CN104646037A - BiOXs pholocatalyst, grapheme-compounded BiOXs pholocatalyst and preparation method thereof - Google Patents
BiOXs pholocatalyst, grapheme-compounded BiOXs pholocatalyst and preparation method thereof Download PDFInfo
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- CN104646037A CN104646037A CN201510013143.0A CN201510013143A CN104646037A CN 104646037 A CN104646037 A CN 104646037A CN 201510013143 A CN201510013143 A CN 201510013143A CN 104646037 A CN104646037 A CN 104646037A
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Abstract
The invention relates to a BiOXs pholocatalyst, a grapheme-compounded BiOXs pholocatalyst and a preparation method thereof and relates to the field of photocatalytic materials. According to the invention, the BiOXs pholocatalyst is prepared by utilizing a solvent thermal method, so that the BiOXs pholocatalyst has excellent photocatalytic performances and is especially capable of efficiently degrading organic pollutants under visible light. Photocatalytic performances of the BiOXs pholocatalyst can be further improved by compounding with grapheme in-situ. The BiOXs pholocatalyst, the grapheme-compounded BiOXs pholocatalyst and the preparation method have the advantages of simple manufacturing process, simplicity in operation, low manufacturing cost, small pollution and one-step compounding process.
Description
Technical field
The invention belongs to field of photocatalytic material, be specifically related to BiOXs photochemical catalyst, also relate to the preparation method of above-mentioned catalyst.
Background technology
Photocatalysis oxidation technique directly converts solar energy into chemical energy and electric energy by conductor photocatalysis material, and by organic pollution permineralization degraded poisonous and hazardous in environment, be considered to solve one of the human society energy and the potential technical scheme of environmental problem most at present.At present, the principal element restricting photocatalysis technology development has that the utilization rate of sunshine is low, electron-hole pair recombination rate is high, photo-quantum efficiency is low.Due to traditional titanium dioxide (TiO
2) photochemical catalyst has wide energy gap (as the TiO of rutile
2for 3.0eV, the TiO of anatase
2for 3.2eV) and make it can only have response to the ultraviolet light of be less than sunshine 5%.In order to make full use of solar energy, building the structure with low energy gap width excited by visible light and having great importance.
In recent years, BiOX BiOXs (X=Cl, Br, I) was not only cheaply easy to get as a kind of novel photochemical catalyst, stable performance, activity is good, preparation condition is simply gentle, and with traditional photochemical catalyst P
25(TiO
2nano particle) to compare, the open layer structure of its uniqueness is more conducive to effective separation and the Charger transfer of electron-hole pair, thus makes it have better photocatalytic activity and stability.Therefore pay close attention to greatly because BiOXs receives researchers to the strong absorption of visible ray and excellent photocatalysis performance.The change of preparation condition can cause the change of material structure, and then can affect its photocatalysis performance.
In addition, SP
2the special construction that the carbon atom of hydridization connects imparts the high electron mobility of Graphene [25], by Graphene and semiconductors coupling, light induced electron can be made to be quickly transferred to its surface, realize effective separation of photo-generate electron-hole, and the light absorption range of semiconductor can be widened thus improve light-catalyzed reaction efficiency.
Summary of the invention
The object of the present invention is to provide BiOXs photochemical catalyst and their preparation method of BiOXs photochemical catalyst that a kind of degradation capability is under visible light strong, Graphene compound.
The preparation method of the BiOXs photochemical catalyst of BiOXs and Graphene compound, preparation process is as follows:
(1) ethylene glycol of volume ratio (1-4:1) and glacial acetic acid are made into the solution of 40ml, and the bismuth nitrate of 0.005-0.008mol are put into above-mentioned solution, magnetic agitation 0.5-1 hour, make it fully dissolve.
(2) absolute ethyl alcohol of volume ratio (1-4:1) and deionized water are made into the solution of 40ml, and by a certain amount of NaX (X=Cl, Br or I, the mol ratio of X and Bi is 1:1) put into above-mentioned solution, magnetic agitation 0.5-1 hour, make it fully dissolve.
(3) solution prepared by step (2) is slowly added drop-wise in the solution of the continuous stirring of preparing by step (1), after dripping, continue to stir 0.5-1 hour, then mixed liquor is transferred in 100ml teflon-lined stainless steel cauldron, 80-180 DEG C of reaction 10 minutes-24 hours, after reaction terminates, sediment is filtered, with deionized water and absolute ethanol washing three times, finally put into the baking oven of 80 DEG C, vacuum drying 8h.Grind into powder, obtains sample.Sample composition can comprise BiOCl
1-mbr
m, BiOCl
1-mi
mand BiOBr
1-mi
m, wherein 0≤m≤1, or three halogens, BiOC1
abr
bi
1-a-b, wherein 0<a<1,0<b<1, a+b<1) BiOXs photochemical catalyst.
(4) the BiOXs photochemical catalyst of Graphene compound is prepared: the solution absolute ethyl alcohol of volume ratio (1:1-4) and deionized water being made into 40ml, then will be that the Graphene ultrasonic disperse of 0.5-5% is in above-mentioned solution with BiOXs mass ratio, and a certain amount of sodium halide (mol ratio of X and Bi is 1:1) is put into above-mentioned solution, magnetic agitation 0.5-1 hour, makes it fully dissolve.Subsequent step is identical with (3), can obtain the photochemical catalyst of the BiOXs of Graphene compound.
(5) the photocatalysis performance test of the BiOXs of above-mentioned preparation or the BiOXs photochemical catalyst of Graphene compound: RhB solution 20mg photochemical catalyst being put into 100mL15mg/L, first carry out the dark adsorption of 10min, to adsorption equilibrium, 4mL is taken out as sample every 10min in dark adsorption process, centrifugation, after having adsorbed, light-catalyzed reaction is carried out under the xenon lamp of 300W irradiates, when carrying out visible light photocatalysis reaction, adopt the optical filter of 400nm cut to be filtered by the ultraviolet portion in xenon lamp to remove, in photocatalytic process, RhB4mL is taken out as sample every 10min, centrifugation, the concentration of rear derived sample and the concentration of initial sample have been adsorbed in test.Wherein, the present invention adopts 20mg photochemical catalyst to put into the RhB solution of 100mL15mg/L, much smaller compared with other document consumption.
Beneficial effect of the present invention: production technology of the present invention is simple, easy and simple to handle, production cost is low, it is little to pollute, recombination process one step completes, and the photochemical catalyst of preparation has degradation effect fast to organic pollution under visible light.
Below in conjunction with specific embodiment, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of BiOBr and BiOCl;
Fig. 2 is different photochemical catalyst degraded figure under visible light;
Fig. 3 is the BiOXs degraded figure under visible light of BiOXs and Graphene compound;
Fig. 4 is the degraded figure (i.e. partial enlarged drawing) of Fig. 3 at 10-50min.
Detailed description of the invention
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
Embodiment 1:
The bismuth nitrate of 0.005mol is put into the ethylene glycol that 40ml volume ratio is 2:1 and glacial acetic acid solution, and magnetic agitation 0.5 hour, makes it fully dissolve, obtains solution A.Then added in the absolute ethyl alcohol and deionized water solution that 40ml volume ratio is 2:1 by 0.005molNaBr (also can with KBr), magnetic agitation 0.5 hour, makes it fully dissolve, obtains B solution.Subsequently B solution is slowly added drop-wise in the solution A constantly stirred, after dripping, continue stirring 0.5 hour, then mixed liquor is transferred in 100ml teflon-lined stainless steel cauldron, 110 DEG C of reactions 10 hours, after reaction terminates, sediment is filtered, with deionized water and absolute ethanol washing three times, finally put into the baking oven of 80 DEG C, vacuum drying 8h.Grind into powder, obtains sample, and its chemical composition is BiOBr.
Photocatalysis performance is tested: the RhB solution of 100mL15mg/L put into by the photochemical catalyst prepared by 20mg, first carry out the dark adsorption of 10min, to adsorption equilibrium, 4mL is taken out as sample every 10min in dark adsorption process, centrifugation, after having adsorbed, light-catalyzed reaction is carried out under the xenon lamp of 300W irradiates, when carrying out visible light photocatalysis reaction, adopt the optical filter of 400nm cut to be filtered by the ultraviolet portion in xenon lamp to remove, in photocatalytic process, RhB4mL is taken out as sample every 10min, centrifugation, the concentration of rear derived sample and the concentration of initial sample have been adsorbed in test.
Embodiment 2:
The bismuth nitrate of 0.008mol is put into the ethylene glycol that 40ml volume ratio is 3:1 and glacial acetic acid solution, and magnetic agitation 1 hour, makes it fully dissolve, obtains solution A.Then added by 0.006molNaCl and 0.002molNaBr in the absolute ethyl alcohol that 40ml volume ratio is 3:1 and deionized water solution, magnetic agitation 1 hour, makes it fully dissolve, obtains B solution.Subsequently B solution is slowly added drop-wise in the solution A constantly stirred, after dripping, continue stirring 0.5 hour, then mixed liquor is transferred in 100ml teflon-lined stainless steel cauldron, 120 DEG C of reactions 12 hours, after reaction terminates, sediment is filtered, with deionized water and absolute ethanol washing three times, finally put into the baking oven of 80 DEG C, vacuum drying 8h.Grind into powder, obtains sample, and its chemical composition is BiOCl
0.75br
0.25.
Photocatalysis performance is tested: the RhB solution of 100mL15mg/L put into by the photochemical catalyst prepared by 20mg, first carry out the dark adsorption of 10min, to adsorption equilibrium, 4mL is taken out as sample every 10min in dark adsorption process, centrifugation, after having adsorbed, light-catalyzed reaction is carried out under the xenon lamp of 300W irradiates, when carrying out visible light photocatalysis reaction, adopt the optical filter of 400nm cut to be filtered by the ultraviolet portion in xenon lamp to remove, in photocatalytic process, RhB4mL is taken out as sample every 10min, centrifugation, the concentration of rear derived sample and the concentration of initial sample have been adsorbed in test.
Embodiment 3:
The bismuth nitrate of 0.006mol is put into the ethylene glycol that 40ml volume ratio is 1:1 and glacial acetic acid solution, and magnetic agitation 1 hour, makes it fully dissolve, obtains solution A.Then added by 0.006molNaCl in the absolute ethyl alcohol that 40ml volume ratio is 1:1 and deionized water solution, magnetic agitation 1 hour, makes it fully dissolve, obtains B solution.Subsequently B solution is slowly added drop-wise in the solution A constantly stirred, after dripping, continue stirring 0.5 hour, then mixed liquor is transferred in 100ml teflon-lined stainless steel cauldron, 120 DEG C of reactions 12 hours, after reaction terminates, sediment is filtered, with deionized water and absolute ethanol washing three times, finally put into the baking oven of 80 DEG C, vacuum drying 8h.Grind into powder, obtains sample, and its chemical composition is BiOCl.
Photocatalysis performance is tested: the RhB solution of 100mL15mg/L put into by the photochemical catalyst prepared by 20mg, first carry out the dark adsorption of 10min, to adsorption equilibrium, 4mL is taken out as sample every 10min in dark adsorption process, centrifugation, after having adsorbed, light-catalyzed reaction is carried out under the xenon lamp of 300W irradiates, when carrying out visible light photocatalysis reaction, adopt the optical filter of 400nm cut to be filtered by the ultraviolet portion in xenon lamp to remove, in photocatalytic process, RhB4mL is taken out as sample every 10min, centrifugation, the concentration of rear derived sample and the concentration of initial sample have been adsorbed in test.
Embodiment 4:
The bismuth nitrate of 0.005mol is put into the ethylene glycol that 40ml volume ratio is 1:1 and glacial acetic acid solution, and magnetic agitation 1 hour, makes it fully dissolve, obtains solution A.Then 0.003molNaCl, 0.001molNaBr and 0.001molNaI are added in the absolute ethyl alcohol that 40ml volume ratio is 1:1 and deionized water solution, magnetic agitation 1 hour, makes it fully dissolve, obtains B solution.Subsequently B solution is slowly added drop-wise in the solution A constantly stirred, after dripping, continue stirring 0.5 hour, then mixed liquor is transferred in 100ml teflon-lined stainless steel cauldron, 100 DEG C of reactions 15 hours, after reaction terminates, sediment is filtered, with deionized water and absolute ethanol washing three times, finally put into the baking oven of 80 DEG C, vacuum drying 8h.Grind into powder, obtains sample, and its chemical composition is BiOCl
0.6br
0.2i
0.2.
Photocatalysis performance is tested: the RhB solution of 100mL15mg/L put into by the photochemical catalyst prepared by 20mg, first carry out the dark adsorption of 10min, to adsorption equilibrium, 4mL is taken out as sample every 10min in dark adsorption process, centrifugation, after having adsorbed, light-catalyzed reaction is carried out under the xenon lamp of 300W irradiates, when carrying out visible light photocatalysis reaction, adopt the optical filter of 400nm cut to be filtered by the ultraviolet portion in xenon lamp to remove, in photocatalytic process, RhB4mL is taken out as sample every 10min, centrifugation, the concentration of rear derived sample and the concentration of initial sample have been adsorbed in test.
Embodiment 5:
The bismuth nitrate of 0.006mol is put into the ethylene glycol that 40ml volume ratio is 1:1 and glacial acetic acid solution, and magnetic agitation 1 hour, makes it fully dissolve, obtains solution A.Then by 15.6mg Graphene ultrasonic disperse in 40ml volume ratio is the absolute ethyl alcohol of 1:1 and deionized water solution, add 0.006molNaCl subsequently, magnetic agitation 1 hour, makes it fully dissolve, obtains B solution.Subsequently B solution is slowly added drop-wise in the solution A constantly stirred, after dripping, continue stirring 0.5 hour, then mixed liquor is transferred in 100ml teflon-lined stainless steel cauldron, 120 DEG C of reactions 12 hours, after reaction terminates, sediment is filtered, with deionized water and absolute ethanol washing three times, finally put into the baking oven of 80 DEG C, vacuum drying 8h.Grind into powder, obtains the sample of Graphene compound, and its chemical composition is BiOCl-GR.
Photocatalysis performance is tested: the RhB solution of 100mL15mg/L put into by the photochemical catalyst prepared by 20mg, first carry out the dark adsorption of 10min, to adsorption equilibrium, 4mL is taken out as sample every 10min in dark adsorption process, centrifugation, after having adsorbed, light-catalyzed reaction is carried out under the xenon lamp of 300W irradiates, when carrying out visible light photocatalysis reaction, adopt the optical filter of 400nm cut to be filtered by the ultraviolet portion in xenon lamp to remove, in photocatalytic process, RhB4mL is taken out as sample every 10min, centrifugation, the concentration of rear derived sample and the concentration of initial sample have been adsorbed in test.
Embodiment 6
Fig. 1 is the XRD spectra of the BiOBr of embodiment 1 synthesis and the BiOCl sample of embodiment 3 synthesis, from peak position, article two, each peak of spectrogram all one_to_one corresponding pure phase BiOCl (JCPDS no.73-2060) and BiOBr (JCPDSno.73-2061) PDF cards, in figure, diffraction maximum peak shape is sharp-pointed, illustrates that product crystal property is good.
Fig. 2 is different photochemical catalyst degraded figure under visible light, as can be seen from Figure, and the traditional photochemical catalyst TiO prepared by sol-gel process
2to be only 12%, EG-BiOBr obtained under pure ethylene glycol solution for the degradation rate of 50min to RhB under visible light, and other conditions are identical with embodiment 1, and each degradation curve contrast can obtain the BiOBr that embodiment 1 obtains and have good catalytic performance.
Fig. 3 is the BiOXs degraded figure under visible light of BiOXs and Graphene compound, Fig. 4 is the degraded figure of Fig. 3 at 10-50min.Can be found out by Fig. 3 and Fig. 4, adopt the catalyst of this invention preparation to have efficient catalytic performance to RhB all under visible light, the catalytic efficiency of all kinds of catalyst to RhB dye molecule is followed successively by from high to low: embodiment 5> embodiment 4> embodiment 3> embodiment 2> embodiment 1.Especially embodiment 3,4,5 reaches more than 90% at 20min degradation rate.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (10)
1. a BiOXs photochemical catalyst, is characterized in that it is BiOCl
1-mbr
m, BiOCl
1-mi
m, BiOBr
1-mi
mor BiOC1
abr
bi
1-a-b, wherein 0≤m≤1; 0<a<1,0<b<1, a+b<1; And it adopts solvent-thermal method to be prepared from, wherein, bismuth salt is dissolved in the mixed solvent of ethylene glycol and glacial acetic acid, halogen is dissolved in the mixed solvent of absolute ethyl alcohol and deionized water.
2. BiOXs photochemical catalyst as claimed in claim 1, is characterized in that the volume ratio of ethylene glycol and glacial acetic acid is 1-4:1; The volume ratio of absolute ethyl alcohol and deionized water is 1-4:1.
3. BiOXs photochemical catalyst as claimed in claim 1 or 2, when it is characterized in that preparation, is added drop-wise in bismuth salting liquid by halide salt solution; Wherein, bismuth salt is bismuth nitrate, and halogen is sodium halide or potassium halide.
4. a BiOXs photochemical catalyst for Graphene compound, is characterized in that BiOXs is BiOCl
1-mbr
m, BiOCl
1-mi
m, BiOBr
1-mi
mor BiOC1
abr
bi
1-a-b, wherein 0≤m≤1; 0<a<1,0<b<1, a+b<1;
It adopts solvent-thermal method to be prepared from, and wherein, bismuth salt is dissolved in the mixed solvent of ethylene glycol and glacial acetic acid, and Graphene and halogen are dissolved in the mixed solvent of absolute ethyl alcohol and deionized water;
The mass ratio of Graphene and BiOXs is 0.5-5%.
5. the BiOXs photochemical catalyst of Graphene compound as claimed in claim 4, is characterized in that the volume ratio of ethylene glycol and glacial acetic acid is 1-4:1; The volume ratio of absolute ethyl alcohol and deionized water is 1-4:1.
6. the BiOXs photochemical catalyst of the Graphene compound as described in claim 4 or 5, when it is characterized in that preparation, is added drop-wise to Graphene and halide salt solution in bismuth salting liquid; Wherein, bismuth salt is bismuth nitrate, and halogen is sodium halide or potassium halide.
7. a preparation method for BiOXs photochemical catalyst, it is characterized in that adopting solvent-thermal method to be prepared from, wherein, bismuth salt is dissolved in the mixed solvent of ethylene glycol and glacial acetic acid, and halogen is dissolved in the mixed solvent of absolute ethyl alcohol and deionized water; Gained BiOXs is BiOCl
1-mbr
m, BiOCl
1-mi
m, BiOBr
1-mi
mor BiOC1
abr
bi
1-a-b, wherein 0≤m≤1; 0<a<1,0<b<1, a+b<1.
8. the preparation method of BiOXs photochemical catalyst as claimed in claim 7, is characterized in that the volume ratio of ethylene glycol and glacial acetic acid is 1-4:1; The volume ratio of absolute ethyl alcohol and deionized water is 1-4:1.
9. the preparation method of the BiOXs photochemical catalyst as described in any one of claim 7-9, when it is characterized in that preparation, is added drop-wise in bismuth salting liquid by halide salt solution; Wherein, bismuth salt is bismuth nitrate, and halogen is sodium halide or potassium halide.
10. the preparation method of the BiOXs photochemical catalyst of the Graphene compound as described in any one of claim 4-6, it is characterized in that adopting solvent-thermal method to be prepared from, wherein, bismuth salt is dissolved in the mixed solvent of ethylene glycol and glacial acetic acid, and Graphene and halogen are dissolved in the mixed solvent of absolute ethyl alcohol and deionized water; Gained BiOXs is BiOCl
1-mbr
m, BiOCl
1-mi
m, BiOBr
1-mi
mor BiOC1
abr
bi
1-a-b, wherein 0≤m≤1; 0<a<1,0<b<1, a+b<1; The mass ratio of Graphene and BiOXs is 0.5-5%.
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| CN111822055A (en) * | 2020-07-25 | 2020-10-27 | 合肥学院 | Preparation method and application of BiOBr/COF composite photocatalyst |
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Application publication date: 20150527 |