550 nm; thickness of about 20nm, Fe
2O
3The nanoparticle size was about 25nm (not shown).
Example 7.Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol of bismuth nitrate pentahydrate in 35mL of methanol, fully stirring for 1h until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding 70mL of aqueous solution containing 15mmol of ferric chloride, continuously stirring for 2h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 20h at 180 ℃, filtering after the reaction is finished, washing for three times by using water and absolute ethyl alcohol respectively, and drying in a 50 ℃ oven to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3Molar ratio to BiOCl 1.5: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; the resulting Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 350 nm; thickness of about 50nm, Fe
2O
3The size of the nanoparticles is about15nm (not shown).
Example 8 Fe
2O
3Preparation of a BiOCl composite photocatalyst.
Dissolving 5mmol bismuth nitrate pentahydrate in 40mL ethylene glycol, stirring for 1.5h to dissolve completely, dripping 160mL aqueous solution containing 20mmol ferric chloride, stirring for 1h, transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 9h at 200 ℃, filtering after the reaction is finished, washing with water and absolute ethyl alcohol for three times respectively, and drying in an oven at 60 ℃ to obtain Fe
2O
3/BiOCl composite photocatalyst, Fe
2O
3The molar ratio to BiOCl was 2: 1.
the X-ray powder diffraction pattern was similar to that of example 1, indicating that the obtained solid powder was Fe
2O
3a/BiOCl composite material; the resulting Fe
2O
3The shape of/BiOCl is that Fe is loaded on a BiOCl square nano-sheet
2O
3The side length of the BiOCl square nanosheet is 400 nm; thickness of about 40nm, Fe
2O
3The nanoparticle size was about 50nm (not shown).
Application example 1: taking Fe prepared in example 1
2O
350mg of/BiOCl is dispersed in 100mL of 10mg/L rhodamine B solution, the mixture is stirred for 40 minutes under the dark condition, a 300W xenon lamp is started to irradiate after the adsorption reaches the balance, an optical filter is used for filtering ultraviolet light below 420nm in a light source, and an ultraviolet-visible spectrophotometer is used for detecting the concentration of the rhodamine B in the solution every 15 minutes. Through detection, the Fe prepared by the invention
2O
3The degradation rate of rhodamine B in 60 minutes under visible light by/BiOCl can reach more than 98 percent as shown in figure 3.
Application example 2: taking Fe prepared in example 1
2O
350mg of/BiOCl is dispersed in 100mL of 10mg/L methyl orange solution, stirred for 40 minutes under the dark condition, a 300W xenon lamp is turned on to radiate after the adsorption reaches the balance, an optical filter is used for filtering ultraviolet light below 420nm in a light source, and an ultraviolet-visible spectrophotometer is used for detecting the concentration of the methyl orange in the solution every 15 minutes. Through detection, the Fe prepared by the invention
2O
3/BiOCl inUnder the light, the degradation rate of methyl orange in 90 minutes can reach more than 99 percent, as shown in figure 4.
Claims (10)
1.Fe with high catalytic degradation activity
2O
3the/BiOCl composite photocatalyst is characterized in that Fe
2O
3Fe in/BiOCl composite photocatalyst
2O
3The molar ratio of BiOCl to BiOCl is 1-3: 1.
2.Fe of claim 1
2O
3the/BiOCl composite photocatalyst is characterized in that Fe
2O
3Is in a nano-particle structure, and the particle size is 10-50 nm; BiOCl is a square nanosheet structure, the side length is 200-600nm, and the thickness is 10-50 nm; fe
2O
3The nanoparticles are loaded on the BiOCl nanosheets.
3.Fe as claimed in claim 1 or 2
2O
3The preparation method of the/BiOCl composite photocatalyst is characterized by comprising the following steps: dissolving bismuth nitrate pentahydrate in organic alcohol, stirring until the bismuth nitrate pentahydrate is completely dissolved, dropwise adding an iron trichloride aqueous solution into the organic alcohol, and stirring for 1-2 hours to obtain a mixed solution; then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, reacting for 8-24h at 140-200 ℃, and after the reaction is finished, sequentially filtering, washing and drying to obtain Fe
2O
3/BiOCl composite photocatalyst.
4. The method according to claim 3, wherein the organic alcohol is a mixture of one or more of methanol, ethanol, propanol, isopropanol and ethylene glycol.
5. The method according to claim 3, wherein the ratio of the bismuth nitrate pentahydrate to the organic alcohol is 1 mmol: 2-8 mL.
6. The preparation method according to claim 3, wherein the molar ratio of the bismuth nitrate pentahydrate to the ferric trichloride is 1: 2-6.
7. The method according to claim 3, wherein the volume ratio of the organic alcohol to the aqueous solution of ferric trichloride is 1: 1-4.
8. The method according to claim 3, wherein the washing is washing with water and absolute ethanol for 3 times; and drying at 40-80 ℃.
9. Fe as claimed in claim 1 or 2
2O
3Application of the BiOCl composite photocatalyst in degradation of organic dye.
10. Use according to claim 9, characterized in that it is Fe according to claim 1 or 2
2O
3the/BiOCl composite photocatalyst is dispersed in the dye to be degraded, stirred in the dark for adsorption, and after the adsorption reaches the balance, the dye is degraded under the irradiation of visible light.
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