CN104275183A - Transition metal ion doped photocatalyst and preparation method thereof - Google Patents
Transition metal ion doped photocatalyst and preparation method thereof Download PDFInfo
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- CN104275183A CN104275183A CN201310277468.0A CN201310277468A CN104275183A CN 104275183 A CN104275183 A CN 104275183A CN 201310277468 A CN201310277468 A CN 201310277468A CN 104275183 A CN104275183 A CN 104275183A
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Abstract
The invention belongs to the technical field of material preparation, and relates to a doped ZnO photocatalyst and a preparation method thereof. The method comprises the following steps: 1, adding a zinc salt, a transition metal salt solid and deionized water into a reactor, adding concentrated hydrochloric acid, and slowly adding an alkaline solution under strong stirring to neutralize to make the pH value of the obtained solution to 7-8 in order to obtain a turbid solution containing white precipitate; 2, centrifuging to obtain the white precipitate, and sequentially washing the white precipitate by deionized water and ethanol; 3, drying to obtain a dried catalyst precursor; and 4, grinding to form superfine powder, and calcining to obtain the transition metal ion doped ZnO photocatalyst powder. The catalyst has the characteristics of simple preparation, low price, high catalysis efficiency and the like, and can be used to degrade many organic pollutants by using ultraviolet/visible light as a light source, and can be widely used in wastewater treatment and water protection.
Description
Technical field
The present invention relates to technical field of material, relate to a kind of doped transition metal ions photochemical catalyst and preparation method thereof.
Background technology
In recent decades, along with the development of modern industry, the especially development of organic chemical industry, petrochemical industry and pesticide chemical, problem of environmental pollution especially water pollution problem has become one of whole mankind's significant problem in the urgent need to address.Photocatalysis oxidation technique be solve at present water pollution, administer waste water the most effective, simple and easy to do method.
Photocatalysis oxidation technique refers under the irradiation of ultraviolet light or visible ray, the energy of photochemical catalyst absorb photons, create and there is extremely strong oxidability photohole, therefore can fast by the pollutant of all kinds of organic-inorganic under the reaction condition of gentleness, as: hydro carbons and polycyclic aromatic hydrocarbon, halogenated aromatic compound, dyestuff, surfactant, agricultural chemicals, oils, cyanide etc. are degraded into the innocuous substances such as micromolecular water and carbon dioxide.
The core of photocatalysis oxidation technique is photochemical catalyst, and the activity of photochemical catalyst in photocatalytic process and existing forms thereof are the key factors that can photocatalytic process complete smoothly.The semiconductor light-catalyst majority of current comparative maturity all belongs to broad stopband n-type semiconductor compound, wherein with TiO
2the product of series is maximum, and kind is the abundantest.But TiO
2band-gap energy comparatively large, hole is easily buried in oblivion, so photocatalysis efficiency is very not high.
Summary of the invention
The object of the invention is to the defect for overcoming prior art and ZnO photocatalyst of a kind of inorganic metal ion mixing and preparation method thereof is provided.
For achieving the above object, the technical solution used in the present invention is as follows:
A preparation method for doping type ZnO photocatalyst, adopts coprecipitation to prepare this composite photo-catalyst, mainly comprises the following steps:
(1) in reactor, add zinc salt, transition metal salt solid and deionized water, then add concentrated hydrochloric acid, then slowly drip alkaline solution neutralization under vigorous stirring and make, between pH value to 7 ~ 8 of solution, to obtain the turbid solution comprising white precipitate;
(2) turbid solution comprising white precipitate step (1) obtained, through centrifugation, obtains white precipitate, uses deionized water, absolute ethanol washing white precipitate successively; Then dry, obtain dry catalyst precursor;
(3) catalyst precursor of drying is ground to ultrafine powder, then this superfine powder is calcined, the ZnO photocatalyst powder of obtained doped transition metal ions.
In described step (1), zinc salt is Zn (NO
3)
26H
2o, ZnSO
47H
2o or ZnC
2o
42H
2one or more in O.
In described step (1), transition metal salt is FeCl
36H
2o, CoCl
26H
2o or CrCl
36H
2one or more of O, wherein, the quality of transition metal salt is 0.1 ~ 1% of zinc salt quality.
Concentrated hydrochloric acid is the concentrated hydrochloric acid of mass fraction 38% in described step (1), and described alkaline solution is one or more of the NaOH solution of mass fraction 10 ~ 30% or KOH solution.Add 5 ~ 10 and prevent zinc salt and the hydrolysis of transition metal salt solid,
Described step (1) or (2) middle deionized water are resistivity > 10
6the ultra-pure water of Ω cm, washing times is 10 ~ 20 times;
In described step (1), mixing speed is more than or equal to 1500RPM.In described step (2), absolute ethyl alcohol is pure for analyzing, and washing times is 5 ~ 10 times.
In described step (2), bake out temperature is 90 ~ 120 DEG C, and the baking needed time is 2 ~ 4 hours.
In described step (3), ultrafine powder is order number 80 ~ 200 object powder.
In described step (3), calcining heat is 500 ~ 600 DEG C, and calcining required time is 4 ~ 8 hours.
The doping type ZnO photocatalyst that a kind of said method is obtained.
The present invention compared with the existing technology, has the following advantages and beneficial effect:
Catalyst of the present invention has easy, cheap, the catalytic efficiency high of preparation, and ultraviolet/visible light can be utilized for light source, degraded Some Organic Pollutants, and at improvement waste water, protection water body has a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of the embodiment of the present invention 1 products obtained therefrom.
Fig. 2 is the TEM image of the embodiment of the present invention 1 products obtained therefrom.
Detailed description of the invention
The present invention is further illustrated below in conjunction with specific embodiment.
The present invention is with methyl orange solution of degrading for template, and characterize the catalytic efficiency of the doping type photochemical catalyst that the present invention obtains, concrete steps are as follows:
Get the doping type ZnO photocatalyst powder 0.12g prepared in the following example 1-6 and join 100mL, concentration is in the methyl orange solution of 10mg/L, after sonic oscillation certain hour, be positioned over illumination in photocatalysis apparatus (pH value of solution is about 6, and temperature is room temperature).Controlling mixing speed makes catalyst powder fully be suspended in solution, and after illumination certain hour, sampling, centrifugation, measures solution absorbance with UV2550 type ultraviolet-uisible spectrophotometer.The degradation rate of methyl orange shows with following formula table:
The sonic oscillation time is 15 ~ 30 minutes; Light source in photocatalysis apparatus is 40W incandescent lamp and peak wavelength 365nm, the uviol lamp of power 18W, and the light application time under incandescent lamp and uviol lamp is respectively 4 hours and 1 hour.
The following example step (1) or (2) middle deionized water are resistivity > 10
6the ultra-pure water of Ω cm.
Embodiment 1
(1) in 2000mL there-necked flask, 50 grams of Zn (NO are added
3)
26H
2o and 0.05 gram of (being 0.1% of zinc salt quality) FeCl
36H
2o, then the deionized water of 1000ml and the concentrated hydrochloric acid 0.25ml of 38% is added, under strong agitation, (mixing speed is more than or equal to 1500RPM) slow NaOH alkaline solution neutralization dripping mass fraction 10%, between pH value to 7 ~ 8 of adjustment solution, obtains white precipitate.
(2) white precipitate obtained is taken out, after centrifugation, first spend deionized water 10 times, then use absolute ethanol washing 5 times.Then dry 4 hours under being placed in 90 DEG C of temperature conditions, obtain dry catalyst precursor.
(3) catalyst precursor of drying is placed in mortar and is ground to 80 object powders, then powder is calcined 8 hours under 500 DEG C of temperature conditions, obtained Fe
3+doping ZnO photochemical catalyst powder.
Through test 0.1%Fe
3+doping ZnO catalyst, the degradation rate of illumination 4 hours degraded methyl orange solutions is 31.23% under visible light, and the degradation rate of illumination 1 hour degraded methyl orange solution is 60.79% under ultraviolet light.
Fig. 1 is the XRD diffraction pattern of the product doping type ZnO photocatalyst of the present embodiment gained; Fig. 2 is the TEM image of the product of the present embodiment gained.As can be seen from Fig. 1 we, Fe
3+the XRD collection of illustrative plates of doping ZnO, compared with pure ZnO, does not find new diffraction maximum, and just the position at peak slightly offsets, and does not generate new thing phase.Fig. 2 then illustrates, this photochemical catalyst diameter of particle, between 10 ~ 20nm, is a kind of photochemical catalyst of Nano grade.
Embodiment 2
(1) in 2000mL there-necked flask, 50 grams of ZnSO are added
47H
2o and 0.5 gram of (being 1% of zinc salt quality) CoCl
26H
2o, then the deionized water of 1000ml and the concentrated hydrochloric acid 0.30ml of 38% is added, under strong agitation, (mixing speed is more than or equal to 1500RPM) slow NaOH alkaline solution neutralization dripping mass fraction 20%, between pH value to 7 ~ 8 of adjustment solution, obtains white precipitate.
(2) white precipitate obtained is taken out, after centrifugation, first spend deionized water 12 times, then use absolute ethanol washing 6 times.Then dry 3 hours under being placed in 100 DEG C of temperature conditions, obtain dry catalyst precursor.
(3) catalyst precursor of drying is placed in mortar and is ground to 120 object powders, then powder is calcined 6 hours under 550 DEG C of temperature conditions, obtained Co
2+doping ZnO photochemical catalyst powder.
Through test 1%Co
2+doping ZnO catalyst, the degradation rate of illumination 4 hours degraded methyl orange solutions is 21.17% under visible light, and the degradation rate of illumination 1 hour degraded methyl orange solution is 48.16% under ultraviolet light.
Embodiment 3
(1) in 2000mL there-necked flask, 50 grams of ZnC are added
2o
42H
2o and 0.1 gram of (being 0.2% of zinc salt quality) CrCl
36H
2o, then the deionized water of 1000ml and the concentrated hydrochloric acid 0.40ml of 38% is added, under strong agitation, (mixing speed is more than or equal to 1500RPM) slow NaOH alkaline solution neutralization dripping mass fraction 30%, between pH value to 7 ~ 8 of adjustment solution, obtains white precipitate.
(2) white precipitate obtained is taken out, after centrifugation, first spend deionized water 15 times, then use absolute ethanol washing 8 times.Then dry 2 hours under being placed in 120 DEG C of temperature conditions, obtain dry catalyst precursor.
(3) catalyst precursor of drying is placed in mortar and is ground to 200 object powders, then powder is calcined 4 hours under 600 DEG C of temperature conditions, obtained Cr
3+doping ZnO photochemical catalyst powder.
Through test 0.2%Cr
3+doping ZnO catalyst, the degradation rate of illumination 4 hours degraded methyl orange solutions is 24.38% under visible light, and the degradation rate of illumination 1 hour degraded methyl orange solution is 53.89% under ultraviolet light.
Embodiment 4
(1) in 2000mL there-necked flask, 50 grams of Zn (NO are added
3)
26H
2o and 0.1(is 0.2% of zinc salt quality) gram FeCl
36H
2o, 0.1 gram of CrCl
36H
2o, then adds the deionized water of 1000ml and the concentrated hydrochloric acid 0.50ml of 38%, and under strong agitation, (mixing speed is more than or equal to 1500RPM) slow KOH alkaline solution neutralization dripping mass fraction 10%, between pH value to 7 ~ 8 of adjustment solution, obtains white precipitate.
(2) white precipitate obtained is taken out, after centrifugation, first spend deionized water 20 times, then use absolute ethanol washing 10 times.Then dry 4 hours under being placed in 90 DEG C of temperature conditions, obtain dry catalyst precursor.
(3) catalyst precursor of drying is placed in mortar and is ground to 80 object powders, then powder is calcined 8 hours under 500 DEG C of temperature conditions, obtained Fe
3+/ Cr
3+doping ZnO photochemical catalyst powder.
Through test 0.2%Fe
3+/ 0.2%Cr
3+doping ZnO catalyst, the degradation rate of illumination 4 hours degraded methyl orange solutions is 37.51% under visible light, and the degradation rate of illumination 1 hour degraded methyl orange solution is 63.72% under ultraviolet light.
Embodiment 5
(1) in 2000mL there-necked flask, 50 grams of ZnSO are added
47H
2o and 0.1 gram of (being 0.2% of zinc salt quality) CoCl
26H
2o, 0.2 gram of CrCl
36H
2o, then adds the deionized water of 1000ml and the concentrated hydrochloric acid 0.30ml of 38%, and under strong agitation, (mixing speed is more than or equal to 1500RPM) slow KOH alkaline solution neutralization dripping mass fraction 20%, between pH value to 7 ~ 8 of adjustment solution, obtains white precipitate.
(2) white precipitate obtained is taken out, after centrifugation, first spend deionized water 15 times, then use absolute ethanol washing 8 times.Then dry 3 hours under being placed in 100 DEG C of temperature conditions, obtain dry catalyst precursor.
(3) catalyst precursor of drying is placed in mortar and is ground to 120 object powders, then powder is calcined 6 hours under 550 DEG C of temperature conditions, obtained Co
2+/ Cr
3+doping ZnO photochemical catalyst powder.
Through test 0.2%Co
2+/ 0.4%Cr
3+doping ZnO catalyst, the degradation rate of illumination 4 hours degraded methyl orange solutions is 26.02% under visible light, and the degradation rate of illumination 1 hour degraded methyl orange solution is 54.26% under ultraviolet light.
Embodiment 6
(1) in 2000mL there-necked flask, 50 grams of ZnC are added
2o
42H
2o and 0.3 gram of (being 0.6% of zinc salt quality) FeCl
36H
2o, 0.2 gram of CoCl
26H
2o, then adds the deionized water of 1000ml and the concentrated hydrochloric acid 0.30ml of 38%, and under strong agitation, (mixing speed is more than or equal to 1500RPM) slow KOH alkaline solution neutralization dripping mass fraction 30%, between pH value to 7 ~ 8 of adjustment solution, obtains white precipitate.
(2) white precipitate obtained is taken out, after centrifugation, first spend deionized water 12 times, then use absolute ethanol washing 7 times.Then dry 2 hours under being placed in 120 DEG C of temperature conditions, obtain dry catalyst precursor.
(3) catalyst precursor of drying is placed in mortar and is ground to 200 object powders, then powder is calcined 4 hours under 600 DEG C of temperature conditions, obtained Co
2+/ Fe
3+doping ZnO photochemical catalyst powder.
Through test 0.6%Co
2+/ 0.4%Fe
3+doping ZnO catalyst, the degradation rate of illumination 4 hours degraded methyl orange solutions is 22.74% under visible light, and the degradation rate of illumination 1 hour degraded methyl orange solution is 51.93% under ultraviolet light.
In above-described embodiment doping type ZnO photocatalyst prepare easy, cheap, catalytic efficiency is high, this doping type photochemical catalyst can utilize ultraviolet/visible light for light source, degraded Some Organic Pollutants, improvement waste water, protection water body have a wide range of applications.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. a preparation method for doping type ZnO photocatalyst, is characterized in that: comprise the following steps:
(1) in reactor, add zinc salt, transition metal salt solid and deionized water, then add concentrated hydrochloric acid, then slowly drip alkaline solution neutralization under vigorous stirring and make, between pH value to 7 ~ 8 of solution, to obtain the turbid solution comprising white precipitate;
(2) turbid solution comprising white precipitate step (1) obtained, through centrifugation, obtains white precipitate, uses deionized water, absolute ethanol washing white precipitate successively; Then dry, obtain dry catalyst precursor;
(3) catalyst precursor of drying is ground to ultrafine powder, then this superfine powder is calcined, the ZnO photocatalyst powder of obtained doped transition metal ions.
2. preparation method according to claim 1, is characterized in that: in described step (1), zinc salt is Zn (NO
3)
26H
2o, ZnSO
47H
2o or ZnC
2o
42H
2one or more in O.
3. preparation method according to claim 1, is characterized in that: in described step (1), transition metal salt is FeCl
36H
2o, CoCl
26H
2o or CrCl
36H
2one or more of O, wherein, the quality of transition metal salt is 0.1 ~ 1% of zinc salt quality.
4. preparation method according to claim 1, is characterized in that: concentrated hydrochloric acid is the concentrated hydrochloric acid of mass fraction 38% in described step (1), and described alkaline solution is one or more of the NaOH solution of mass fraction 10 ~ 30% or KOH solution.
5. preparation method according to claim 1, is characterized in that: described step (1) or (2) middle deionized water are resistivity > 10
6the ultra-pure water of Ω cm, washing times is 10 ~ 20 times.
6. preparation method according to claim 1, is characterized in that: in described step (1), mixing speed is more than or equal to 1500RPM.
7. preparation method according to claim 1, is characterized in that: in described step (2), and absolute ethyl alcohol is pure for analyzing, and washing times is 5 ~ 10 times.
8. preparation method according to claim 1, is characterized in that: in described step (2), bake out temperature is 90 ~ 120 DEG C, and the baking needed time is 2 ~ 4 hours.
9. preparation method according to claim 1, is characterized in that: in described step (3), and ultrafine powder is order number 80 ~ 200 object powder;
Or in described step (3), calcining heat is 500 ~ 600 DEG C, calcining required time is 4 ~ 8 hours.
10. the doping type ZnO photocatalyst that in a claim 1-9, arbitrary described method is obtained.
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| CN110124657A (en) * | 2019-06-14 | 2019-08-16 | 辽宁大学 | K ion doping ZnO catalysis material and its preparation method and application |
| CN114797835A (en) * | 2021-01-27 | 2022-07-29 | 中国科学院理化技术研究所 | ZnO/ZnCr 2 O 4 Preparation method of heterojunction photocatalyst and application of heterojunction photocatalyst in ammonia photocatalytic synthesis |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105381802A (en) * | 2015-12-23 | 2016-03-09 | 哈尔滨工业大学 | Method for preparing dandelion-shaped Fe3O4@ZnO core-shell structure compound on basis of heterogeneous nucleation method and application |
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| CN110124657A (en) * | 2019-06-14 | 2019-08-16 | 辽宁大学 | K ion doping ZnO catalysis material and its preparation method and application |
| CN110124657B (en) * | 2019-06-14 | 2021-07-20 | 辽宁大学 | K ion doped ZnO photocatalytic material and preparation method and application thereof |
| CN114797835A (en) * | 2021-01-27 | 2022-07-29 | 中国科学院理化技术研究所 | ZnO/ZnCr 2 O 4 Preparation method of heterojunction photocatalyst and application of heterojunction photocatalyst in ammonia photocatalytic synthesis |
| CN114797835B (en) * | 2021-01-27 | 2024-02-20 | 中国科学院理化技术研究所 | ZnO/ZnCr 2 O 4 Preparation method of heterojunction photocatalyst and application of heterojunction photocatalyst in ammonia synthesis |
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Application publication date: 20150114 |