CN104368362A - Microemulsion-like photocatalyst, preparation method and applications thereof - Google Patents
Microemulsion-like photocatalyst, preparation method and applications thereof Download PDFInfo
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- CN104368362A CN104368362A CN201410477445.9A CN201410477445A CN104368362A CN 104368362 A CN104368362 A CN 104368362A CN 201410477445 A CN201410477445 A CN 201410477445A CN 104368362 A CN104368362 A CN 104368362A
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Abstract
The present invention discloses a microemulsion-like BiOBr photocatalyst, wherein any one selected from BiBr3, Bi(NO3)3.5H2O and Bi2O3 is adopted as a bismuth source, hydrobromic acid is adopted as a bromine source, water or ethanol is adopted as a solvent, ammonia water is adopted as a pH value adjusting agent, sodium metaphosphate is adopted as a dispersant, and a simple hydrolysis or alcoholysis method is adopted to prepare the microemulsion-like BiOBr photocatalyst at a room temperature. The present invention further discloses a preparation method and applications of the microemulsion-like BiOBr photocatalyst. Compared with the existing BiOBr powder photocatalyst, the microemulsion-like BiOBr photocatalyst has the following characteristics that: the microemulsion-like BiOBr photocatalyst exists in the emulsion form in the photocatalytic treatment system, and has good dispersity, good repeatability and excellent photocatalytic property, the defects of easy agglomeration and poor dispersion of the powder catalyst, and the problem of complex process and activity reducing of the film catalyst are effectively avoided, and the large specific surface area of the catalyst is ensured.
Description
Technical field
The present invention relates to a kind of microemulsion photochemical catalyst, specifically a kind of microemulsion BiOBr photochemical catalyst, its preparation method and its process organic pollution in application, belong to inorganic environment-friendly synthesis photocatalyst technology field.
Background technology
In recent years, along with the develop rapidly of modern industry (especially dye industry), the problem aggravations such as waste water from dyestuff disposal of pollutants.Wherein, dye organic pollutant is difficult to be oxidized by common oxidizer or be degraded by microorganisms, and causes the pollution of serious water body, soil and ecological environment.Finding out a kind of quick, cost-effective method and solve waste water from dyestuff, is that China realizes sustainable development and fitness-for-all and to survive a subject under discussion that must face.
Heterogeneous photocatalysis technology can utilize renewable clean solar energy process organic pollution, its course of reaction is simple, rapidly, thoroughly, non-secondary pollution, the selective advantage such as low and receive much concern.In recent years, [the Bi of suitable indirect band gap (about 2.92 eV) novel B iOBr semiconductor
2o
2]
2+layer and Br
–there is electrostatic field and layer structure feature thereof between layer, give the electronic structure of its uniqueness, good optical property and catalytic performance.Such as, Zhang Li in 2008 know the micro-nano spherical BiOBr of professor's report under visible light illumination in photocatalysis water treatment since degradation of organic substances [
j. Phys. Chem. C, 2008,112:747 – 753], the Chinese scholars visible light catalytic performance good to it gives very big concern, Oxford University Jiang Zheng teaches [
j. Photochem. Photobiol. A:Chem., 2010,212:8 – 13], mountain region disaster and Environmental Research Institute Huang Yingping researcher [
environ. Sci. Technol., 2011,45:1593 – 1600], Nankai University [
j. Hazard. Mater., 2011,192:538 – 544], China Environmental Science Research Institute Meng Wei academician [
appl. Catal. B:Environ.2011,107:355 – 362], Hanoverian, Germany university Bahnemann teaches [J. Mol. Catal. A:Chem., 2012,365:1 – 7] etc. BiOBr powder photocatalyst is studied respectively, found that the activity of visible light photocatalytic degradation methyl orange, Microcystin, toluene, tetrabromobisphenol A, azo dyes Recalcitrant chemicals, be all better than commercial photocatalytic agent P25.
But the research about BiOBr photochemical catalyst mainly concentrates on development and the immobilization technology research and development thereof of powder, and has no report about the microemulsion BiOBr photochemical catalyst of high dispersive performance.
Summary of the invention
The present invention aims to provide a kind of microemulsion BiOBr photochemical catalyst, compares other forms of catalyst, can the organic pollution of the effective poisonous and harmful difficult degradation such as methyl orange, phenol, bisphenol-A of trace in mineralized water, and recycling performance is good.Present invention also offers the preparation method of this photochemical catalyst and the application in process organic pollution thereof.
The invention provides a kind of microemulsion BiOBr photochemical catalyst, it is characterized in that: with BiBr
3, Bi (NO
3)
35H
2o or Bi
2o
3any one is bismuth source, and hydrobromic acid is bromine source, and water or ethanol are solvent, and ammoniacal liquor is pH adjusting agent, and calgon is dispersant, utilizes hydrolysis or alcoholysis method obtained microemulsion BiOBr photochemical catalyst at normal temperatures.
The invention provides the preparation method of described microemulsion BiOBr photochemical catalyst, it is characterized in that: comprise the following steps:
1) taking containing bismuth element molal quantity is the bismuth source of 0.1 ~ 1 mmol, joins in the beaker filling 5 ~ 20 mL solvents, and stirring at normal temperature dissolves 1 ~ 4 h, forms solution A;
2) measure the 0.1 mol/L hydrobromic acid solution of 2 ~ 20 mL, be designated as solution B;
3) solution B be added drop-wise to gradually in solution A, keeping dripping speed is 1.5 mL/min, abundant stirring 40 min after titration completes, again by dropping 27% concentrated ammonia liquor, after solution ph is adjusted to 7 ~ 10, make both fully reaction 1 ~ 2 h, obtain suspended catalyst system, be designated as suspension C;
4) take the calgon of 0.001 ~ 0.01 mmol, join in above-mentioned suspended catalyst system, more fully mix through ultrasonic wave, after 1 ~ 2 h that vibrates, the BiOBr photochemical catalyst of microemulsion can be obtained.
In above-mentioned preparation method, described bismuth source is BiBr
3, Bi (NO
3)
35H
2o or Bi
2o
3in any one, the addition of bismuth element is 0.02 ~ 0.4 mol/L solvent.
In above-mentioned preparation method, described solvent is distilled water, alcohol or the mixing of the two; Wherein, the ratio both when distilled water and ethanol use simultaneously is 1:1.
The invention provides the application of described microemulsion BiOBr photocatalyst for degrading organic pollution.Described organic pollution is any one in methyl orange, phenol, bisphenol-A.
The concrete grammar of described microemulsion BiOBr photocatalyst treatment organic pollution is: at normal temperatures and pressures, microemulsion BiOBr photochemical catalyst is used under light source irradiation, consumption is that every 100 mL add 10 ~ 60 mL microemulsion BiOBr photochemical catalysts containing in the solution of organic pollution, and in solution, the concentration of organic pollution is 10 mg/L.
In above-mentioned processing method, described light source be sunshine, simulated solar irradiation, ultraviolet light, visible ray any one.
The present invention takes economic environmental protection, simple water or ethanol solution, with BiBr
3, Bi (NO
3)
35H
2o or Bi
2o
3in any one be bismuth source, hydrobromic acid is bromine source, ammoniacal liquor is pH adjusting agent, calgon is dispersant, successfully obtain microemulsion BiOBr photochemical catalyst at normal temperatures and pressures, not only eliminate centrifugal, washing and the complex operations such as oven dry, reduce its industrialization cost and energy resource consumption, and the catalyst obtained has excellent photocatalysis performance.Sodium hexametaphosphate dispersant plays following three kinds of effects in the solution: the surface tension that 1) effectively can reduce solvent, improves wetability and the dispersion effect thereof of particle surface; 2) formed necessarily coated to BiOBr nano particle in solution, increase particle or intermolecular distance, effectively reduce intermolecular Van der Waals force gravitation, improve its decentralization; 3) charged by dissociation in the solution, and then increase the absolute value of BiOBr nano grain surface current potential, improve electrostatic repulsion energy between particle, form stable dispersion.Therefore by this experimental program, made BiOBr catalyst is present in photocatalysis treatment system with microemulsion form, dispersed high, reproducible, efficiently avoid the intrinsic easy reunion of powder catalyst, poor dispersion, the defect of easily flying upward, not only decrease powder pollution but also ensure the specific area that catalyst is larger, show the feature of approximate catalysis in a homogeneous system, not only improve its photocatalysis performance, and overcome cumbersome process and the active problem reduced that the defect of powder catalyst Separation of Solid and Liquid difficulty in the process of recycling and film catalyst bring.
Of the present invention
beneficial effect:
1, compare with film BiOBr photochemical catalyst with powder, microemulsion BiOBr photochemical catalyst of the present invention has higher photocatalysis performance, preparation process low-temperature environment-friendly, simple, and needed raw material is simple and easy to get, byproduct is nontoxic, easy to use, be convenient to large-scale production;
2, microemulsion BiOBr photochemical catalyst is present in photocatalysis treatment system with emulsus form, dispersed and reproducible, efficiently avoid the intrinsic easy reunion of powder catalyst, poor dispersion, the defect of easily flying upward, not only reduced powder and polluted but also ensure the specific area that catalyst is larger;
3, microemulsion BiOBr photochemical catalyst of the present invention can apply to the process of liquid phase and oily pollutant, the feature of its approximate catalysis in a homogeneous system improves its photocatalysis performance, and overcomes cumbersome process and the active problem reduced thereof that the defect of powder catalyst Separation of Solid and Liquid difficulty in the process of recycling and film catalyst bring;
4, emulsus catalyst is successfully applied to photocatalysis degradation organic contaminant by the invention of microemulsion BiOBr photochemical catalyst, extends the application of such catalyst.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates that embodiment 1 ~ 3 and embodiment 6 obtain microemulsion BiOBr photochemical catalyst.
Fig. 2 is the absorbance change curve that embodiment 6 obtains microemulsion BiOBr photocatalytic degradation bisphenol-A.
detailed description of the invention
Further illustrate the present invention below by embodiment, but be not limited to following examples.
embodiment 1: utilize Hydrolyze method to prepare microemulsion BiOBr photochemical catalyst
Concrete steps are:
1) BiBr of 0.2 mmol is taken
3powder is placed in 5 mL distilled water at normal temperatures, and stirring at normal temperature dissolves 3 h, forms solution A-1;
2) measure 2 mL 0.1 mol/L hydrobromic acid solutions, be designated as solution B-1;
3) solution B-1 be added drop-wise to gradually in solution A-1, keeping dripping speed is 1.5 mL/min, to be titrated complete after abundant stirring 40 min, and drip 27wt% concentrated ammonia liquor, adjust ph is 8, makes both fully after reaction 1 h, obtains solution C-1;
4) take the calgon of 0.0047 mmol, join in above-mentioned solution C-1, more fully mix through ultrasonic wave, after 1 h that vibrates, the BiOBr photochemical catalyst of microemulsion can be obtained, be designated as BiOBr-1.
The microemulsion catalyst B iOBr-1 of above gained is through centrifugal, washing, after oven dry, we have carried out X-ray diffraction to it and have characterized as shown in Figure 1, the diffraction maximum of institute's controlling catalyst is all consistent with the pure tetragonal phase BiOBr standard diagram that JCPDS 09-0393 standard card records, and shows that Kaolinite Preparation of Catalyst is pure BiOBr.
embodiment 2: utilize hydrolysis and alcoholysis method to prepare microemulsion BiOBr photochemical catalyst
Concrete steps are:
1) Bi (NO of 0.4 mmol is taken
3)
35H
2o powder is placed in the mixed solvent of 5 mL water and 5 mL ethanol composition at normal temperatures, and stirring at normal temperature dissolves 4 h, forms solution A-2;
2) measure 4 mL 0.1 mol/L hydrobromic acid solutions, be designated as solution B-2;
3) solution B-2 be added drop-wise to gradually in solution A-2, keeping dripping speed is 1.5 mL/min, to be titrated complete after abundant stirring 40 min, and drip 27wt% concentrated ammonia liquor, adjust ph is 9, makes both fully after reaction 2 h, obtains solution C-2;
4) take the calgon of 0.0094 mmol, join in above-mentioned solution C-2, more fully mix through ultrasonic wave, after 2 h that vibrate, the BiOBr photochemical catalyst of microemulsion can be obtained, be designated as BiOBr-2.
The microemulsion catalyst B iOBr-2 of above gained is through centrifugal, washing, after oven dry, we have carried out X-ray diffraction to it and have characterized as shown in Figure 1, the diffraction maximum of institute's controlling catalyst is all consistent with the pure tetragonal phase BiOBr standard diagram that JCPDS 09-0393 standard card records, and shows that Kaolinite Preparation of Catalyst is pure BiOBr.
embodiment 3: utilize alcoholysis method to prepare microemulsion BiOBr photochemical catalyst
Concrete steps are:
1) Bi of 0.5 mmol is taken
2o
3powder is placed in 10 mL ethanol at normal temperatures, and stirring at normal temperature dissolves 2 h, forms solution A-3;
2) measure 10 mL 0.1 mol/L hydrobromic acid solutions, be designated as solution B-3;
3) solution B-3 be added drop-wise to gradually in solution A-3, keeping dripping speed is 1.5 mL/min, to be titrated complete after abundant stirring 40 min, and drip 27wt% concentrated ammonia liquor, adjust ph is 7, makes both fully after reaction 2 h, obtains solution C-3;
4) take the calgon of 0.0098 mmol, join in above-mentioned solution C-3, more fully mix through ultrasonic wave, after 2 h that vibrate, the BiOBr photochemical catalyst of microemulsion can be obtained, be designated as BiOBr-3.
The microemulsion catalyst B iOBr-3 of above gained is through centrifugal, washing, after oven dry, we have carried out X-ray diffraction to it and have characterized as shown in Figure 1, the diffraction maximum of institute's controlling catalyst is all consistent with the pure tetragonal phase BiOBr standard diagram that JCPDS 09-0393 standard card records, and shows that Kaolinite Preparation of Catalyst is pure BiOBr.
embodiment 4: the application of microemulsion BiOBr photocatalyst for degrading methyl orange solution
1) prepare to treat degradation solution: the methyl orange accurately taking 10 mg respectively, is dissolved in distilled water, and is settled to 1000 mL with volumetric bottle, obtained 10 mg/L treat degradation solution;
2) adopt BiOBr-1, BiOBr-2, BiOBr-3 photochemical catalyst of embodiment 1 ~ 3 gained to carry out photocatalysis treatment three groups respectively and treat degradation solution:
Accurately pipette 100 mL above-mentioned 1 with pipette) treat degradation solution, add BiOBr-1, BiOBr-2, BiOBr-3 catalyst respectively, temperature of reaction system controls at 25 DEG C, to adsorb 1 h under lucifuge condition, to reaching adsorption equilibrium; Then open ultraviolet source, photocatalytic degradation experiment is carried out to methyl orange solution, every 5 min samplings once, utilize UV-VIS spectrophotometry analyze the concentration remaining methyl orange in solution and calculate its degradation rate.
By the solution C-1 in above-described embodiment 1,2,3, C-2, C-3 respectively by centrifugal, washing and drying after obtain powder catalyst corresponding to each preparation method, be designated as powder-1, powder-2, powder-3, carry out contrast test, the results are shown in Table shown in 1.
The BiOBr microemulsion photochemical catalyst that table 1 is preparation and corresponding powder catalyst are to the degradation effect of methyl orange.These show that the photocatalytic activity of no matter which kind of preparation method's gained microemulsion BiOBr is all better than powder catalyst, can reach the degradation effect to methyl orange more than 99% in 30 min.
BiOBr emulsus photochemical catalyst prepared by table 1 and corresponding powder catalyst are to the degradation rate of methyl orange
。
embodiment 5: the application of microemulsion BiOBr photocatalyst for degrading bisphenol-A solution
1) prepare to treat degradation solution: the bisphenol-A accurately taking 10 mg respectively, is dissolved in distilled water, and is settled to 1000 mL with volumetric bottle, obtained 10 mg/L treat degradation solution;
2) adopt BiOBr-1, BiOBr-2, BiOBr-3 photochemical catalyst of embodiment 1 ~ 3 gained to carry out photocatalysis treatment three groups respectively and treat degradation solution:
Accurately pipette 100 mL above-mentioned 1 with pipette) treat degradation solution, add BiOBr-1, BiOBr-2, BiOBr-3 catalyst respectively, temperature of reaction system controls at 25 DEG C, to adsorb 1 h under lucifuge condition, to reaching adsorption equilibrium; Then open simulated solar radiant, photocatalytic degradation experiment is carried out to bisphenol-A solution, every 5 min samplings once, utilize UV-VIS spectrophotometry analyze the concentration remaining bisphenol-A in solution and calculate its degradation rate.
By the solution C-1 in above-described embodiment 1,2,3, C-2, C-3 respectively by centrifugal, washing and drying after obtain powder catalyst corresponding to each preparation method, be designated as powder-1, powder-2, powder-3, carry out contrast test, the results are shown in Table shown in 2.
The BiOBr emulsus photochemical catalyst that table 2 is preparation and corresponding powder catalyst are to the degradation effect of bisphenol-A.These show that the photocatalytic activity of no matter which kind of preparation method's gained microemulsion BiOBr is all better than powder catalyst, can reach the degradation effect to bisphenol-A more than 98% in 30 min.
BiOBr emulsus photochemical catalyst prepared by table 2 and corresponding powder catalyst contrast the degradation rate of bisphenol-A
embodiment 6: microemulsion BiOBr photochemical catalyst preparation method and application
1, the preparation process of photochemical catalyst
1) Bi of 100 mg (about 0.215 mmol) is taken with analytical electron balance
2o
3powder, measures 8 mL ethanol with graduated cylinder and pours small beaker into, at normal temperatures by Bi
2o
3powder stirs 3 h and is dissolved in ethanol, forms solution A;
2) measure 5 mL 0.1 mol/L hydrobromic acid solutions with pipette, put into buret, be designated as solution B;
3) solution B be added drop-wise to gradually in solution A, keeping dripping speed is 1.5 mL/min, to be titrated complete after abundant stirring 40 min, and measure 40 mL 27wt% concentrated ammonia liquors, adjust ph is 8 gradually, makes both fully after reaction 2 h, obtains solution C;
4) take the calgon of 6 mg (about 0.0098 mmol), join in above-mentioned solution C, more fully mix through ultrasonic wave, after 2 h that vibrate, the BiOBr photochemical catalyst of microemulsion can be obtained, be designated as BiOBr.
The microemulsion catalyst B iOBr of above gained is through centrifugal, washing, after oven dry, carry out X-ray diffraction to it to characterize as shown in Figure 1, the diffraction maximum of institute's controlling catalyst is all consistent with the pure tetragonal phase BiOBr standard diagram that JCPDS 09-0393 standard card records, and shows that Kaolinite Preparation of Catalyst is pure BiOBr.
2, Photocatalytic Degradation Process
1) take the bisphenol-A powder of 10 mg with analytical electron balance, be dissolved in 100 mL distilled water, and be settled to 1000 mL with volumetric bottle, obtained 10 mg/L treat degradation solution;
2) by obtained microemulsion BiOBr catalyst and 100 mL, the bisphenol-A solution of 10 mg/L mixes in quartz beaker, and under light protected environment, in thermostat water bath (control temperature is 20 DEG C), stirring a period of time (is generally 1 h), when the concentration of bisphenol-A solution no longer changes, namely show that photochemical catalyst reaches adsorption-desorption balance, now open adjustable type xenon lamp power supply, degradation solution is irradiated with simulated solar irradiation, and regulate quartz beaker to make its light intensity control at 110 klx (10 cm) apart from the distance of light source at every turn, after this then 3 mL degradation solutions are measured every 5 min, carry out centrifugation, and spectrophotometry sign is carried out to its supernatant liquor, until degradation process terminates, obtain degradation product absorbance curve (as shown in Figure 2) over time, the extinction peak of bisphenol-A weakens gradually along with the increase of photocatalysis time as can be seen from Figure 2, almost disappear completely after 30 min, calculate bisphenol-A degradation rate and reach 99.8%, detailed data is shown in Table 3.
The degradation rate of BiOBr emulsus photochemical catalyst to bisphenol-A under simulated solar irradiation irradiates prepared by table 3
。
Claims (8)
1. a microemulsion BiOBr photochemical catalyst, is characterized in that: with BiBr
3, Bi (NO
3)
35H
2o or Bi
2o
3any one is bismuth source, and hydrobromic acid is bromine source, and ammoniacal liquor is pH adjusting agent, and calgon is dispersant, utilizes hydrolysis or alcoholysis method obtained microemulsion BiOBr photochemical catalyst at normal temperatures.
2. a preparation method for microemulsion BiOBr photochemical catalyst according to claim 1, is characterized in that: comprise the following steps:
(1) taking containing bismuth element molal quantity is the bismuth source of 0.1 ~ 1 mmol, joins in the beaker filling 5 ~ 20 mL solvents, and stirring at normal temperature dissolves 1 ~ 4 h, forms solution A;
(2) measure the 0.1 mol/L hydrobromic acid solution of 2 ~ 20 mL, be designated as solution B;
(3) solution B be added drop-wise to gradually in solution A, keeping dripping speed is 1.5 mL/min, abundant stirring 40 min after titration completes, again by dropping 27% concentrated ammonia liquor, after solution ph is adjusted to 7 ~ 10, make both fully reaction 1 ~ 2 h, obtain suspended catalyst system, be designated as suspension C;
(4) take the calgon of 0.001 ~ 0.01 mmol, join in above-mentioned suspended catalyst system, more fully mix through ultrasonic wave, after 1 ~ 2 h that vibrates, namely obtain the BiOBr photochemical catalyst of microemulsion.
3. the preparation method of microemulsion BiOBr photochemical catalyst according to claim 2, is characterized in that: in described step (1), the addition of bismuth element is 0.02 ~ 0.4 mol/L solvent.
4. the preparation method of microemulsion BiOBr photochemical catalyst according to claim 2, is characterized in that: in described step (1), solvent is distilled water, ethanol or the mixing of the two, and wherein, the ratio both when distilled water and ethanol use simultaneously is 1:1.
5. the application of a microemulsion BiOBr photocatalyst for degrading organic pollution according to claim 1.
6. application according to claim 5, is characterized in that: described organic pollution is any one in methyl orange, phenol, bisphenol-A.
7. application according to claim 5, it is characterized in that: concrete grammar is: at normal temperatures and pressures, microemulsion BiOBr photochemical catalyst is used under light source irradiation, consumption is that every 100 mL add 10 ~ 60 mL microemulsion BiOBr photochemical catalysts containing in the solution of organic pollution, and in solution, the concentration of organic pollution is 10 mg/L.
8. application according to claim 7, is characterized in that: described light source be sunshine, simulated solar irradiation, ultraviolet light, visible ray any one.
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| CN109772378A (en) * | 2019-03-28 | 2019-05-21 | 西南大学 | Method for preparing highly active Fe doping BiOX light fenton catalyst and products thereof and application |
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| CN114377698A (en) * | 2022-01-18 | 2022-04-22 | 中国科学技术大学 | Bismuth oxybromide composite material, preparation method, photocatalytic decontamination agent based on bismuth oxybromide composite material and application of photocatalytic decontamination agent |
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| CN106607063A (en) * | 2015-10-27 | 2017-05-03 | 湖南城市学院 | Floating visible-light-induced photocatalyst, and preparation method and application thereof |
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| CN109772378A (en) * | 2019-03-28 | 2019-05-21 | 西南大学 | Method for preparing highly active Fe doping BiOX light fenton catalyst and products thereof and application |
| CN110422905A (en) * | 2019-09-05 | 2019-11-08 | 太原师范学院 | A method of BiOCl catalytic eliminating bisphenol-A is loaded using coke |
| CN110422905B (en) * | 2019-09-05 | 2021-07-23 | 太原师范学院 | Method for removing bisphenol A by coke-loaded BiOCl catalysis |
| CN112588309A (en) * | 2020-12-30 | 2021-04-02 | 四川大学 | P-doped BiOCl visible-light-driven photocatalyst and preparation method thereof |
| CN114377698A (en) * | 2022-01-18 | 2022-04-22 | 中国科学技术大学 | Bismuth oxybromide composite material, preparation method, photocatalytic decontamination agent based on bismuth oxybromide composite material and application of photocatalytic decontamination agent |
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