CN103846085B - The ZnWO of hydro-thermal method preparation doping Bi 4photochemical catalyst - Google Patents
The ZnWO of hydro-thermal method preparation doping Bi 4photochemical catalyst Download PDFInfo
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- CN103846085B CN103846085B CN201410104948.1A CN201410104948A CN103846085B CN 103846085 B CN103846085 B CN 103846085B CN 201410104948 A CN201410104948 A CN 201410104948A CN 103846085 B CN103846085 B CN 103846085B
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Abstract
The invention belongs to photocatalyst technology field, be specifically related to the ZnWO of a kind of hydro-thermal method preparation doping Bi
4photochemical catalyst.Concrete steps are: soluble tungstate salt and soluble zinc salt that the amount of substance 1-10mmol such as to get, add deionized water, stirs.After the pH value of mixed solution is adjusted to 8-12, add the polyacrylamide that mass fraction is 0.01-0.05%, simultaneously magnetic agitation.At 150-180 DEG C, be incubated 24-48 hour carry out hydro-thermal reaction, after cooling washing and drying, obtain needle-like ZnWO
4powder.Get five water bismuth nitrate and glucose, be dissolved in respectively in ethylene glycol and water.Above-mentioned two kinds of solution are mixed, then adds a certain amount of needle-like ZnWO
4powder, is incubated 15-24 hour hydro-thermal reaction at 120-150 DEG C, after cooling washing and drying, finally obtains the ZnWO of doping Bi
4photochemical catalyst.Take two one-step hydrothermals in the present invention, polyacrylamide adulterates as template and Bi, ensure that operation and process simply easily control, needle-like photochemical catalyst uniformity is good, has higher photocatalytic activity.
Description
Technical field
The invention belongs to photocatalyst technology field, relate to the ZnWO of a kind of hydro-thermal method preparation doping Bi
4the method of photochemical catalyst.
Background technology
In recent years, metal tungstates was as Na
2w
4o
13, Bi
2w
2o
9, (NaBi)
0.5wO
4, AgInW
2o
8, Bi
2wO
6research Deng catalyst also causes the interest of people.These tungstate materials have higher photocatalysis effect in photocatalysis degradation organic contaminant, wherein ZnWO
4there is good stability, photocatalytic and Photoluminescence, can be used for effectively degrading to the organic pollution (formaldehyde, rhodamine B and peacock green) in air and water as photochemical catalyst, thus cause the concern of researcher.
Current synthesis ZnWO
4roughly there are two kinds of methods: solid phase method and liquid phase process.The former such as Wang Qian equality people, in " a kind of method of preparing superfine zinc tungstate antibacterial agent by ultrasonic molten salt " (ZL201010251129.1), under ultrasound condition, first adopts concentration to be all the Na of 0.2mol/L
2wO
4with Zn (NO
3)
2the aqueous solution prepares ZnWO
4presoma; And then this precursor is calcined to obtain cured product in nitric acid sodium salt material, product fully soaks through distilled water, washing; Then filter, dry to remove remaining fused salt, ZnWO
4antimicrobial powder.The people such as Zhou Mingjie, in " manganese chromium codope zinc tungstate luminescent material, preparation method and application thereof " (CN201110191460.3), take ZnO, WO
3, MnO
2and Cr
2o
3powder also to mix at 900 DEG C ~ 1300 DEG C sintering and makes target in 0.5 ~ 5 hour, the target obtained and substrate load the vacuum cavity of magnetic-controlled sputtering coating equipment, then be filmed, obtain film sample, then film sample vacuum annealing process 2h at 600 DEG C.The people such as Li Minghua at " growth of crystal and scintillation properties research " thereof (" artificial lens journal " 1994,23 volumes, the 03rd phase, 240-242), with ZnO and WO
3, Bi
2o
3for raw material, at ZnWO
4bi is mixed in the raw material of crystal
2o
3, from melt, grown Bi:ZnWO with czochralski method
4crystal, finds that Bi ion can eliminate ZnWO effectively
4the color of crystal, improves luminous efficiency and the energy resolution of crystal.These solid phase methods above-mentioned, reaction needed high temperature, process control is complicated, and product grain lack of homogeneity, cost of equipment is high.And liquid phase method, the advantages such as especially hydro-thermal method has simple to operate, and stoichiometry is controlled, and sample crystallinity is high, good dispersion.As Wei the people such as bright lamp at " high-purity monoclinic phase ZnWO
4the preparation method of nano particle and application thereof " in (ZL201110176966.7), adopt 1mmolZn (NO
3)
26H
2o, 1mmolNa
2wO
4be dissolved in 30mL distilled water with 0.5mmol citric acid and stir after 30 minutes, be transferred to by solution in reactor, at 160 DEG C-200 DEG C reaction 12-24h, reaction terminates rear cooling naturally, product, through distilled water and absolute ethanol washing several, obtains described high-purity monoclinic phase ZnWO after drying
4nano particle.The people such as Cao Liyun are " a kind of complexing microwave hydrothermal prepares flower ball-shaped ZnWO
4the method of catalysis material " in (CN201210458084.4), Disodium tungstate (Na2WO4) dihydrate is dissolved in deionized water and obtains solution A; CTAB is dissolved in deionized water and obtains solution B; Zinc vitriol is dissolved in solution B and obtains solution C; Solution A is slowly added in solution C, and regulates pH value of solution=4 ~ 4.5, form colourless transparent solution D; Solution D is added in microwave hydrothermal reaction kettle, add thermal response, after question response terminates, naturally cool to room temperature; Open reactor, adopt deionized water and washes of absolute alcohol product respectively, then drying obtains flower ball-shaped ZnWO
4catalysis material.In addition the people such as Cao Li cloud is by changing reagent type and reaction condition obtains various types of ZnWO
4, as flower ball-shaped (CN201210458137.2 " a kind of flower ball-shaped ZnWO
4the preparation method of catalysis material "), spherical (CN201210458467.1 " a kind of spherical ZnWO
4the preparation method of catalysis material "), the flat flower ball-shaped of six lobes (CN201210458470.3 " the flat flower ball-shaped ZnWO of a kind of six lobe
4the preparation method of catalysis material "), cube (CN201210458710.X " a kind of cubic structure ZnWO
4the preparation method of nano-crystalline photocatalysis material "), bar-shaped (CN201210458736.4 " a kind of ZnWO
4the preparation method of nanometer rods catalysis material ") etc.
But due to ZnWO
4energy gap comparatively large, light absorption wavelength scope is mainly at ultra-violet (UV) band (254nm), and the recombination rate in light induced electron and hole is higher, therefore visible light part capacity usage ratio is low, therefore as improved ZnWO further
4photocatalysis performance, should spectral response range be expanded.
Summary of the invention
Technical problem to be solved by this invention is the defect overcoming the existence of above-mentioned prior art, provides a kind of hydro-thermal method to prepare the ZnWO of doping Bi
4the method of photochemical catalyst, it is with soluble tungstate salt and soluble zinc salt for raw material, with polyacrylamide (PAM) for chelating polymer template, adopts hydro-thermal method to prepare the ZnWO of doping Bi
4photochemical catalyst.Photochemical catalyst uniformity prepared by the method is good, has higher photocatalytic activity, and operation and process simply easily control.
The object of the invention is to be achieved through the following technical solutions, the ZnWO of hydro-thermal method preparation doping Bi
4photochemical catalyst, concrete steps are:
(1) hydro-thermal method prepares needle-like ZnWO
4
First, soluble tungstate salt and each portion of soluble zinc salt of amount of substance 1-10mmol such as to get, add a certain amount of deionized water, at room temperature stir.With NaOH or potassium hydroxide solution, the pH value of mixed solution is adjusted to 8-12.Polyacrylamide (PAM, number-average molecular weight 2.13 × 10 that mass fraction is 0.01-0.05% is added under being placed on room temperature
7), magnetic agitation 30-120min, is transferred in reactor and reactor is put into baking oven simultaneously, at 150-180 DEG C, be incubated 24-48 hour, be cooled to after room temperature until it, repeatedly wash 2-3 time with deionized water and absolute ethyl alcohol, be placed in baking oven to dry, obtain needle-like ZnWO
4powder.
(2) ZnWO of hydro-thermal method preparation doping Bi
4photochemical catalyst
Get five water bismuth nitrates and glucose (mass ratio is 2: 1), be dissolved in ethylene glycol and water respectively, form A and B solution.Above-mentioned AB solution is mixed, then adds a certain amount of needle-like ZnWO
4powder, obtains suspension C.Transfer in reactor by suspension C, reaction temperature 120-150 DEG C, reaction time 15-24 hour, wash several times by ethanol and deionized water after being cooled to room temperature, dry 4-24 hour at 50 DEG C, finally obtains the ZnWO of doping Bi
4photochemical catalyst.
As improvement, described soluble tungstate salt is a kind of in Disodium tungstate (Na2WO4) dihydrate and potassium tungstate or their mixture.
As improvement, described soluble zinc salt is a kind of in zinc nitrate hexahydrate, Zinc vitriol and zinc chloride or their mixture.
Compared with prior art, good effect of the present invention is:
(1) in process of the present invention, take two one-step hydrothermals, ensure that uniformity and the dispersiveness of sample, simplify experiment condition, for large-scale industry preparation is laid a good foundation;
(2) polyacrylamide (PAM, number-average molecular weight 2.13 × 10 is adopted
7) as chelating polymer template, cause ZnWO
4the final shape of crystal is needle-like;
(3) adopt five water bismuth nitrates as Bi source, Bi enters ZnWO
4crystals, thus carry out element doping, effectively improve the photocatalysis performance of catalyst.
Accompanying drawing explanation
Fig. 1: needle-like ZnWO
4sEM.
Fig. 2: Bi doping is on the impact of sample crystal formation.(a：ZnWO
4/ZnO；b：0.05Bi/Zn；c：0.10Bi/Zn；d：0.15Bi/Zn)
Fig. 3: Bi doping is for the impact (for (011) and (110)) of angle of diffraction numerical value.(a：ZnWO
4/ZnO；b：0.05Bi/Zn；c：0.10Bi/Zn；d：0.15Bi/Zn)
Fig. 4: the ZnWO of hydro-thermal method preparation doping Bi
4the electron scanning micrograph of photochemical catalyst.
Fig. 5: light application time is on the impact of photocatalysis effect.(a：ZnWO
4；b：Bi
2WO
6；c：0.10Bi/Zn；d：0.05Bi/Zn；e：0.15Bi/Zn)
Fig. 6: the ZnWO of hydro-thermal method preparation doping Bi
4the electron scanning micrograph of photochemical catalyst.
Fig. 7: sample quality is on the impact of photocatalysis effect.(a：ZnWO
4；b：Bi
2WO
6；c：0.10Bi/Zn；d：0.05Bi/Zn；e：0.15Bi/Zn)
Fig. 8: Bi doping is on the impact (UV-vis DRS spectrum) of the absorbing properties of sample.(a：ZnWO
4/ZnO；b：0.05Bi/Zn；c：0.10Bi/Zn；d：0.15Bi/Zn)
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
This specific embodiment is only explanation of the invention; it is not limitation of the present invention; those skilled in the art can make to the present embodiment the amendment not having creative contribution as required after reading this description, as long as but be all subject to the protection of Patent Law in right of the present invention.
Embodiment 1
First, Disodium tungstate (Na2WO4) dihydrate and each portion of zinc nitrate hexahydrate of amount of substance 1mmol such as to get, add a certain amount of deionized water, at room temperature stir.With sodium hydroxide solution, the pH value of mixed solution is adjusted to 8.Polyacrylamide (PAM, number-average molecular weight 2.13 × 10 that mass fraction is 0.01% is added under being placed on room temperature
7), magnetic agitation 30min, is transferred in reactor and reactor is put into baking oven simultaneously, is incubated 48 hours, is cooled to after room temperature, repeatedly washes 2-3 time with deionized water and absolute ethyl alcohol, be placed in baking oven and dry, obtain ZnWO until it at 180 DEG C
4powder, is shown as needle-like (Fig. 1) by SEM.Get five water bismuth nitrates and and glucose (mass ratio is 2: 1), be dissolved in ethylene glycol and water respectively, form A and B solution.Above-mentioned AB solution is mixed, then adds a certain amount of needle-like ZnWO
4powder is (with five water bismuth nitrate and needle-like ZnWO
4the ratio of the amount of substance of powder is 0.05,0.10 and 0.15), obtain suspension C.Transfer in reactor by suspension C, reaction temperature 120 DEG C, 15 hours reaction time, after being cooled to room temperature, ethanol and deionized water are washed several times, and at 50 DEG C, drying 4 hours, finally obtains the ZnWO of doping Bi
4photochemical catalyst.Shown by XRD test (Fig. 2), when the content of Bi is 0.15, the peak position of characteristic peak is the strongest, and the ZnWO being now mixed with Bi is described
4the degree of crystallinity of photochemical catalyst improves.Do not adulterate the ZnWO of Bi
4can obviously find out the existence having ZnO.The ZnWO of doping Bi can be found out
4the XRD characteristic peak of powder occurs all, and peak type also becomes comparatively sharp-pointed.Along with the increase of Bi concentration, ZnO characteristic spectral line is also more and more not obvious, and illustrate that the content of impurity ZnO is in minimizing, product purity is higher.Fig. 2 is amplified, obtains Fig. 3, in figure, show ZnWO
4/ ZnO mainly grows along cylinder (011) and (110) direction crystal face, the ZnWO of Bi doping
4have the angle of diffraction being obviously different from ZnO, low-angle skew describes the doping of Bi.After Bragg equation 2dsin θ=n λ, Bi doping, interplanar distance becomes large, and θ reduces, and crystal plane direction offsets left.Fig. 4 is the ZnWO of hydro-thermal method preparation doping Bi
4the electron scanning micrograph of photochemical catalyst, illustrates that the doping of Bi exists and fails to have influence on ZnWO
4crystal habit.
The ZnWO of the doping Bi of 10mg
4photochemical catalyst adds in the 10ml rhodamine B solution be equipped with, after ultrasonic for mixture homogenizing, the 150W visible ray lower magnetic force being placed in preheating stirs the different time, then centrifugation, extract supernatant liquor (about 2/3) with dropper, this clear liquid is at 752 ultraviolet specrophotometers (rhodamine B λ
max=553nm) on carry out the mensuration of absorbance, according to the fitting formula between formula absorbance and rhodamine B concentration, calculate the concentration values after rhodamine B is degraded.Using the rhodamine B solution of 10mg/L as photocatalytic degradation object, test in different light application times, obtain Fig. 5.When light application time only has 20min, its photocatalysis effect of 0.15Bi/Zn only has 15.6%, and when light application time is increased to 80min, its photocatalysis effect just reaches 41.8%.Illustrate at identical conditions, in certain limit, along with the increase of light application time, the ZnWO of doping Bi
4with better to the degradation effect of rhodamine B.The rhodamine B solution concentration of the degraded of 0.15Bi/Zn sample is minimum always simultaneously, and its catalytic effect is best.
Embodiment 2
First, potassium tungstate and each portion of Zinc vitriol of amount of substance 10mmol such as to get, add a certain amount of deionized water, at room temperature stir.With potassium hydroxide solution, the pH value of mixed solution is adjusted to 12.Polyacrylamide (PAM, number-average molecular weight 2.13 × 10 that mass fraction is 0.05% is added under being placed on room temperature
7), magnetic agitation 120min, is transferred in reactor and reactor is put into baking oven simultaneously, is incubated 24 hours, is cooled to after room temperature, repeatedly washes 2-3 time, dry in baking oven, obtain ZnWO with deionized water and absolute ethyl alcohol until it at 150 DEG C
4powder.With embodiment 1, suspension C transfers in reactor, reaction temperature 150 DEG C, 24 hours reaction time, and wash several times by ethanol and deionized water after being cooled to room temperature, at 50 DEG C, drying 24 hours, finally obtains the ZnWO of the doping Bi of needle-like
4photochemical catalyst, as Fig. 6.Photocatalysis experiment, with embodiment 1, using the rhodamine B solution of 10mg/L as photocatalytic degradation object, changes catalyst quality and tests, obtain Fig. 7.When the quality of photochemical catalyst increases, its photocatalysis efficiency synchronously rises.When quality is 0.05mg, the ZnWO of 0.15 doping Bi
4photocatalysis effect only have 5.36%, when being raised to 0.25mg qualitatively, its photocatalysis effect reaches 25.3%.Illustrate at identical conditions, in certain limit, along with the increase of photochemical catalyst quality, with better to the degradation effect of rhodamine B.And the rhodamine B solution concentration of the degraded of 0.15Bi/Zn sample under equal in quality is minimum always, its catalytic effect is best.
Embodiment 3
First, get the total amount of substance 5mmol of mixture of Disodium tungstate (Na2WO4) dihydrate and potassium tungstate, its total amount of substance of zinc nitrate hexahydrate, Zinc vitriol and zinc chloride composition mixture is 5mmol, adds a certain amount of deionized water respectively, at room temperature stirs.With NaOH or potassium hydroxide solution, the pH value of mixed solution is adjusted to 10.Polyacrylamide (PAM, number-average molecular weight 2.13 × 10 that mass fraction is 0.03% is added under being placed on room temperature
7), magnetic agitation 100min, is transferred in reactor and reactor is put into baking oven simultaneously, is incubated 36 hours, is cooled to after room temperature, repeatedly washes 2-3 time with deionized water and absolute ethyl alcohol, be placed in baking oven and dry, obtain ZnWO until it at 160 DEG C
4powder.With embodiment 1, suspension C transfers in reactor, reaction temperature 140 DEG C, 20 hours reaction time, and wash several times by ethanol and deionized water after being cooled to room temperature, at 50 DEG C, drying 12 hours, finally obtains the ZnWO of doping Bi
4photochemical catalyst.The test of ultraviolet-visible solid diffuse reflectance spectra is carried out to sample, obtains Fig. 8.As shown in Figure 8, the catalyst after doping Bi enhances the absorption to ultraviolet light, and expands the photoresponse scope of catalyst, also there is certain absorption at visible region (more than 380nm).Generally, along with the increase of Bi incorporation, the absorbability of catalyst to light increases gradually, facilitates the raising of photocatalysis effect.
Claims (3)
1. the ZnWO of a hydro-thermal method preparation doping Bi
4the method of photochemical catalyst, the method comprises the following steps:
(1) hydro-thermal method prepares needle-like ZnWO
4
First, soluble tungstate salt and each portion of soluble zinc salt of amount of substance 1-10mmol such as to get, add a certain amount of deionized water, at room temperature stir, with NaOH or potassium hydroxide solution, the pH value of mixed solution is adjusted to 8-12; The polyacrylamide PAM that mass fraction is 0.01-0.05% is added, number-average molecular weight 2.13 × 10 under being placed on room temperature
7, magnetic agitation 30-120min, is transferred in reactor and reactor is put into baking oven, at 150-180 DEG C, be incubated 24-48 hour, be cooled to after room temperature until it, repeatedly wash 2-3 time with deionized water and absolute ethyl alcohol, be placed in baking oven and dry, obtain needle-like ZnWO simultaneously
4powder;
(2) ZnWO of hydro-thermal method preparation doping Bi
4photochemical catalyst
Get five water bismuth nitrate and glucose, mass ratio is 2: 1, is dissolved in ethylene glycol and water respectively, forms A and B solution; Above-mentioned AB solution is mixed, then adds a certain amount of needle-like ZnWO
4powder, obtains suspension C; Transfer in reactor by suspension C, reaction temperature 120-150 DEG C, reaction time 15-24 hour, wash several times by ethanol and deionized water after being cooled to room temperature, dry 4-24 hour at 50 DEG C, finally obtains the ZnWO of doping Bi
4photochemical catalyst.
2. the method for claim 1, is characterized in that: described soluble tungstate salt is a kind of in Disodium tungstate (Na2WO4) dihydrate and potassium tungstate or their mixture.
3. the method for claim 1, is characterized in that: described soluble zinc salt is a kind of in zinc nitrate hexahydrate, Zinc vitriol and zinc chloride or their mixture.
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| CN106753361A (en) * | 2016-11-14 | 2017-05-31 | 华南理工大学 | A kind of bismuth doping tungstate red fluorescent powder and preparation method, application |
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| CN105271414A (en) * | 2015-10-30 | 2016-01-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of microspheres with doping of Ag ions and zinc tungstate ZnWO4 |
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