CN104069876A - Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method - Google Patents
Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on [001] crystal face of BiOCl nanometer sheet and method Download PDFInfo
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Abstract
The invention discloses an Ag-BiOCl compound photocatalyst prepared by depositing nanometer silver on the [001] crystal face of a BiOCl nanometer sheet and a method. The Ag-BiOCl compound photocatalyst comprises a BiOCl nanometer sheet with a thickness of 500 nm-1 mu m and nanometer silver attached on the [001] face of a BiOCl monocrystal nanometer sheet, wherein the particle size of the nanometer silver is 100-200 nm. The preparation method comprises the following steps: (1) preparing the BiOCl monocrystal nanometer sheet (SCNSs) with an exposed [001] face; and (2) dispersing the BiOCl monocrystal nanometer sheet (SCNSs) with the exposed [001] face, prepared in the step (1), in a polyhydroxy-alcohol non-aqueous solvent to obtain a dispersion liquid, then adding AgNO3 in the dispersion liquid, uniformly mixing and then performing microwave treatment at the temperature of 130-180 DEG C for 7-15min to obtain the Ag-BiOCl compound photocatalyst. The Ag-BiOCl compound photocatalyst is high in visible light response activity and good in catalytic activity.
Description
Technical field
The invention belongs to catalyst technical field, relate to a kind of BiOCl nanometer sheet { Ag-BiOCl composite photo-catalyst and method thereof that 001} crystal face selection depositing nano silvery is standby.
Background technology
Since the seventies in last century, the toxic organic pollutant in photocatalytic degradation environment causes environmentalists' extensive concern gradually because of the environmental problem that it provides a kind of environmentally friendly approach to solve facing mankind.Originally, TiO
2because its photocatalytic activity is high, stable chemical nature, non-secondary pollution, the advantage such as cheap and easy to get, be widely used in the toxic organic pollutant in photocatalytic degradation environment.Yet, TiO
2energy gap is wider, can only be excited by the ultraviolet light in sunshine, and to accounting for the not response of visible ray that the wavelength of solar energy 45-50% is 400-750nm, this has limited TiO
2effective application of photocatalyst.Material scholars are to TiO subsequently
2adulterate, form with TiO
2for the dopant material of matrix is as heterogeneous photocatalyst, based on consequent cooperative effect to improve TiO
2the visible light catalysis activity of sill.But, TiO
2quito phase catalysis material is at high temperature calcined or needs a lot of reactions steps at doping process need, and often needs expensive ion implantation equipment, and this has limited its commercial Application potentiality greatly.
Another thinking of research photochemical catalyst is that development and Design goes out the novel not single-phase oxidation photocatalyst of doping and can under visible ray, be excited, as BiOX, X=Cl, Br, the I anisotropic layer structure of height that especially chlorine oxygen bismuth (BiOCl) has based on it is convenient to the separation at light induced electron acupuncture point and is had stable photocatalytic activity, thereby has caused relevant scholar's concern.But (~3.0eV) is wider for the energy gap of BiOCl, limited equally its utilization to visible ray.Also there are recently bibliographical information [Hong, Deng; Yadong Li, Chem.Eur.J.2005,11,6519-6524] by the pH value of simple adjusting five water bismuth nitrates and cetyl chloride ammonium mixed liquor, then at 160-180 ℃ of temperature, hydro-thermal 12 can obtain the different single-phase Bi that measure ratios to 24 hours
24o
31cl
10increase gradually along with pH, the color of product has become yellow gradually from white, and the UV Diffuse Reflectance Spectroscopy of product also shows that its absorption maximum edge is moving to visible region gradually, and these all illustrate that its strengthens being absorbed in gradually of visible ray.In addition, [Zhang Li knows etc. for we, Chinese invention patent, application publication number: CN102553620A once adopted inorganic salts potassium chloride to substitute cetyl chloride ammonium as chlorine source, by NaOH, regulate pH value to 12.5~13 of reaction solution, then at the temperature of 160 ℃, hydro-thermal synthesizes a kind of Bi1 of brand-new metering ratio for 24 hours
2o
17cl
2single-phase visible light catalyst.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of BiOCl nanometer sheet { Ag-BiOCl composite photo-catalyst and method thereof that 001} crystal face depositing nano silvery is standby.This silver-chlorine oxygen bismuth (Ag-BiOCl) composite photo-catalyst visible light response activity is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Ag-BiOCl composite photo-catalyst, it is the BiOCl nanometer sheet of 500nm~1 μ m by thickness and is attached to BiOCl single crystal nanoplate { Nano Silver of 001} face forms, and the particle diameter of described Nano Silver is 100~200nm.
Above-mentioned BiOCl nanometer sheet 001} crystal face depositing nano silvery is for the method for Ag-BiOCl composite photo-catalyst, and its step is as follows:
(1) preparation { the BiOCl single crystal nanoplate (SCNSs) that 001} face exposes: bismuth salt and villaumite are added to the water to dissolving, constantly stir simultaneously, regulate pH to 0.5~2, then 200~240 ℃ of hydrothermal treatment consists 18~30 hours in hydrothermal reaction kettle, post processing obtains { the BiOCl single crystal nanoplate that 001} face exposes, wherein: bismuth salt is in bismuth, and villaumite is in chlorine, and both mol ratios are 1:1;
(2) prepare Ag-BiOCl composite photo-catalyst: { the BiOCl single crystal nanoplate that 001} face exposes is scattered in polyhydroxy-alcohol nonaqueous solvents, obtains its dispersion liquid, then add AgNO in described dispersion liquid by step (1) gained
3, 130~180 ℃ of radiation 7~15 minutes in microwave reaction system after mixing, post processing obtains Ag-BiOCl composite photo-catalyst.
Press such scheme, the bismuth salt in described step (1) is five water bismuth nitrates, and described villaumite is potassium chloride.
Press such scheme, in the aqueous solution of described step (1), the amount of substance concentration of bismuth salt and villaumite is 0.06~0.065mol/L.
Press such scheme, the post processing of described step (1) is for being cooled to room temperature, and washing, is dried and obtains { the BiOCl single crystal nanoplate that 001} face exposes.
Press such scheme, in described step (1), pH adjusting is NaOH solution with conditioning agent.
Press such scheme, the reactor in described step (1) is Teflon reactor.
Press such scheme, AgNO in described step (2)
3in the quality of Ag, account for the 3-6% of BiOCl nanometer monocrystalline tablet quality.
Press such scheme, the polyhydroxy-alcohol nonaqueous solvents in described step (2) includes but not limited to ethylene glycol, polyethylene glycol.
Press such scheme, the ratio of the quality of described step (2) BiOCl single crystal nanoplate and the volume of polyhydroxy-alcohol nonaqueous solvents is 0.004~0.006g/mL.
Press such scheme, the described post processing of step (2) is: be cooled to room temperature, with absolute ethanol washing for several times, in 60 ℃ of vacuum drying 12h.
Beneficial effect of the present invention:
1. Ag-BiOCl composite photo-catalyst visible light response activity provided by the invention is high.The visible light activity of its reduction of hexavalent chromium and oxidation penta sodium pentachlorophenate is far away higher than the non-selective deposition Ag-BiOCl composite photo-catalyst that utilizes sodium borohydride electronation to prepare.
2. the present invention first prepares { the BiOCl single crystal nanoplate that 001} face exposes through hydro-thermal reaction, then BiOCl single crystal nanoplate is scattered in to microwave treatment in polyhydroxy-alcohol nonaqueous solvents, in BiOCl nanometer sheet, { 001} crystal face forms oxygen room to microwave action energy polyhydroxy-alcohol nonaqueous solvents fast, and generated in-situ oxygen room reduction silver ion can have been realized the selective deposition of Nano Silver.3. a building-up process is all carried out in reactor, and technical process is very easy to operation, and industrial amplification factor is little, and raw material is easy to get, and cost is low, and productive rate is higher, the needs of very realistic production.
Accompanying drawing explanation
Fig. 1 is the BiOCl nanometer sheet of the embodiment of the present invention 1 and the XPS collection of illustrative plates of Ag-BiOCl composite photo-catalyst;
Fig. 2 is the BiOCl nanometer sheet of embodiment 1 and the XRD collection of illustrative plates of Ag-BiOCl composite photo-catalyst;
Fig. 3 is SEM figure and the HRTEM collection of illustrative plates of the BiOCl of embodiment 1;
Fig. 4 is the SEM figure of the Ag-BiOCl composite photo-catalyst of embodiment 1;
Fig. 5 is the elemental composition analysis chart of the Ag-BiOCl composite photo-catalyst of embodiment 1;
Fig. 6 is the UV Diffuse Reflectance Spectroscopy of the Ag-BiOCl composite photo-catalyst of embodiment 1;
Fig. 7 is Ag-BiOCl the composite photo-catalyst reduction of hexavalent chromium and the curve map that is oxidized penta sodium pentachlorophenate under radiation of visible light of embodiment 1.
The specific embodiment
For making those skilled in the art understand better technical scheme of the present invention, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
Step (1): bismuth salt and villaumite are dissolved in stirring in 16mL water obtain the aqueous solution that bismuth salt and villaumite concentration are 0.0625mol/L, with the NaOH aqueous solution of 1mol/L, regulating the pH value of the aqueous solution is 1, then in 25mL Teflon reactor, is heated to 220 ℃ and be incubated hydrothermal treatment consists 24h; Be cooled to after room temperature centrifugally, and by gained solid product with distilled water and ethanol washing for several times, drier at 60 ℃, obtain { the BiOCl nanometer sheet (being labeled as BOC-001) that 001} face exposes;
Step (2): get the above-mentioned preparation of 0.1g { 001}BiOCl nanometer sheet is scattered in 20mL ethylene glycol solution, adds 0.0079g AgNO
3, mix.Gained mixed liquor is microwave irradiation 10min in the time of 160 ℃, makes Ag-BiOCl composite photo-catalyst (being labeled as Ag-BOC-001).
Fig. 1 is shown in by the XPS of BiOCl nanometer sheet and Ag-BiOCl composite photo-catalyst (x-ray photoelectron power spectrum) collection of illustrative plates: the high-resolution Bi that Fig. 1 a is sample
4fcollection of illustrative plates, in conjunction with can for 165.6 and 160.2eV place there is BiOCl in Bi
3+characteristic peak, corresponding to Bi
3+bi
4f7/2and Bi
4f5/2, and after BiOCl surface deposition Ag, there is not the skew at peak; Fig. 1 b is the high-resolution Ag of Ag-BiOCl
3dcollection of illustrative plates, in conjunction with can for 368.2 and a pair of peak that occurs of 374.1eV corresponding to the Ag of metal A g
3d5/2and Ag
3d3/2, the deposition that has metal A g on BiOCl is described.Fig. 2 is shown in by XRD collection of illustrative plates, as can be seen from Figure 2: XRD collection of illustrative plates and the BiOCl sample of Ag-BiOCl sample are basically identical, but be 38.2 ° in angle of diffraction, located to occur the characteristic diffraction peak of weak metal A g.SEM figure and HRTEM (high-resolution transmission electron microscope) figure of BiOCl are shown in Fig. 3, and Fig. 3 shows: it is { 001} crystal face, and the decahedron structure that sample is 500nm-1 μ m rule by thickness forms that BiOCl sample prepared by this method exposes crystal face.The SEM spectrogram of Ag-BiOCl composite photo-catalyst is shown in Fig. 4, and constituent analysis figure is shown in Fig. 5, and Fig. 4 and Fig. 5 show: this Ag-BiOCl compound by the Nano Silver of 100-200nm be attached to BiOCl monocrystalline micro-nano thin slice { 001} face forms.
The UV Diffuse Reflectance Spectroscopy figure (DRS) of Ag-BiOCl composite photo-catalyst is shown in Fig. 6, and as can be seen from Figure 6, prepared Ag-BiOCl composite photo-catalyst has very strong absorption from ultraviolet region to visible region, and visible region absorption maximum is at 531nm.
Ag-BiOCl composite photo-catalyst prepared by the present embodiment is for being oxidized the catalytic treatment of penta sodium pentachlorophenate and reduction of hexavalent chromium, 500W xenon lamp is light source (upper sea blue bright XQ500W), at one, carry out in the Photoreactor of glass condensation sleeve pipe, and be furnished with 420nm optical filter.Concrete grammar is: it is in 10mg/L penta sodium pentachlorophenate or Cr VI solution that 0.05g catalyst is joined to 50mL concentration, after system reaches adsorption-desorption poised state, starts illumination.Every 1h sampling 5mL, after centrifugal sedimentation, get the variation (ultraviolet-visible spectrophotometer, HITACHI U-3310) that supernatant liquor is measured uv-visible absorption spectra.According to remaining penta sodium pentachlorophenate in solution or chromic amount, determine the situation of carrying out of light-catalyzed reaction.Separately get 0.1g BOC-001 and be scattered in 20mL deionized water, add wherein 0.0079g AgNO
3, mix, under magnetic agitation effect, by stoichiometry, in solution, dropwise add 0.01mol/L NaBH
4solution, in the dark react centrifugal after 2h, and by distilled water and ethanol washing several for gained solid product, dry at 60 ℃ again, obtain non-selective deposition Ag/BiOCl composite photo-catalyst (being labeled as Ag/BOC), itself and BOC-001 are done respectively ratio, and under radiation of visible light, the design sketch of reduction of hexavalent chromium and oxidation penta sodium pentachlorophenate is shown in Fig. 7.As seen from Figure 7, the visible light activity that the prepared Ag-BiOCl composite photo-catalyst of the present invention is oxidized penta sodium pentachlorophenate and reduction of hexavalent chromium is far away higher than the non-selective deposition Ag/BiOCl composite photo-catalyst that utilizes sodium borohydride electronation to prepare.
Embodiment 2
Step (1): bismuth salt and villaumite are dissolved in stirring in 16mL water obtain the aqueous solution that bismuth salt and villaumite concentration are 0.0625mol/L, with the NaOH aqueous solution of 1mol/L, regulating the pH value of the aqueous solution is 0.5, then in 25mL Teflon reactor, is heated to 200 ℃ and be incubated hydrothermal treatment consists 24h; Be cooled to after room temperature centrifugally, and by gained solid product with distilled water and ethanol washing for several times, drier at 60 ℃, obtain { the BiOCl nanometer sheet (being labeled as BOC-001) that 001} face exposes;
Step (2): get the above-mentioned preparation of 0.1g { 001}BiOCl nanometer sheet is scattered in 20mL polyglycol solution, adds 0.0079g AgNO
3, mix.Gained mixed liquor is microwave irradiation 15min in the time of 160 ℃, makes Ag-BiOCl composite photo-catalyst (being labeled as Ag-BOC-001).
First gained Ag-BOC-001 sample in gained BOC-001 sample in step (1) and step (2) is carried out to SEM and XRD sign, result shows: it is { 001} crystal face that BiOCl sample prepared by this method exposes crystal face, and the decahedron structure that sample is 500nm-1 μ m rule by thickness forms, it is laminar that Ag-BiOCl compound is that the Nano Silver by 100-200nm is attached to BiOCl monocrystalline micro-nano; The XRD collection of illustrative plates of BiOCl sample and the XRD collection of illustrative plates of Ag-BiOCl sample are basically identical, but be 38.2 ° in angle of diffraction, have located to occur the characteristic diffraction peak of weak metal A g.
Next the Ag-BiOCl composite photo-catalyst of being prepared by the present embodiment, for being oxidized the catalytic treatment of penta sodium pentachlorophenate and reduction of hexavalent chromium, separately will utilize NaBH in the BiOCl nanometer sheet with in embodiment 2 and embodiment 1
4the non-selective deposition Ag/BiOCl composite photo-catalyst that the method for reduction prepares is example in contrast, result shows: the Ag-BiOCl composite photo-catalyst that the present embodiment is prepared, the visible light activity of oxidation penta sodium pentachlorophenate and reduction of hexavalent chromium is far away higher than the non-selective deposition Ag/BiOCl composite photo-catalyst that utilizes sodium borohydride electronation to prepare.
Embodiment 3
Step (1): bismuth salt and villaumite are dissolved in stirring in 50mL water obtain the aqueous solution that bismuth salt and villaumite concentration are 0.6mol/L, with the NaOH aqueous solution of 1mol/L, regulating the pH value of the aqueous solution is 1, then in 25mL Teflon reactor, is heated to 240 ℃ and be incubated hydrothermal treatment consists 24h; Be cooled to after room temperature centrifugally, and by gained solid product with distilled water and ethanol washing for several times, drier at 60 ℃, obtain { the BiOCl nanometer sheet (being labeled as BOC-001) that 001} face exposes;
Step (2): get the above-mentioned preparation of 0.1g { 001}BiOCl nanometer sheet is scattered in 25mL polyglycol solution, adds 0.0079g AgNO
3, mix.Gained mixed liquor is microwave irradiation 15min in the time of 160 ℃, makes Ag-BiOCl composite photo-catalyst (being labeled as Ag-BOC-001).
First gained Ag-BOC-001 sample in gained BOC-001 sample in step (1) and step (2) is carried out to SEM and XRD sign, result shows: it is { 001} crystal face that BiOCl sample prepared by this method exposes crystal face, and the decahedron structure that sample is 500nm-1 μ m rule by thickness forms, Ag-BiOCl compound is that the Nano Silver by 100-200nm is attached to BiOCl monocrystalline micro-nano thin slice; The XRD collection of illustrative plates of BiOCl sample and the XRD collection of illustrative plates of Ag-BiOCl sample are basically identical, but be 38.2 ° in angle of diffraction, have located to occur the characteristic diffraction peak of weak metal A g.
Next the Ag-BiOCl composite photo-catalyst of being prepared by the present embodiment, for being oxidized the catalytic treatment of penta sodium pentachlorophenate and reduction of hexavalent chromium, separately will utilize NaBH in the BiOCl nanometer sheet with in embodiment 3 and embodiment 1
4the non-selective deposition Ag/BiOCl composite photo-catalyst that the method for reduction prepares is example in contrast, result shows: the Ag-BiOCl composite photo-catalyst that the present embodiment is prepared, the visible light activity of oxidation penta sodium pentachlorophenate and reduction of hexavalent chromium is far away higher than the non-selective deposition Ag/BiOCl composite photo-catalyst that utilizes sodium borohydride electronation to prepare.
Each raw material that the present invention is cited, and the bound of each raw material of the present invention, interval value, and the bound of technological parameter (as temperature, time etc.), interval value can realize the present invention, at this, do not enumerate embodiment.
Claims (10)
1. BiOCl nanometer sheet { the Ag-BiOCl composite photo-catalyst that 001} crystal face depositing nano silvery is standby, it is characterized in that, it is the BiOCl nanometer sheet of 500nm~1 μ m by thickness and is attached to BiOCl single crystal nanoplate { Nano Silver of 001} face forms, and the particle diameter of described Nano Silver is 100~200nm.
BiOCl nanometer sheet 001} crystal face depositing nano silvery, for a method for Ag-BiOCl composite photo-catalyst, is characterized in that step is as follows:
(1) preparation { the BiOCl single crystal nanoplate that 001} face exposes: bismuth salt and villaumite are added to the water to dissolving, constantly stir simultaneously, regulate pH to 0.5~2, then 200~240 ℃ of hydrothermal treatment consists 18~30 hours in hydrothermal reaction kettle, post processing obtains { the BiOCl single crystal nanoplate that 001} face exposes, wherein: bismuth salt is in bismuth, and villaumite is in chlorine, and both mol ratios are 1:1;
(2) prepare Ag-BiOCl composite photo-catalyst: { the BiOCl single crystal nanoplate that 001} face exposes is scattered in polyhydroxy-alcohol nonaqueous solvents, obtains its dispersion liquid, then add AgNO in described dispersion liquid by step (1) gained
3, 130~180 ℃ of radiation 7~15 minutes in microwave reaction system after mixing, post processing obtains Ag-BiOCl composite photo-catalyst.
3. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: the bismuth salt in described step (1) is five water bismuth nitrates, and described villaumite is potassium chloride.
4. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: in the aqueous solution of described step (1), the amount of substance concentration of bismuth salt and villaumite is 0.06~0.065mol/L.
5. { 001} crystal face depositing nano silvery is for the method for Ag-BiOCl composite photo-catalyst for BiOCl nanometer sheet according to claim 2, it is characterized in that: the post processing of described step (1) is for being cooled to room temperature, washing, dry { the BiOCl single crystal nanoplate that 001} face exposes that obtains.
6. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: in described step (1), pH adjusting is NaOH solution with conditioning agent.
7. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: the reactor in described step (1) is Teflon reactor.
8. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: AgNO in described step (2)
3in the quality of Ag, account for the 3-6% of BiOCl nanometer monocrystalline tablet quality.
9. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: the polyhydroxy-alcohol nonaqueous solvents in described step (2) is ethylene glycol or polyethylene glycol.
10. { 001} crystal face depositing nano silvery, for the method for Ag-BiOCl composite photo-catalyst, is characterized in that BiOCl nanometer sheet according to claim 2: the ratio of the quality of described step (2) BiOCl single crystal nanoplate and the volume of polyhydroxy-alcohol nonaqueous solvents is 0.004~0.006g/mL.
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