CN102744087B - Electrochemistry preparation method for flaky nanometer bismuth oxychloride film photocatalyst - Google Patents
Electrochemistry preparation method for flaky nanometer bismuth oxychloride film photocatalyst Download PDFInfo
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Abstract
The invention relates to an electrochemistry preparation method for a flaky nanometer bismuth oxychloride film photocatalyst, and belongs to the technical field of environmental chemical engineering photocatalysis water treatment. The method is characterized by: adopting a Ti substrate as a cathode, adopting a platinum wire electrode as an anode, adopting a Bi(NO3)3.5H2O as an electrolyte solution, and adopting a constant current deposition method to prepare a film A at the cathode; adopting the film A as an anode, adopting a graphite electrode as a cathode, adopting a NaCl solution as an electrolyte solution, and adopting a constant potential oxidation method to prepare a BiOCl film at the anode; and washing with distilled water, and carrying out natural open-air drying. The resulting BiOCl film has characteristics of uniform crystal phase structure, uniform distribution, and flaky nanometer structure. The preparation method of the present invention has the following characteristics that: a process is simple and environmental protection, conditions are mild, an operating period is short, and the prepared film has characteristics of uniform distribution, no toxicity, harmlessness and good photocatalytic activity, and is suitable for photocatalytic degradation of organic pollutants in water or air.
Description
Technical field
The electrochemical preparation method of a kind of flake nano bismoclite of the present invention film photocatalyst, belongs to environmental chemical engineering photocatalysis technology field, is specifically related to a kind of electrochemical preparation method of flake nano BiOCl film photocatalytic material and the technical scheme of application.
Background technology
Bismoclite (BiOCl) is a kind of indirect band-gap semiconductor, by [Bi
2o
2] layer and free Cl atomic building, thering is the highly layer structure of anisotropic, these two obvious advantages are convenient to the separation in light induced electron-hole, have guaranteed the good stable photocatalytic activity (chemical progress, 2009,21:1734 – 1741) of BiOCl.Therefore,, as a kind of catalysis material that has vast potential for future development in organic pollution process field, BiOCl is subject to showing great attention to of researchers.Many researchers have reported the (X=Cl to BiOX; Br; I) preparation of serial powder photocatalyst, sign and photocatalytic activity research work; by hydrolysis or solvent-thermal method, made BiOX powder; there is the BiOX series powder of Nano microsphere shape microscopic appearance by wide coverage (Rare Metals; 2008,27:243 – 250; Journal of Catalysis, 2009,262:144 – 149; Catalysis Communications, 2011,12:1136 – 1141; Journal of Hazardous Materials, 2011,192:538 – 544; Colloids and Surfaces A:Physicochem.Eng.Aspects, 2011,387:23 – 28).Modification work to BiOX powder catalyst is also day by day in the news.In order to improve the extinction property of BiOCl, make its optical absorption band red shift, the Pare of India etc. have made the BiOCl powder of Mn doping by Hydrolyze method, by sign, learn, mixing of Mn not only makes the band gap of BiOCl be down to 2.74eV by 3.48eV, also make the particle diameter of BiOCl reduce (Applied Surface Science, 2011,258:247 – 253).Zhu etc. have reported the sterilization process of Ag/BiOI to E.coli8099, have made the BiOI (Separation and Purification Technology, 2011) of Ag doping by the hot method of ethylene glycol solvent.In addition, Fe
3o
4, WO
3report (Applied Catalysis B:Environmental, 2009,90:458 – 462 with the composite modified BiOCl powder catalyst such as BOH also studied persons; Applied Catalysis A:General 2011; Catalysis Communications, 2011,16:229 – 233; Journal of Colloid and Interface Science, 2011,356:465 – 472).The advantages such as it is large that powder photocatalyst has specific area, and catalytic activity is good, but aspect practical application, there is intrinsic inferior position, as bad dispersibility, Separation of Solid and Liquid problem and recycling problem etc.Therefore, the research to photocatalyst fixation technology, is having obvious value aspect the actual application problem of solution photocatalysis technology.In existing report, about the immobilization problem of BiOX series photochemical catalyst, be not subject to researchers' common concern, only have report few in number.Cao Sihai etc. provide and have adopted physical vapour deposition (PVD) and chemical oxidization method to prepare the method (CN101724839A of BiOCl film; Nanotechnology; 2009; 20:275702); the film making has flower ball-shaped structure; but in preparation process, need by complicated processes of physical vapor deposition, need special instrument and equipment and high-purity gas as protection gas, the cost of preparing film is higher; operating process is complicated, is unfavorable for suitability for industrialized production.Wu Sujuan etc. have adopted template synthesis BiOCl nano-wire array, and investigated its under UV-irradiation to the degrading activity of rhodamine B (Materials Letters, 2010,64:115 – 118), but the method needs alumina formwork, in preparation process, need higher baking temperature and longer drying time.The employing continuous ionic layer adsorption reaction legal systems such as Zhang Li knows obtain BiOI membrane electrode, and pointed out the application potential (CN101857382A) of membrane electrode in area of solar cell, method is simple, without special reactor and instrument, but need to be through repeatedly just making required film, operating process is comparatively loaded down with trivial details.Existing BiOX process for fixation or physics preparation process that need to be complicated, need to prepare template, or manufacturing cycle is longer, therefore, find out that a kind of reaction condition is gentle, simple and to prepare crystal phase structure unified, the method for the BiOCl film being evenly distributed is necessary.Electrochemical reaction mild condition, without HTHP and special instrument and equipment, cathodic electrodeposition and anodizing at the film photocatalytic material of other kinds (as TiO
2film etc.) in preparation, repeatedly adopted, but also do not find so far to adopt electrochemical method to prepare the report of BiOCl film.
Summary of the invention
The object of the electrochemical preparation method of a kind of flake nano bismoclite of the present invention film photocatalyst is to provide a kind of process for fixation of BiOCl photochemical catalyst, by electrochemical method, prepare a kind of flake nano BiOCl film photocatalytic material, and be applied in the processing of organic pollutant in water.The method is by cathode electrodeposition and two steps of anodic oxidation, on Ti matrix, make BiOCl film, through washing, naturally drying after operation, under room temperature normal pressure, prepared flake nano BiOCl film, the simple process for fixation of molecule catalyst is provided.Raw materials usedly commonly be easy to get, reaction condition is room temperature normal pressure, simple to operate, the cycle is short, be easy to realize suitability for industrialized production.Made BiOCl film has good Photocatalytic activity to methyl orange under ultraviolet light, and film performance is stable, can be recycled.
The electrochemical preparation method of a kind of flake nano bismoclite of the present invention film photocatalytic material, the simple process for fixation that it is characterized in that a kind of molecule catalyst, specifically be a kind of by cathode electrodeposition and two steps of anodic oxidation, on Ti matrix, make BiOCl film, through washing and naturally drying after operation, under room temperature normal pressure, prepare the method for flake nano BiOCl film, its processing step is as follows:
I, cathodic electrodeposition process
Take 1～10 gram and analyze pure Bi (NO
3)
35H
2o is positioned in 50～150mL small beaker, adds 40～140mL distilled water, under magnetic agitation, splashes into dense HCl regulation system pH value to forming settled solution; The oxalic acid solution that employing is 20% through mass fraction titanium sheet matrix after acid etching at 90 ℃ is negative electrode, and platinum electrode is anode, and it is electrolyte that solution is joined by institute, with 2～5mAcm
-2for current density galvanostatic deposition 3～10h, form film A;
II, anode oxidation process
Take 1～10 gram of pure NaCl of analysis and be positioned in 50～150mL small beaker, add 40～140mL distilled water, stir and make its dissolving; The prepared film A of the I of take is anode, graphite is negative electrode, it is electrolyte that NaCl solution is joined by institute, at 1～3V constant voltage oxidation, 30～120min, form BiOCl film, after being taken out, cleans with distilled water the BiOCl film making, naturally after drying, make required flake nano BiOCl film, this film consists of Tetragonal BiOCl, there is staggered laminated structure (as shown in Figure 1 and Figure 2), film has good absorption to ultraviolet light, learns that as calculated the band gap of made BiOCl film is about 3.42eV (as shown in Figure 3);
Said method adopts the BiOCl film photocatalytic material make to can be applicable in water in organic Treatment by Photocatalysis Oxidation, particularly in water, trace toxic is harmful in the processing of hardly degraded organic substance, light source used is wavelength 365nm ultraviolet light, reaction condition is: normal temperature and pressure, made BiOCl film photocatalytic material is positioned in aqueous organopolysiloxane over against light source, from reactor bottom, blasts air.
The advantage of the electrochemical preparation method of a kind of flake nano bismoclite of the present invention film photocatalytic material is:
1) adopt first electrochemical method to make BiOCl film photocatalyst;
2) reaction condition is gentle, and whole preparation process can complete under room temperature normal pressure, and electrochemical deposition and oxidation complete under low current density and low-voltage, the flake nano BiOCl film photocatalytic material that adopts simple method to make to be evenly distributed;
3) realize the immobilization of nano-sheet BiOCl, facilitated recycling of Separation of Solid and Liquid and catalyst, and the degraded that had both conveniently been applied to organic pollution in water or in air;
4) made BiOCl film photocatalytic material is evenly distributed, and crystal lattice orientation is obvious, and specific area is larger;
5) made BiOCl film photocatalytic material has good and stable photocatalytic activity under ultraviolet light, and has the longer life-span;
6) made BiOCl film photocatalytic material is conveniently realized additional small electrical field control, thereby can realize the method degradable organic pollutant that adopts photoelectrocatalysis.
Accompanying drawing explanation
Fig. 1 is the SEM picture of the flake nano bismoclite film photocatalytic material of embodiment of the present invention 1 preparation.
Fig. 2 is the XRD spectra of the flake nano bismoclite film photocatalytic material of embodiment of the present invention 1 preparation.
Fig. 3 is the UV-Vis DRS collection of illustrative plates of the flake nano bismoclite film photocatalytic material of embodiment of the present invention 1 preparation.
The specific embodiment
In order to make technical scheme of the present invention clearer, will specifically describe in detail with embodiment below, but content of the present invention is not confined to the scope of cited embodiment.
Embodiment 1
1) cathodic electrodeposition process
Take 3 grams and analyze pure Bi (NO
3)
35H
2o is positioned in 100mL small beaker, adds 90mL distilled water, under magnetic agitation, splashes into dense HCl regulation system pH value to forming settled solution; The oxalic acid solution that employing is 20% through mass fraction titanium sheet matrix after acid etching at 90 ℃ is negative electrode, and platinum filament is anode, and it is electrolyte that solution is joined by institute, with 3mAcm
-2for current density galvanostatic deposition 6h, form film 1;
2) anode oxidation process
Take 3 grams of pure NaCl of analysis and be positioned in 100mL small beaker, add 100mL distilled water, stir and make its dissolving; Take film 1 as anode, and graphite is negative electrode, and it is electrolyte that NaCl solution is joined by institute, at 2.0V constant voltage oxidation 60min, forms BiOCl film, after taking-up, with distilled water, cleans, and makes flake nano BiOCl film photocatalytic material after naturally drying;
Institute's made membrane is used for to photocatalytic degradation water methyl orange, reaction condition is: normal temperature and pressure, the methyl orange aqueous solution 50mL of 10mg/L, get the made membrane 1cm * 6cm of institute as photochemical catalyst, from reactor bottom, blast air, at interval of certain hour sample analysis, with UV-VIS spectrophotometry, measure the conversion ratio of methyl orange.Under ultraviolet light, as shown in table 1 to the degradation results of methyl orange in 150min:
| Time (min) | 0 | 15 | 30 | 45 | 60 | 75 | 90 | 105 | 120 | 135 | 150 |
| Degradation rate (%) | 0 | 21.8 | 36.6 | 56.4 | 67.3 | 76.2 | 84.1 | 90.1 | 93.1 | 96.0 | 98.0 |
1) cathodic electrodeposition process
Take 2 grams and analyze pure Bi (NO
3)
35H
2o is positioned in 100mL small beaker, adds 90mL distilled water, under magnetic agitation, splashes into dense HCl regulation system pH value to forming settled solution; The oxalic acid solution that employing is 20% through mass fraction titanium sheet matrix after acid etching at 90 ℃ is negative electrode, and platinum filament is anode, and it is electrolyte that solution is joined by institute, with 4mAcm
-2for current density galvanostatic deposition 3h, form film 1;
2) anode oxidation process
Take 1 gram of pure NaCl of analysis and be positioned in 100mL small beaker, add 100mL distilled water, stir and make its dissolving; Take film 1 as anode, and graphite is negative electrode, and it is electrolyte that NaCl solution is joined by institute, at 1.5V constant voltage oxidation 120min, form BiOCl film, after the BiOCl film making is taken out, with distilled water, clean, after naturally drying, make flake nano BiOCl film photocatalytic material;
Institute's made membrane is used for to photocatalytic degradation water methyl orange, reaction condition is: normal temperature and pressure, the methyl orange aqueous solution 50mL of 10mg/L, get the made membrane 1cm * 6cm of institute as photochemical catalyst, from reactor bottom, blast air, at interval of certain hour sample analysis, with UV-VIS spectrophotometry, measure the conversion ratio of methyl orange.Under ultraviolet light, as shown in table 2 to the degradation results of methyl orange in 150min:
| Time (min) | 0 | 15 | 30 | 45 | 60 | 75 | 90 | 105 | 120 | 135 | 150 |
| Degradation rate (%) | 0 | 15.5 | 25.6 | 33.4 | 40.3 | 47.2 | 52.1 | 54.1 | 56.1 | 57.0 | 58.0 |
Embodiment 3
1) cathodic electrodeposition process
Take 5 grams and analyze pure Bi (NO
3)
35H
2o is positioned in 100mL small beaker, adds 90mL distilled water, under magnetic agitation, splashes into dense HCl regulation system pH value to forming settled solution; The oxalic acid solution that employing is 20% through mass fraction titanium sheet matrix after acid etching at 90 ℃ is negative electrode, and platinum filament is anode, and it is electrolyte that solution is joined by institute, with 5mAcm
-2for current density galvanostatic deposition 8h, form film 1;
2) anode oxidation process
Take 1 gram of pure NaCl of analysis and be positioned in 100mL small beaker, add 100mL distilled water, stir and make its dissolving; Take film 1 as anode, and graphite is negative electrode, and it is electrolyte that NaCl solution is joined by institute, at 1.0V constant voltage oxidation 90min, form BiOCl film, after the BiOCl film making is taken out, with distilled water, clean, after naturally drying, make flake nano BiOCl film photocatalytic material;
Institute's made membrane is used for to photocatalytic degradation water methyl orange, reaction condition is: normal temperature and pressure, the methyl orange aqueous solution 50mL of 10mg/L, get the made membrane 1cm * 6cm of institute as photochemical catalyst, from reactor bottom, blast air, at interval of certain hour sample analysis, with UV-VIS spectrophotometry, measure the conversion ratio of methyl orange.Under ultraviolet light, as shown in table 3 to the degradation results of methyl orange in 150min:
| Time (min) | 0 | 15 | 30 | 45 | 60 | 75 | 90 | 105 | 120 | 135 | 150 |
| Degradation rate (%) | 0 | 37 | 45 | 57 | 69 | 77 | 82 | 86 | 89 | 89 | 89 |
Embodiment 4
1) cathodic electrodeposition process
Take 10 grams and analyze pure Bi (NO
3)
35H
2o is positioned in 100mL small beaker, adds 90mL distilled water, under magnetic agitation, splashes into dense HCl regulation system pH value to forming settled solution; The oxalic acid solution that employing is 20% through mass fraction titanium sheet matrix after acid etching at 90 ℃ is negative electrode, and platinum filament is anode, and it is electrolyte that solution is joined by institute, with 1mAcm
-2for current density galvanostatic deposition 10h, form film 1;
2) anode oxidation process
Take 6 grams of pure NaCl of analysis and be positioned in 100mL small beaker, add 100mL distilled water, stir and make its dissolving; Take film 1 as anode, and graphite is negative electrode, and it is electrolyte that NaCl solution is joined by institute, at 2.0V constant voltage oxidation 30min, form BiOCl film, after the BiOCl film making is taken out, with distilled water, clean, after naturally drying, make flake nano BiOCl film photocatalytic material;
Institute's made membrane is used for to photocatalytic degradation water methyl orange, reaction condition is: normal temperature and pressure, the methyl orange aqueous solution 50mL of 10mg/L, get the made membrane 1cm * 6cm of institute as photochemical catalyst, from reactor bottom, blast air, at interval of certain hour sample analysis, with UV-VIS spectrophotometry, measure the conversion ratio of methyl orange.Under ultraviolet light, as shown in table 4 to the degradation results of methyl orange in 150min:
| Time (min) | 0 | 15 | 30 | 45 | 60 | 75 | 90 | 105 | 120 | 135 | 150 |
| Degradation rate (%) | 0 | 27.2 | 42.6 | 53.4 | 62.4 | 69.3 | 74.2 | 79.2 | 83.2 | 87.1 | 90.0 |
Claims (2)
1. the electrochemical preparation method of a flake nano bismoclite film photocatalytic material, the simple process for fixation that it is characterized in that a kind of molecule catalyst, specifically be a kind of by cathode electrodeposition and two steps of anodic oxidation, on Ti matrix, make BiOCl film, through washing and naturally drying after operation, under room temperature normal pressure, prepare the method for flake nano BiOCl film, its processing step is as follows:
Take 1 ~ 10 gram and analyze pure Bi (NO
3)
35H
2o is positioned in 50 ~ 150 mL small beakers, adds 40 ~ 140 mL distilled water, under magnetic agitation, splashes into dense HCl regulation system pH value to forming settled solution; The oxalic acid solution that employing is 20% through mass fraction titanium sheet matrix after acid etching at 90 ℃ is negative electrode, and platinum electrode is anode, and it is electrolyte that solution is joined by institute, with 2 ~ 5 mAcm
-2for current density galvanostatic deposition 3 ~ 10 h, form film A;
Take 1 ~ 10 gram of pure NaCl of analysis and be positioned in 50 ~ 150 mL small beakers, add 40 ~ 140 mL distilled water, stir and make its dissolving; With
prepared film A is anode, graphite is negative electrode, it is electrolyte that NaCl solution is joined by institute, at 1 ~ 3 V constant voltage oxidation 30 ~ 120 min, forms BiOCl film, after being taken out, cleans with distilled water the BiOCl film making, naturally after drying, make required flake nano BiOCl film, this film consists of Tetragonal BiOCl, has staggered laminated structure, film has good absorption to ultraviolet light, learns that as calculated the band gap of made BiOCl film is about 3.42 eV.
2. adopt the prepared flake nano BiOCl of the electrochemical preparation method film photocatalytic material of a kind of flake nano bismoclite film photocatalytic material described in claim 1, it is characterized in that can be applicable in water in organic Treatment by Photocatalysis Oxidation, particularly in water, trace toxic is harmful in the processing of hardly degraded organic substance, light source used is wavelength 365 nm ultraviolet lights, reaction condition is: normal temperature and pressure, made BiOCl film photocatalytic material is positioned in aqueous organopolysiloxane over against light source, from reactor bottom, blasts air.
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| CN103779102B (en) * | 2014-01-17 | 2016-08-24 | 许昌学院 | Low-temperature in-site builds BiOI/Bi2s3hetero-junction thin-film and flexible optoelectronic chemistry solar cell device |
| CN107815701B (en) * | 2017-10-26 | 2019-09-27 | 太原理工大学 | A kind of nano-sheet is fluorinated electrochemical preparation method and its application of bismuth thin film |
| CN108745386A (en) * | 2018-04-28 | 2018-11-06 | 广州大学 | A kind of preparation method of BiOX photocatalyst |
| CN109518217B (en) * | 2018-11-23 | 2023-08-15 | 济南大学 | Preparation method of cobalt boride-based oxygen evolution catalyst |
| CN111530481A (en) * | 2020-05-26 | 2020-08-14 | 广东石油化工学院 | Method for rapidly preparing BiOBr nanosheet |
| CN114669308A (en) * | 2022-04-01 | 2022-06-28 | 哈尔滨理工大学 | BiOCl/Bi preparation by means of electrochemical method in-situ reaction24O31Cl10Method for compounding powder |
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| CN101024188A (en) * | 2007-02-15 | 2007-08-29 | 中国科学院上海硅酸盐研究所 | Halogen-oxide photocatalytic material and preparing method |
| CN101724839B (en) * | 2008-10-21 | 2011-07-27 | 国家纳米科学中心 | Micron/nanoscale BiOCl film material and preparation method thereof |
| CN101664687A (en) * | 2009-09-29 | 2010-03-10 | 福州大学 | Preparation of visible light catalyst of dye-sensitized bismuth oxyhalogenide and application thereof |
| CN102068998B (en) * | 2011-01-14 | 2012-12-12 | 太原理工大学 | Preparation and application methods of BiOBr/BiOCl compound photocatalyst |
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Inventor after: Fan Caimei Inventor after: Li Shuangzhi Inventor after: Wang Yunfang Inventor after: Liu Xiaoxia Inventor after: Wang Qin Inventor after: Zhang Weigang Inventor after: Zhang Xiaochao Inventor before: Fan Caimei Inventor before: Liu Xiaoxia |
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