CN105749945A - A Preparation Method of Fe(Ш)/Bi2O2CO3 Photocatalyst - Google Patents
A Preparation Method of Fe(Ш)/Bi2O2CO3 Photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract 11
- 238000002360 preparation method Methods 0.000 title claims abstract 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract 7
- 239000007864 aqueous solution Substances 0.000 claims abstract 5
- 239000000243 solution Substances 0.000 claims abstract 4
- 239000011521 glass Substances 0.000 claims abstract 3
- 239000011259 mixed solution Substances 0.000 claims 4
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 claims 3
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 claims 3
- 238000010438 heat treatment Methods 0.000 claims 2
- 229950000845 politef Drugs 0.000 claims 2
- 238000007789 sealing Methods 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052797 bismuth Inorganic materials 0.000 claims 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 230000009514 concussion Effects 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 abstract 1
- 229940074439 potassium sodium tartrate Drugs 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 abstract 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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
本发明公开了一种Fe(Ш)/Bi2O2CO3光催化剂的制备方法。该方法包括如下步骤：先将Bi(NO3)3·5H2O和酒石酸钾钠溶于水中，再将上述溶液超声1小时后转入到聚四氟乙烯水热釜中，在一定温度下反应12小时后，得到花状Bi2O2CO3；将上述所得的Bi2O2CO3分散到一定体积的Fe(NO3)3水溶液中，搅拌20分钟；将上述所得溶液转入到密封的玻璃反应器中，在一定温度下保温一定时间后，将所得的沉淀过滤，洗涤，再真空干燥，既得到Fe(Ш)/Bi2O2CO3光催化剂。本发明所制备的Fe(Ш)/Bi2O2CO3光催化剂具有良好的可见光光催化活性，能在模拟太阳光下降解有机污染物。
The invention discloses a preparation method of Fe(Ш)/Bi 2 O 2 CO 3 photocatalyst. The method comprises the following steps: first dissolving Bi(NO 3 ) 3 .5H 2 O and potassium sodium tartrate in water, then ultrasonicating the above solution for 1 hour, and then transferring it to a polytetrafluoroethylene hydrothermal kettle, at a certain temperature After 12 hours of reaction, flower-shaped Bi 2 O 2 CO 3 was obtained; the Bi 2 O 2 CO 3 obtained above was dispersed into a certain volume of Fe(NO 3 ) 3 aqueous solution, and stirred for 20 minutes; the solution obtained above was transferred to In a sealed glass reactor, after holding at a certain temperature for a certain period of time, the obtained precipitate is filtered, washed, and then vacuum-dried to obtain a Fe(Ш)/Bi 2 O 2 CO 3 photocatalyst. The Fe(Ш)/Bi 2 O 2 CO 3 photocatalyst prepared by the invention has good visible light photocatalytic activity and can degrade organic pollutants under simulated sunlight.
Description
Technical field
The invention belongs to photocatalyst technology field.It is specifically related to a kind of Fe (Ш)/Bi2O2CO3The preparation method of photocatalyst.
Background technology
Along with developing rapidly of industry, environmental pollution is increasingly severe, threatens the existence of the mankind gradually.Utilize solar energy, be the pollution treatment technology of a kind of energy-saving and environmental protection by photocatalysis technology degradation of contaminant, it is believed that be solve environmental problem method most effective, most promising.Bi2O2CO3A kind of novel photocatalyst, can degradable organic pollutant under ultraviolet light, than commercial P25, there is higher activity.But, Bi2O2CO3Energy gap be about 3.4eV, it is impossible to absorb visible ray.Additionally, the ultraviolet light in sunlight only accounts for about 4.5%, and visible ray accounts for 45%.It is therefore desirable to improve Bi2O2CO3Visible light photocatalysis performance.
Recent studies indicate that: modify Fe (Ш) in photocatalyst surface, it is possible to significantly improve TiO2, the photocatalyst such as BiOCl visible ray photoresponse scope, and improve their visible light photocatalysis active.But there is presently no and improve Bi about by modification Fe (Ш)2O2CO3The report of photocatalytic activity.
Summary of the invention
It is an object of the invention to provide a kind of Fe (Ш)/Bi2O2CO3The preparation method of photocatalyst.This preparation method is simple to operate, and synthesis condition is gentle, and cost is low, prepared Fe (Ш)/Bi2O2CO3There is obvious visible light photocatalysis active, can at degradable organic pollutant under simulated solar irradiation.
The technical solution of the present invention is: a kind of Fe (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that comprise the steps:
(1) with Bi (NO3)3·5H2O is bismuth source, and sodium potassium tartrate tetrahydrate is carbon source, with water for solvent, by Bi (NO3)3·5H2The consumption proportion of O, sodium potassium tartrate tetrahydrate and water respectively 2～6g:4～10g:90mL water makes mixed solution；
(2) it is transferred in politef water heating kettle after above-mentioned mixed solution ultrasonic wave concussion being processed 1 hour, at 100～200 DEG C, is incubated 12 hours, obtains flower-shaped Bi2O2CO3；
(3) by the Bi of step (2) gained2O2CO3It is distributed to the Fe (NO of 0.005～0.02 mol/L3)3In aqueous solution, stir 20 minutes；
(4) solution obtained by step (3) is transferred in the glass reactor of sealing, after being incubated 1 hour at 50～98 DEG C, the precipitation of gained is filtered, washing, then carry out vacuum drying, both obtain Fe (Ш)/Bi2O2CO3Photocatalyst.
Further, in above-mentioned steps (3), by Bi2O2CO3With Fe (NO3)3The consumption proportion that aqueous solution is 0.5～1.5g:5～30mL mixes.
Further, in above-mentioned steps (1), by Bi (NO3)3·5H2The consumption proportion of O, sodium potassium tartrate tetrahydrate and water respectively 4.5～5g:8.5～9g:90mL makes mixed solution.
Further, in above-mentioned steps (2), described mixed solution is transferred in politef water heating kettle, after reacting 12 hours, obtains flower-shaped Bi at 170～190 DEG C2O2CO3。
Further, in above-mentioned steps (3), by Bi2O2CO3With Fe (NO3)3The consumption proportion that aqueous solution is 0.8～1.1g:18～22mL mixes, described Fe (NO3)3The concentration of aqueous solution is 0.008～0.01 mol/L.
Further, in above-mentioned steps (4), after described solution is transferred in the glass reactor of sealing, at 85～95 DEG C, it is incubated 1 hour.
The beneficial effects of the present invention is；Compare existing Bi2O2CO3Photocatalyst, the present invention is by Bi2O2CO3Photocatalyst surface modifies Fe (Ш), greatly improves Bi2O2CO3The visible light photocatalysis active of photocatalyst, can at degradable organic pollutant under simulated solar irradiation.Additionally, the preparation method of the present invention is simple to operate, synthesis condition is gentle, less costly, is beneficial to popularization and application.
Accompanying drawing explanation
Fig. 1 is Fe (the Ш)/Bi prepared by embodiment 12O2CO3The scanning electron microscope (SEM) photograph of photocatalyst；
Fig. 2 is Fe (the Ш)/Bi prepared by embodiment 12O2CO3The XRD spectra of photocatalyst；
Fig. 3 is Fe (the Ш)/Bi prepared by embodiment 12O2CO3The XPS high-resolution spectrogram of the Fe element in photocatalyst；
Fig. 4 is Fe (the Ш)/Bi prepared by embodiment 12O2CO3Photocatalyst and Bi2O2CO3Photocatalyst declines in visible ray (A) illumination and solves the photocatalytic activity comparison diagram of methyl orange；
Fig. 5 is Fe (the Ш)/Bi prepared by embodiment 12O2CO3Photocatalyst and Bi2O2CO3Photocatalyst declines in simulated solar irradiation (B) illumination and solves the photocatalytic activity comparison diagram of methyl orange.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated.
Fe (Ш)/Bi prepared by the present invention2O2CO3The photocatalytic activity of photocatalyst is respectively through under visible ray and simulated solar irradiation, and the methyl orange in photocatalytic degradation solution carries out characterizing.Experimentation is as follows: Fe (Ш)/Bi2O2CO3The test of the Photocatalytic Activity for Degradation methyl orange of photocatalyst is to carry out in the culture dish that diameter is 7 centimetres, and the initial concentration of methyl orange is 4 × 10-5Mol/L, with the xenon lamp of 300 watts for light source, and puts into one piece between xenon lamp and culture dish and can excise the wavelength optical filter at below 420nm ultraviolet light.By 0.1 gram of Fe (Ш)/Bi during experiment2O2CO3Photocatalyst coating is bottom culture dish, container adds 25 milliliters of methyl orange solutions, container is placed in from light source 20 centimeters, and make beam orthogonal in sample irradiation, every illumination detects the concentration of methyl orange in a solution after 10 minutes, the concentration of methyl orange is measured by ultraviolet-visual spectrometer (UV-2550).Fe(Ш)/Bi2O2CO3Photocatalyst is also carry out in the culture dish that diameter is 7 centimetres in the test of simulated solar irradiation photo-catalytic degradation of methyl-orange, and the initial concentration of methyl orange is 4 × 10-5Mol/L, with the xenon lamps of 300 watts for simulated solar radiant.By 0.1 gram of Fe (Ш)/Bi during experiment2O2CO3Photocatalyst coating is bottom culture dish, container adds 25 milliliters of methyl orange solutions, container is placed in from light source 20 centimeters, and make beam orthogonal in sample irradiation, every illumination detects the concentration of methyl orange in a solution after 10 minutes, the concentration of methyl orange is measured by ultraviolet-visual spectrometer (UV-2550).
Fe(Ш)/Bi2O2CO3The characterizing method of the micro structure of photocatalyst is: be X-ray source, sweep speed at Cu target K α be 0.05 ° of s-1X-ray diffractometer (HZG41/B-PC type) on X-ray diffraction (XRD) collection of illustrative plates that obtains.Fe (Ш)/Bi is observed with field emission scanning electron microscope (SEM)2O2CO3The pattern of photocatalyst.Fe (Ш)/Bi is have detected with x-ray photoelectron spectroscopy (XPS) High Resolution Spectrum2O2CO3The chemical state of Fe element in photocatalyst.
Owing to the electrode potential of Fe (Ш)/Fe (II) compares Bi2O2CO3Conduction band potential just, so Bi2O2CO3Light induced electron in valence band can be transferred to after excited by visible light on the relatively low Fe in electromotive force position (Ш), so Fe (Ш)/Bi2O2CO3The light-catalyzed reaction mechanism of photocatalyst is: under visible ray illumination, Bi2O2CO3Being excited, produce light induced electron and hole, the raw electron transfer of the light splitting that is excited is to Bi2O2CO3On the Fe (Ш) on surface, generating Fe (II), Fe (Ш) is oxidized to Fe (Ш) with the oxygen effect in solution again, stays Bi2O2CO3Hole in valence band just can oxidation Decomposition organic pollution.Under simulated solar irradiation irradiates, Bi2O2CO3By sunlight medium ultraviolet light and excited by visible light, producing light induced electron and hole, wherein the mechanism of the electron-hole pair degradable organic pollutant that visible ray produces is with above visible ray mechanism is the same.The Bi that the light induced electron produced by ultraviolet excitation directly transits to2O2CO3Conduction band on, be then transferred to Bi2O2CO3On the Fe (Ш) on surface, then generate superoxide radical, superoxide radical energy oxidation Decomposition organic pollution with the oxygen effect in solution.
Embodiment 1:
A kind of Fe (Ш)/Bi2O2CO3The preparation method of photocatalyst, comprises the following steps:
(1) by 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water；
(2) it is transferred in politef water heating kettle after above-mentioned solution ultrasonic wave concussion being processed 1 hour, after reacting 12 hours at 180 DEG C, obtains flower-shaped Bi2O2CO3；
(3) by the Bi prepared by 1 gram of above-mentioned steps (2)2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, stir 20 minutes；
(4) solution of above-mentioned steps (3) gained is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Fig. 1 is Fe (the Ш)/Bi prepared by the present embodiment2O2CO3The scanning electron microscope (SEM) photograph of photocatalyst, it is seen that Fe (Ш)/Bi2O2CO3Photocatalyst is flower-shaped.
Fig. 2 is Fe (the Ш)/Bi prepared by the present embodiment2O2CO3The XRD figure of photocatalyst, it is seen that all of diffraction maximum both corresponds to Bi2O2CO3.Owing to the content of Fe (Ш) ion is little, can't see their associated diffraction peak.
Fig. 3 is Fe (the Ш)/Bi prepared by the present embodiment2O2CO3The XPS High-Resolution Map of Fe element in photocatalyst, combine can be 711.0 and 724.7eV occur two peaks correspond respectively to Fe2p3/2And Fe2p5/2, this is the peak of typical iron ion, illustrates that Fe (Ш) has successfully loaded to Bi2O2CO3The surface of photocatalyst.
Fe (Ш)/Bi that Fig. 4, Fig. 5 are respectively prepared by the present embodiment2O2CO3With Bi2O2CO3Photocatalyst declines at visible ray (A) and simulated solar irradiation (B) and solves the expression activitiy of methyl orange, and the C/C0 in vertical coordinate represents the concentration after methyl orange degradation and the ratio of the methyl orange initial concentration before degraded；It is seen that under visible ray, Fe (Ш)/Bi2O2CO3Photocatalyst within 120 minutes, can degrade 38% methyl orange, and pure phase Bi2O2CO3Only degrade the methyl orange of 2.3%, Bi prepared by case study on implementation 1 is described2O2CO3The visible light photocatalysis active of photocatalyst significantly improves；Under simulated solar irradiation, Fe (Ш)/Bi2O2CO3Photocatalyst within 60 minutes, can degrade 82.2% methyl orange, and pure phase Bi2O2CO3Only degrade the methyl orange of 63.1%, Fe (Ш)/Bi2O2CO3There is higher activity.
Embodiment 2:
By 4.85 grams of Bi (NO3)3·5H2O and 8.5 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Embodiment 3:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Embodiment 4:
By 4.85 grams of Bi (NO3)3·5H2O and 9 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Above-described embodiment 2-4 is to check sodium potassium tartrate tetrahydrate to Fe (Ш)/Bi2O2CO3The impact of properties of catalyst and the embodiment that designs, except the mass change of sodium potassium tartrate tetrahydrate, other reaction conditions are all identical with case study on implementation 1.It was found that when sodium potassium tartrate tetrahydrate respectively 8.5 grams, 8.8 grams, 9 grams, prepared Fe (Ш)/Bi2O2CO3Photocatalyst under visible ray illumination, within 120 minutes, can degrade respectively 34.5%, 38% and 36.2% methyl orange；Under simulated solar irradiation, within 60 minutes, can degrade respectively 75.4%, 82.2% and 78.6% methyl orange, therefore best sodium potassium tartrate tetrahydrate quality is 8.5～9 grams.
Embodiment 5:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 18 ml concns are 0.008 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Embodiment 6:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Embodiment 7:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 22 ml concns are 0.01 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Above-described embodiment 5-7 is for inspection Fe (NO3)3To Fe (Ш)/Bi2O2CO3The impact of properties of catalyst and the embodiment that designs, except Fe (NO3)3Volume and concentration change outside, other reaction conditions are all identical with case study on implementation 1.It was found that ought respectively by Bi2O2CO3It is distributed to 18 milliliter of 0.008 mol/L Fe (NO3)3, 20 milliliter of 0.009 mol/L Fe (NO3)3With 22 milliliter of 0.01 mol/L Fe (NO3)3Time, prepared Fe (Ш)/Bi2O2CO3Photocatalyst under visible ray illumination, within 120 minutes, can degrade respectively 32.7%, 38% and 35.8% methyl orange；Under simulated solar irradiation, within 60 minutes, can degrade respectively 73.6%, 82.2% and 77.1% methyl orange, therefore best Fe (NO3)3Addition is 18～22 ml concns is the Fe (NO of 0.008～0.01 mol/L3)3。
Case study on implementation 8:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 85 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Case study on implementation 9:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 90 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Case study on implementation 10:
By 4.85 grams of Bi (NO3)3·5H2O and 8.8 grams of sodium potassium tartrate tetrahydrates are dissolved in 90 milliliters of water, then are processed after 1 hour by above-mentioned solution ultrasonic wave concussion and be transferred in politef water heating kettle, after reacting 12 hours, obtain flower-shaped Bi at 180 DEG C2O2CO3；Then by the Bi of 1 gram of above-mentioned preparation2O2CO3It is distributed to the Fe (NO that 20 ml concns are 0.009 mol/L3)3In aqueous solution, after stirring 20 minutes, above-mentioned solution is transferred in the glass reactor of sealing, after being incubated 1 hour at 95 DEG C, the precipitation of gained is filtered, washing, then vacuum drying, both obtained Fe (Ш)/Bi2O2CO3Photocatalyst.
Above-described embodiment 8-10 is sealed in glass reactor temperature to Fe (Ш)/Bi for inspection2O2CO3The impact of properties of catalyst and the embodiment that designs, except variations in temperature, other reaction conditions are all identical with case study on implementation 1.It was found that when being sealed in glass reactor temperature respectively 85 DEG C, 90 DEG C and 95 DEG C, prepared Fe (Ш)/Bi2O2CO3Photocatalyst under visible ray illumination, within 120 minutes, can degrade respectively 36.3%, 38% and 37.7% methyl orange；Under simulated solar irradiation, within 60 minutes, can degrade respectively 79.5%, 82.2% and 80.4% methyl orange, therefore in glass reactor, optimum temperature is 85～95 DEG C.
It should be noted that; the operation principle of the present invention is described in detail above in association with accompanying drawing; but it will be appreciated by those skilled in the art that; detailed description of the invention illustrates the present invention with being only for demonstration; description is only for explaining claims, and protection scope of the present invention is not limited to description.Any those familiar with the art in technical scope disclosed by the invention, the change that can readily occur in or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. Fe (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that comprise the steps:
(1) with Bi (NO3)3·5H2O is bismuth source, and sodium potassium tartrate tetrahydrate is carbon source, with water for solvent, by Bi (NO3)3·5H2The consumption proportion of O, sodium potassium tartrate tetrahydrate and water respectively 2～6g:4～10g:90mL water makes mixed solution；
(2) it is transferred in politef water heating kettle after above-mentioned mixed solution ultrasonic wave concussion being processed 1 hour, at 100～200 DEG C, is incubated 12 hours, obtains flower-shaped Bi2O2CO3；
(3) by the Bi of step (2) gained2O2CO3It is distributed to the Fe (NO of 0.005～0.02 mol/L3)3In aqueous solution, stir 20 minutes；
(4) solution obtained by step (3) is transferred in the glass reactor of sealing, after being incubated 1 hour at 50～98 DEG C, the precipitation of gained is filtered, washing, then carry out vacuum drying, both obtain Fe (Ш)/Bi2O2CO3Photocatalyst.
2. Fe according to claim 1 (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that in described step (3), by Bi2O2CO3With Fe (NO3)3The consumption proportion that aqueous solution is 0.5～1.5g:5～30mL mixes.
3. Fe according to claim 2 (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that in described step (1), by Bi (NO3)3·5H2The consumption proportion of O, sodium potassium tartrate tetrahydrate and water respectively 4.5～5g:8.5～9g:90mL makes mixed solution.
4. Fe according to claim 1 (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that in described step (2), described mixed solution is transferred in politef water heating kettle, after reacting 12 hours, obtains flower-shaped Bi at 170～190 DEG C2O2CO3。
5. Fe according to claim 1 (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that in described step (3), by Bi2O2CO3With Fe (NO3)3The consumption proportion that aqueous solution is 0.8～1.1g:18～22mL mixes, described Fe (NO3)3The concentration of aqueous solution is 0.008～0.01 mol/L.
6. Fe according to claim 1 (Ш)/Bi2O2CO3The preparation method of photocatalyst, it is characterised in that in step (4), after described solution is transferred in the glass reactor of sealing, is incubated 1 hour at 85～95 DEG C.
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| CN106268895A (en) * | 2016-08-23 | 2017-01-04 | 扬州天辰精细化工有限公司 | A kind of preparation method of iron sesquioxide bismuthyl carbonate composite photo-catalyst |
| CN108212187A (en) * | 2018-01-26 | 2018-06-29 | 湖北文理学院 | Fe adulterates Bi2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Photochemical catalyst |
| CN112774706A (en) * | 2021-01-31 | 2021-05-11 | 湖南科技大学 | Bismuth oxycarbonate/sepiolite composite photocatalyst and preparation method thereof |
| CN112774706B (en) * | 2021-01-31 | 2023-10-24 | 湖南科技大学 | Bismuth oxide carbonate/sepiolite composite photocatalyst and preparation method thereof |
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