CN104801320A - Bismuth oxyfluoride photocatalyst and preparing method of bismuth oxyfluoride photocatalyst - Google Patents

Bismuth oxyfluoride photocatalyst and preparing method of bismuth oxyfluoride photocatalyst Download PDF

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CN104801320A
CN104801320A CN201510229058.8A CN201510229058A CN104801320A CN 104801320 A CN104801320 A CN 104801320A CN 201510229058 A CN201510229058 A CN 201510229058A CN 104801320 A CN104801320 A CN 104801320A
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bismuthyl
fluorite
photochemical catalyst
acetic acid
glacial acetic
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CN104801320B (en
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任鸣
张棋棋
余东方
庞露
赵正阳
张波
杜茜
�田�浩
滕飞
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Nanjing University of Information Science and Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention discloses a bismuth oxyfluoride photocatalyst and a preparing method of the bismuth oxyfluoride photocatalyst. The preparing method comprises the following steps of adding glacial acetic acid into water, wherein the volume ratio of the glacial acetic acid to the water is 1:2-5:1, stirring the glacial acetic acid and the water, adding bismuth nitrate and soluble fluoride salt into glacial acetic acid solution, stirring in thermostatic waterbath of 75 DEG C to 85 DEG C for 20 to 40 minutes to dissolve the bismuth nitrate and the fluoride salt, making mixed solution with the bismuth nitrate concentrate as 0.95mmol/30ml to 1.05mmol/30ml and the mole ratio of bismuth element to fluorine element as 1:1.9 to 1:2.1, adding the mixed solution into a polytetrafluoroethylene lining to be subjected to thermal reaction for 10 to 13 hours in constant-temperature water of 120 DEG C to 160 DEG C, and obtaining the bismuth oxyfluoride photocatalyst after centrifuging, washing and drying. The preparing method is simple, practical, easy to popularize in large scale, suitable for making the bismuth oxyfluoride photocatalyst with high catalytic activity and applied to catalytic degradation of organic pollutants.

Description

Bismuthyl fluorite photochemical catalyst and preparation method thereof
Technical field
The present invention relates to field of catalyst preparation, be specifically related to bismuthyl fluorite photochemical catalyst and preparation method thereof.
Background technology
Along with the development of chemical industry, environmental pollution is day by day serious.Utilize semiconductor oxide materials can by the characteristic of activation at sunlight lower surface, can oxidation Decomposition organic pollution effectively.Compared with traditional environment purification processing method, Photocatalitic Technique of Semiconductor has the advantages such as reaction condition gentleness, non-secondary pollution, simple to operate and degradation effect be remarkable.TiO 2be the most common and be studied one of maximum catalyst, but its photo-generate electron-hole produced is to being easy to compound, cause electronics and hole can not migrate to surface in time and participate in redox reaction, thus phototranstormation efficiency is lower.Therefore the novel photocatalysis material finding excellent performance is very meaningful to obtain the photochemical catalyst with high efficiency photocatalysis activity.
Bismuth-containing series compound has purposes widely, not only may be used for pharmaceuticals industry, also can be applicable to semiconductor.Due to the metal that bismuth element is a kind of nontoxic green relatively, in recent years in the preparation of photochemical catalyst, day by day replace compound that is leaded, the toxic element such as antimony, cadmium, mercury.
Summary of the invention
The object of the present invention is to provide a kind of method preparing bismuthyl fluorite photochemical catalyst, the method is simple, be easy to large-scale promotion, the bismuthyl fluorite photochemical catalyst that catalytic activity is high can be obtained;
Another object of the present invention is to the bismuthyl fluorite photochemical catalyst providing three kinds of different fluorine/oxygen, catalytic activity is high;
An also object of the present invention is the application of bismuthyl fluorite photochemical catalyst in catalyze and degrade organic pollutants providing three kinds of different fluorine/oxygen.
Above-mentioned purpose is achieved by the following technical solution:
Prepare a method for bismuthyl fluorite photochemical catalyst, comprise the steps:
(1) glacial acetic acid solution preparation: Xiang Shuizhong adds glacial acetic acid, and the volume ratio of glacial acetic acid and water is 1:2 ~ 5:1, stirs;
(2) water-bath is dissolved: in glacial acetic acid solution, add bismuth nitrate and soluble fluorinated salt, stir 20 ~ 40 minutes under 75 DEG C ~ 85 DEG C waters bath with thermostatic control, bismuth nitrate and fluoride salt are dissolved, make the mixed solution that bismuth nitrate concentration is 0.95mmol/30ml ~ 1.05mmol/30ml, the mol ratio of bismuth element and fluorine element is 1:1.9 ~ 1:2.1;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 120 ~ 160 DEG C of incubation water heatings reaction 10 ~ 13 hours, namely obtains bismuthyl fluorite photochemical catalyst after centrifugal, washing, drying.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (2) bismuth nitrate is five water bismuth nitrates.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (2) soluble fluorinated salt is sodium fluoride or ammonium fluoride.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (3) the incubation water heating reaction time is 10.5 hours, and temperature is 150 DEG C.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (3) the incubation water heating reaction time is 11.5 hours, and temperature is 150 DEG C.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (3) the incubation water heating reaction time is 12.5 hours, and temperature is 150 DEG C.
150 DEG C of hydro-thermal reactions 10.5 are constantly little, can obtain Bi according to the above-mentioned method preparing bismuthyl fluorite photochemical catalyst 7o 5f 11bismuthyl fluorite photochemical catalyst.
150 DEG C of hydro-thermal reactions 11.5 are constantly little, can obtain BiO according to the above-mentioned method preparing bismuthyl fluorite photochemical catalyst 0.51f 1.98bismuthyl fluorite photochemical catalyst.
150 DEG C of hydro-thermal reactions 12.5 are constantly little, can obtain BiO according to the above-mentioned method preparing bismuthyl fluorite photochemical catalyst 0.67f 1.66bismuthyl fluorite photochemical catalyst.
The application of bismuthyl fluorite photochemical catalyst in catalyze and degrade organic pollutants of above-mentioned three kinds of different fluorine/oxygen.
beneficial effect of the present invention:
1, the method preparing bismuthyl fluorite photochemical catalyst provided by the invention is simple, is easy to large-scale promotion, can obtains the bismuthyl fluorite photochemical catalyst that catalytic activity is high.
2, the equal Absorbable organic halogens of the bismuthyl fluorite photochemical catalyst of three kinds of different fluorine/oxygen provided by the invention exists, and form is good, and catalytic activity is high, can the rhodamine B (RhB) in efficient degradation waste water solution and the methylene blue (MB) in methylene blue solution.
Accompanying drawing explanation
Fig. 1: the uv drs figure implementing three kinds of bismuthyl fluorite photochemical catalysts prepared by 1-3;
Fig. 2: three kinds of bismuthyl fluorite photochemical catalysts prepared by enforcement 1-3 are to the degradation capability curve of RhB and MB;
Fig. 3: the Bi implementing 1 preparation 7o 5f 11with comparing of standard card JCPDS:50-0003;
Fig. 4: the BiO implementing 3 preparations 0.67f 1.66with comparing of standard card JCPDS:24-0146;
Fig. 5: the BiO implementing 2 preparations 0.51f 1.98with comparing of standard card JCPDS:24-0147.
Detailed description of the invention
Technical scheme of the present invention is described in detail below in conjunction with specific embodiment.
embodiment 1:Bi 7 o 5 f 11 the preparation of bismuthyl fluorite photochemical catalyst
(1) glacial acetic acid solution preparation: add 30ml glacial acetic acid in 30ml water, namely glacial acetic acid and water are by volume for 1:1 mixes, stirs;
(2) water-bath is dissolved: get 30ml glacial acetic acid solution, add five water bismuth nitrate 0.4851g(1mmol) and sodium fluoride 0.0840g(2mmol), stir 30 minutes under 80 DEG C of waters bath with thermostatic control, bismuth nitrate and sodium fluoride are dissolved and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 150 DEG C of incubation water heatings react 10.5 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain Bi 7o 5f 11bismuthyl fluorite photochemical catalyst.
As shown in Figure 1, this catalyst has UV absorption, has ultraviolet catalytic activity.As seen from Figure 3, obtained catalyst is pure, and degree of crystallinity is higher.Sodium fluoride can use ammonium fluoride to replace, and addition is 0.0741g(2mmol).
embodiment 2:BiO 0.51 f 1.98 the preparation of bismuthyl fluorite photochemical catalyst
(1) glacial acetic acid solution preparation: add 30ml glacial acetic acid in 30ml water, namely glacial acetic acid and water are by volume for 1:1 mixes, stirs;
(2) water-bath is dissolved: get 30ml glacial acetic acid solution, add five water bismuth nitrate 0.4851g(1mmol) and sodium fluoride 0.0840g(2mmol), stir 30 minutes under 80 DEG C of waters bath with thermostatic control, bismuth nitrate and sodium fluoride are dissolved and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 150 DEG C of incubation water heatings react 11.5 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain BiO 0.51f 1.98bismuthyl fluorite photochemical catalyst.
As shown in Figure 1, this catalyst has UV absorption, has ultraviolet catalytic activity.As seen from Figure 5, obtained catalyst is pure, and degree of crystallinity is higher.Sodium fluoride can use ammonium fluoride to replace, and addition is 0.0741g(2mmol).
embodiment 3:BiO 0.67 f 1.66 the preparation of bismuthyl fluorite photochemical catalyst
(1) glacial acetic acid solution preparation: add 30ml glacial acetic acid in 30ml water, namely glacial acetic acid and water are by volume for 1:1 mixes, stirs;
(2) water-bath is dissolved: get 30ml glacial acetic acid solution, add five water bismuth nitrate 0.4851g(1mmol) and sodium fluoride 0.0840g(2mmol), stir 30 minutes under 80 DEG C of waters bath with thermostatic control, bismuth nitrate and sodium fluoride are dissolved and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 150 DEG C of incubation water heatings react 12.5 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain BiO 0.67f 1.66bismuthyl fluorite photochemical catalyst.
As shown in Figure 1, this catalyst has UV absorption, has ultraviolet catalytic activity.Can be drawn by Fig. 4, obtained catalyst is pure, and degree of crystallinity is higher.Sodium fluoride can use ammonium fluoride to replace, and addition is 0.0741g(2mmol).
embodiment 4:Bi 7 o 5 f 11 the preparation of bismuthyl fluorite photochemical catalyst
(1) glacial acetic acid solution preparation: add 40ml glacial acetic acid in 20ml water, namely glacial acetic acid and water are by volume for 1:2 mixes, stirs;
(2) water-bath is dissolved: get 30ml glacial acetic acid solution, add five water bismuth nitrate 0.4608g(0.95mmol) and sodium fluoride 0.0758g(1.805mmol), stir 40 minutes under 75 DEG C of waters bath with thermostatic control, bismuth nitrate and sodium fluoride are dissolved and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 120 DEG C of incubation water heatings react 13 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain Bi 7o 5f 11bismuthyl fluorite photochemical catalyst.
Obtained catalyst composition is consistent with embodiment 1, and physical property is similar with catalytic activity.
embodiment 5:Bi 7 o 5 f 11 the preparation of bismuthyl fluorite photochemical catalyst
(1) glacial acetic acid solution preparation: add 10ml glacial acetic acid in 50ml water, namely glacial acetic acid and water are by volume for 5:1 mixes, stirs;
(2) water-bath is dissolved: get 30ml glacial acetic acid solution, add five water bismuth nitrate 0.5094g(1.05mmol) and sodium fluoride 0.0926g(2.205mmol), stir 20 minutes under 85 DEG C of waters bath with thermostatic control, bismuth nitrate and sodium fluoride are dissolved and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 160 DEG C of incubation water heatings react 10 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain Bi 7o 5f 11bismuthyl fluorite photochemical catalyst.
Obtained catalyst composition is consistent with embodiment 1, and physical property is similar with catalytic activity.
embodiment 6: three kinds of bismuthyl fluorite photochemical catalysts are to the Degrading experiment of RhB
Take three kinds of bismuthyl fluorite photochemical catalyst 0.1g that embodiment 1-3 is obtained respectively, add the RhB solution of 200ml respectively, RhB concentration is 10mg/L.First lucifuge stirs 30min, makes dyestuff reach absorption/desorption equilibrium at catalyst surface.Then open xenon source and carry out light-catalyzed reaction under UV-irradiation, supernatant spectrophotometer detects.According to RhB change in concentration in 553nm place light absorption value determination degradation process.
RhB degrades situation as shown in Figure 2, and abscissa is light application time, and ordinate is the ratio of RhB concentration value and the RhB initial concentration measured after irradiating a period of time.As can be seen from Figure, after illumination 100min, three kinds of catalyst energy catalytic degradation RhB 60 ~ 80%, have efficient Photocatalytic activity to RhB.
embodiment 7: three kinds of bismuthyl fluorite photochemical catalysts are to the Degrading experiment of MB
Take three kinds of bismuthyl fluorite photochemical catalyst 0.1g that embodiment 1-3 is obtained respectively, add the MB solution of 200ml respectively, MB concentration is 4.5mg/L.First lucifuge stirs 30min, makes dyestuff reach absorption/desorption equilibrium at catalyst surface.Then open xenon source and carry out light-catalyzed reaction under UV-irradiation, supernatant spectrophotometer detects.According to MB change in concentration in 668nm place light absorption value determination degradation process.
MB degrades situation as shown in Figure 2, and abscissa is light application time, and ordinate is the ratio of MB concentration value and the MB initial concentration measured after irradiating a period of time.As can be seen from Figure, bismuthyl fluorite photochemical catalyst reaches 10% ~ 20% to the adsorbance of MB in first 30 minutes; After illumination 30min, in MB dye solution, MB degrades about 50%.After 60min, dyestuff degradation rate reaches 70 ~ 80%.Bismuthyl fluorite photochemical catalyst can be obtained thus and have higher absorption property and efficient photocatalytic activity to MB.

Claims (10)

1. prepare a method for bismuthyl fluorite photochemical catalyst, it is characterized in that comprising the steps:
(1) glacial acetic acid solution preparation: Xiang Shuizhong adds glacial acetic acid, and the volume ratio of glacial acetic acid and water is 1:2 ~ 5:1, stirs;
(2) water-bath is dissolved: in glacial acetic acid solution, add bismuth nitrate and soluble fluorinated salt, stir 20 ~ 40 minutes under 75 DEG C ~ 85 DEG C waters bath with thermostatic control, bismuth nitrate and fluoride salt are dissolved, make the mixed solution that bismuth nitrate concentration is 0.95mmol/30ml ~ 1.05mmol/30ml, the mol ratio of bismuth element and fluorine element is 1:1.9 ~ 1:2.1;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 120 ~ 160 DEG C of incubation water heatings reaction 10 ~ 13 hours, namely obtains bismuthyl fluorite photochemical catalyst after centrifugal, washing, drying.
2. the method preparing bismuthyl fluorite photochemical catalyst according to claim 1, is characterized in that: in step (2), and bismuth nitrate is five water bismuth nitrates.
3. the method preparing bismuthyl fluorite photochemical catalyst according to claim 1, is characterized in that: in step (2), and soluble fluorinated salt is sodium fluoride or ammonium fluoride.
4., according to the arbitrary described method preparing bismuthyl fluorite photochemical catalyst of claims 1 to 3, it is characterized in that: in step (3), the incubation water heating reaction time is 10.5 hours, and temperature is 150 DEG C.
5., according to the arbitrary described method preparing bismuthyl fluorite photochemical catalyst of claims 1 to 3, it is characterized in that: in step (3), the incubation water heating reaction time is 11.5 hours, and temperature is 150 DEG C.
6., according to the arbitrary described method preparing bismuthyl fluorite photochemical catalyst of claims 1 to 3, it is characterized in that: in step (3), the incubation water heating reaction time is 12.5 hours, and temperature is 150 DEG C.
7. the Bi that described in a claim 4 prepared by method 7o 5f 11bismuthyl fluorite photochemical catalyst.
8. the BiO that described in a claim 5 prepared by method 0.51f 1.98bismuthyl fluorite photochemical catalyst.
9. the BiO that described in a claim 6 prepared by method 0.67f 1.66bismuthyl fluorite photochemical catalyst.
10. the application of the arbitrary bismuthyl fluorite photochemical catalyst of claim 7 to 9 in catalyze and degrade organic pollutants.
CN201510229058.8A 2015-05-07 2015-05-07 Bismuthyl fluorite photochemical catalyst and preparation method thereof Expired - Fee Related CN104801320B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104998666A (en) * 2015-08-10 2015-10-28 南京信息工程大学 Method for preparing bowknot-shaped fluorine-oxygen-bismuth photocatalyst and application of catalyst
CN114832847A (en) * 2022-05-07 2022-08-02 南京信息工程大学 NaCl hydrothermal treatment Bi 2 O 2 CO 3 Simple preparation method of photocatalyst
CN115999587A (en) * 2023-02-20 2023-04-25 河南农业大学 Photocatalytic material and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070190414A1 (en) * 2004-10-01 2007-08-16 Rutgers, The State University Bismuth oxyfluoride based nanocomposites as electrode materials
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
CN103920509A (en) * 2014-04-21 2014-07-16 合肥工业大学 Mesoporous BiOX photocatalyst and preparation method and application thereof
CN104258877A (en) * 2014-09-03 2015-01-07 江南大学 Preparation method capable of controlling oriented growth of bismuth oxybromide photocatalysts

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070190414A1 (en) * 2004-10-01 2007-08-16 Rutgers, The State University Bismuth oxyfluoride based nanocomposites as electrode materials
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
CN103920509A (en) * 2014-04-21 2014-07-16 合肥工业大学 Mesoporous BiOX photocatalyst and preparation method and application thereof
CN104258877A (en) * 2014-09-03 2015-01-07 江南大学 Preparation method capable of controlling oriented growth of bismuth oxybromide photocatalysts

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104998666A (en) * 2015-08-10 2015-10-28 南京信息工程大学 Method for preparing bowknot-shaped fluorine-oxygen-bismuth photocatalyst and application of catalyst
CN114832847A (en) * 2022-05-07 2022-08-02 南京信息工程大学 NaCl hydrothermal treatment Bi 2 O 2 CO 3 Simple preparation method of photocatalyst
CN115999587A (en) * 2023-02-20 2023-04-25 河南农业大学 Photocatalytic material and preparation method and application thereof
CN115999587B (en) * 2023-02-20 2024-05-28 河南农业大学 Photocatalytic material and preparation method and application thereof

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