CN1460544A - Preparation method of nano ZnO-SnO2 composite oxide photo-catalyst - Google Patents

Preparation method of nano ZnO-SnO2 composite oxide photo-catalyst Download PDF

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CN1460544A
CN1460544A CN 03126662 CN03126662A CN1460544A CN 1460544 A CN1460544 A CN 1460544A CN 03126662 CN03126662 CN 03126662 CN 03126662 A CN03126662 A CN 03126662A CN 1460544 A CN1460544 A CN 1460544A
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water
zno
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nano
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CN1201860C (en
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安太成
张茂林
王存
盛国英
傅家谟
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Guangzhou Institute of Geochemistry of CAS
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Guangzhou Institute of Geochemistry of CAS
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Abstract

The preparation method of nano ZnO-SnO2 composite oxide photocatalyst uses water soluble zinc salt and SnCl4.5H2O as raw material, uses ammonia water as precipitant, and utilizes the characteristics of that the amine salt formed by combining ammonia water with negative ion being in other solution can be decomposed into gas to escape when it is sintered and has no need of longer-time washing process so as to can obtain the invented catalyst with higher activity. Said catalyst can degrate and pollutant into harmless compound.

Description

Nano-ZnO-SnO 2The preparation method of compound oxide photocatalyst
Technical field
The present invention relates to a kind of nano-ZnO-SnO 2The preparation method of compound oxide photocatalyst.
Technical background
In the research of photocatalytic degradation, there are much relations in (electrons/to) quantity and life-span because the photo-generated carrier of the photocatalysis performance of semiconductor light-catalyst and photochemical catalyst, and quantity is many more, and the life-span is long more, and photocatalysis performance is just good more.Yet photo-generated carrier can be 10 -9Carry out in second compound, thereby cause the usefulness of photochemical catalyst to reduce greatly, one of key issue that therefore improves photocatalytic activity is exactly the recombination probability that how to reduce light induced electron and hole.
Two kinds of semi-conductive recombination energies of different energy gaps strengthen separation of charge, suppress the compound of electronics-hole and expansion photoexcitation wave-length coverage, thereby have demonstrated than better stability of single semiconductor and photocatalytic activity.
Nano-photocatalyst can make photo-generated carrier be diffused into surperficial required time in the body and shorten, the body that has reduced photo-generated carrier is mutually compound, and specific area increases, and has strengthened the ability of catalyst absorption pollutant, thereby improves the efficient of photocatalytic degradation pollutant.Nano-ZnO-SnO 2The preparation method of compound oxide photocatalyst is the Wang C by this seminar first, (the Wang C that Zhao J C and Wang X M set up in 2002, Zhao J C, Wang X M, et al.Preparation, characterization and photocatalytic activity of nano-sized ZnO-SnO 2Coupled photocatalysts.Appl.Catal., B:Environ, 2002,39:269), employed precipitating reagent is NaOH, has obtained photocatalytic activity preferably.But with NaOH during as precipitating reagent, a large amount of Cl in the solution -And SO 4 2-Will could remove fully by very long a period of time washing, otherwise a large amount of ions that contain in the catalyst can influence its catalytic performance greatly.Though therefore above method is simple, and is more time-consuming.
Summary of the invention
The objective of the invention is to solve NaOH as preparation nano-ZnO-SnO 2Need the problem of long washing process during the precipitating reagent of compound oxide photocatalyst, develop a kind of nano-ZnO-SnO fast 2The preparation method of compound oxide photocatalyst.
The present invention adopts ammoniacal liquor as preparation nano-ZnO-SnO 2The precipitating reagent of compound oxide photocatalyst, the ammoniacal liquor of adding can with anion such as the Cl in other solution -And SO 4 2-Form NH with form in conjunction with attitude 4C1 or (NH 4) 2SO 4, these amine salt will decompose in the process of sintering of catalyst with gas form effusion catalyst, and can obtain nano-ZnO-SnO littler when adopting NaOH to be precipitating reagent 2Compound oxide photocatalyst, thus realized purpose of the present invention.
Technical characterictic of the present invention is, takes by weighing water-soluble zinc salt and SnCl in 20: 1 in molar ratio～1: 20 respectively 45H 2O is dissolved in the ratio dissolving of 100～800mL water then in the 100g water-soluble zinc salt, press 100gSnCl 45H 2O is dissolved in the ratio dissolving of 300～500mL water, and it is fully mixed, and drips NH under vigorous stirring 3H 2O solution, up to the pH value is 5～9, and the continuation stirring made gel in 4～48 hours, through behind the filtration under diminished pressure, under 100～120 ℃ of temperature, dry by the fire 12～48 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 300～900 ℃ again and calcined 1～10 hour down, promptly obtain ZnO-SnO 2Nano-powder.
The best approach of the present invention is, takes by weighing analytically pure water-soluble zinc salt and analytically pure SnCl in 2: 1 in molar ratio respectively 45H 2O is dissolved in the ratio dissolving of 300mL deionized water then in the 100g water-soluble zinc salt, press 100gSnCl 45H 2O is dissolved in the ratio dissolving of 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution is 7 up to the pH value, and the continuation stirring made gel in 12 hours, through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 2 hours down, promptly obtain ZnO-SnO 2Nano-powder.
Described water-soluble zinc salt is ZnSO 47H 2O or ZnSO 4H 2O or ZnSO 46H 2O or ZnCl 2Or ZnCl 23H 2O or ZnI 2Or ZnI 22H 2O or ZnBr 2Or ZnBr 22H 2All water-soluble zinc salts such as O.
The present invention has following advantage:
(1) simple to operate: as to adopt simple coprecipitation technology;
(2) reaction speed is fast, does not need the washing process of long period;
(3) can obtain comparing nano-ZnO-SnO littler when adopting NaOH to be precipitating reagent 2Compound oxide photocatalyst (comparative result sees Table 1).
Table 1 ZnO-SnO 2The size ratio of compound oxide photocatalyst is than particle diameter/nm
Precipitating reagent Component Calcining heat (℃)
?300 ?350 ?400 ?500 ?600 ?700 ?800 ?900
NaOH ?ZnO ?31.0 ?46.4 ?97.9 On a small quantity On a small quantity
?SnO 2 Unformed ?3.9 ?8.2 On a small quantity On a small quantity
?Zn 2SnO 4 ?15.4 ?45.4 ?166.5
NH 3·H 2O ?ZnO ?1.7 ?2.1 ?8.3 ?13.2 ?45.4 ?95.9
?SnO 2 ?0.8 ?1.2 ?3.3 ?8.2 ?19.1 ?50.8
?Zn 2SnO 4 ?3.4 ?13.6
(4) adopt the ZnO-SnO of ammoniacal liquor as the precipitating reagent preparation 2Compound oxide photocatalyst, its photocatalytic activity not only activity than simple oxide are high, and compare the ZnO-SnO for preparing when adopting NaOH for precipitating reagent 2Compound oxide photocatalyst activity higher (seeing accompanying drawing 1).
(5) nano-ZnO-SnO for preparing 2It is non-toxic compound that compound oxide photocatalyst can be used for contaminant degradation.
Description of drawings
Fig. 1:
NH 3H 2O and NaOH do the photocatalyst activity contrast of precipitating reagent gained
Solution concentration: 20mg/L, catalytic amount: 2.5g/L
The specific embodiment
Embodiment 1:
Took by weighing the analytically pure ZnSO of 1437.8g in 20: 1 in molar ratio respectively 47H 2O is dissolved in the 4000mL deionized water, the analytically pure SnCl of 87.8g 45H 2O is dissolved in the 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution is 7 up to the pH value, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 2 hours down, obtain specific area 17.6m 2The ZnO-SnO of/g 2Compound oxide photocatalyst is 54.66% to organic degradation rate.
Embodiment 2:
Took by weighing the analytically pure ZnSO of 71.89g in 1: 20 in molar ratio respectively 47H 2O is dissolved in the 300mL deionized water, the analytically pure SnCl of 1752.9g 45H 2O is dissolved in the 7000mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution, up to pH value 7, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 2 hours down, obtain specific area 43.6m 2The ZnO-SnO of/g 2Compound oxide photocatalyst is 21.79% to organic degradation rate.
Embodiment 3:
Took by weighing the analytically pure ZnSO of 143.8g in 2: 1 in molar ratio respectively 47H 2O is dissolved in the 400mL deionized water, the analytically pure SnCl of 87.8g 45H 2O is dissolved in the 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution, up to pH value 7, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 300 ℃ again and calcined 2 hours down, obtaining ZnO is 1.7nm, SnO 2Powder for 0.8nm.
Embodiment 4:
Took by weighing the analytically pure ZnSO of 143.8g in 2: 1 in molar ratio respectively 47H 2O is dissolved in the 400mL deionized water, the analytically pure SnCl of 87.8g 45H 2O is dissolved in the 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution, up to pH value 7, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 2 hours down, obtaining ZnO is 2.1nm, SnO 2Powder for 1.2nm.
Embodiment 5:
Took by weighing the analytically pure ZnSO of 143.8g in 2: 1 in molar ratio respectively 47H 2O is dissolved in the 400mL deionized water, the analytically pure SnCl of 87.8g 45H 2O is dissolved in the 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution, up to pH value 7, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 10 hours down, obtaining ZnO is 7.1nm, SnO 2Powder for 3.2nm.
Embodiment 6:
Took by weighing the analytically pure ZnSO of 143.8g in 2: 1 in molar ratio respectively 47H 2O is dissolved in the 400mL deionized water, the analytically pure SnCl of 87.8g 45H 2O is dissolved in the 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution, up to pH value 7, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 900 ℃ again and calcined 2 hours down, obtaining ZnO is 95.9nm, SnO 2Be 50.8nm and the more weak Zn of photocatalytic activity 2SnO 413.6nm powder.
Embodiment 7:
Took by weighing the analytically pure ZnCl of 272.6g in 2: 1 in molar ratio respectively 2Be dissolved in the 300mL deionized water the analytically pure SnCl of 350.5g 45H 2O is dissolved in the 1300mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution, up to pH value 7, and the continuation stirring made gel in 12 hours.Through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 2 hours down, obtain specific area 48.2m 2The ZnO-SnO of/g 2Compound oxide photocatalyst is 86.96% to organic degradation rate.
Embodiment 8:
Photocatalysis experiment: take by weighing the ZnO-SnO that the foregoing description makes 2Nano-powder 0.25g adds in the 100mL methyl orange solution (20mg/L), opens in dark place ultrasonic 15 minutes, and electromagnetic agitation is 30 minutes again, and it is fully disperseed, and makes absorption reach balance.In will the mixed solution impouring Pyrex glass reactor after adsorption equilibrium, carry out the photocatalytic degradation reaction with 300W ultraviolet high-pressure mercury lamps (dominant wavelength is 365nm) irradiation, sampling and measuring at regular intervals, sample is 20cm apart from the distance of light source.The results are shown in the foregoing description.

Claims (3)

1. nano-ZnO-SnO 2The preparation method of compound oxide photocatalyst is characterized in that taking by weighing respectively in 20: 1 in molar ratio～1: 20 water-soluble zinc salt and SnCl 45H 2O is dissolved in the ratio dissolving of 100～800mL water then in the 100g water-soluble zinc salt, press 100gSnCl 45H 2O is dissolved in the ratio dissolving of 300～500mL water, and it is fully mixed, and drips NH under vigorous stirring 3H 2O solution, up to the pH value is 5～9, and the continuation stirring made gel in 4～48 hours, through behind the filtration under diminished pressure, under 100～120 ℃ of temperature, dry by the fire 12～48 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 300～900 ℃ again and calcined 1～10 hour down, promptly obtain ZnO-SnO 2Nano-powder.
2. a kind of nano-ZnO-SnO according to claim 1 2The preparation method of compound oxide photocatalyst is characterized in that taking by weighing respectively in 2: 1 in molar ratio analytically pure water-soluble zinc salt and analytically pure SnCl 45H 2O is dissolved in the ratio dissolving of 300mL deionized water then in the 100g water-soluble zinc salt, press 100gSnCl 45H 2O is dissolved in the ratio dissolving of 400mL deionized water, and it is fully mixed, and drips analytically pure NH under vigorous stirring 3H 2O solution is 7 up to the pH value, and the continuation stirring made gel in 12 hours, through behind the filtration under diminished pressure, under 110 ℃ of temperature, dry by the fire 24 hours to the dried xerogel that obtains, after fully grinding, in high temperature box type resistance furnace, slowly be warming up to 350 ℃ again and calcined 2 hours down, promptly obtain ZnO-SnO 2Nano-powder.
3. according to claim 1,2 described a kind of nano-ZnO-SnO 2The preparation method of compound oxide photocatalyst is characterized in that described water-soluble zinc salt is ZnSO 47H 2O or ZnSO 4H 2O or ZnSO 46H 2O or ZnCl 2Or ZnCl 23H 2O or ZnI 2Or ZnI 22H 2O or ZnBr 2Or ZnBr 22H 2O.
CN 03126662 2003-05-26 2003-05-26 Preparation method of nano Zno-SnO2 composite oxide photo-catalyst Expired - Fee Related CN1201860C (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331758C (en) * 2005-12-16 2007-08-15 厦门大学 Method for preparing hollow nano-material of stannic oxide
CN100344574C (en) * 2005-12-16 2007-10-24 厦门大学 Core shell type zinc oxide/stancic oxide composite nanometer material and preparation method thereof
CN101791566A (en) * 2010-04-20 2010-08-04 青岛科技大学 New method for nitrating ZnO based compound nano material
CN101342486B (en) * 2008-08-29 2012-05-30 中国科学院上海硅酸盐研究所 Metallic oxide nano-material
CN102513112A (en) * 2011-11-30 2012-06-27 四川长虹电器股份有限公司 Preparation method for CuO/ZnO composite photochemical catalyst
CN102989443A (en) * 2011-09-16 2013-03-27 天津城市建设学院 High activity ZnO/SnO2 core-shell composite photocatalyst preparation method
CN104391010A (en) * 2014-11-19 2015-03-04 上海纳米技术及应用国家工程研究中心有限公司 Cr2O3-ZnO composite nano material as well as preparation method and application thereof
CN105954327A (en) * 2016-07-07 2016-09-21 钟林超 High-reliability CO2 gas sensor
CN106475117A (en) * 2016-09-14 2017-03-08 东北师范大学 A kind of preparation of three-dimensional ZnO SnS P N hetero-junctions and application
CN108176392A (en) * 2017-12-27 2018-06-19 万华化学集团股份有限公司 Composite catalyst of amine salt and preparation method thereof is catalytically decomposed, prepares the method for MDA
CN108417649A (en) * 2018-02-07 2018-08-17 湖南文理学院 A kind of preparation method and application of tin oxide base solar cell nanometer material
CN110176539A (en) * 2019-05-16 2019-08-27 浙江大学 A kind of preparation method of the stable efficient perovskite solar battery of full spectrum light
CN111250133A (en) * 2020-02-11 2020-06-09 四川师范大学 Preparation method and application of aldehyde-removing antibacterial heterojunction photocatalyst

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331758C (en) * 2005-12-16 2007-08-15 厦门大学 Method for preparing hollow nano-material of stannic oxide
CN100344574C (en) * 2005-12-16 2007-10-24 厦门大学 Core shell type zinc oxide/stancic oxide composite nanometer material and preparation method thereof
CN101342486B (en) * 2008-08-29 2012-05-30 中国科学院上海硅酸盐研究所 Metallic oxide nano-material
CN101791566A (en) * 2010-04-20 2010-08-04 青岛科技大学 New method for nitrating ZnO based compound nano material
CN102989443A (en) * 2011-09-16 2013-03-27 天津城市建设学院 High activity ZnO/SnO2 core-shell composite photocatalyst preparation method
CN102513112A (en) * 2011-11-30 2012-06-27 四川长虹电器股份有限公司 Preparation method for CuO/ZnO composite photochemical catalyst
CN104391010A (en) * 2014-11-19 2015-03-04 上海纳米技术及应用国家工程研究中心有限公司 Cr2O3-ZnO composite nano material as well as preparation method and application thereof
CN105954327A (en) * 2016-07-07 2016-09-21 钟林超 High-reliability CO2 gas sensor
CN106475117A (en) * 2016-09-14 2017-03-08 东北师范大学 A kind of preparation of three-dimensional ZnO SnS P N hetero-junctions and application
CN106475117B (en) * 2016-09-14 2018-11-06 东北师范大学 A kind of preparation and application of three-dimensional ZnO-SnS P-N hetero-junctions
CN108176392A (en) * 2017-12-27 2018-06-19 万华化学集团股份有限公司 Composite catalyst of amine salt and preparation method thereof is catalytically decomposed, prepares the method for MDA
CN108176392B (en) * 2017-12-27 2020-09-08 万华化学集团股份有限公司 Composite catalyst for catalytic decomposition of amine salt, preparation method thereof and method for preparing MDA (multidrug resistance)
CN108417649A (en) * 2018-02-07 2018-08-17 湖南文理学院 A kind of preparation method and application of tin oxide base solar cell nanometer material
CN110176539A (en) * 2019-05-16 2019-08-27 浙江大学 A kind of preparation method of the stable efficient perovskite solar battery of full spectrum light
CN111250133A (en) * 2020-02-11 2020-06-09 四川师范大学 Preparation method and application of aldehyde-removing antibacterial heterojunction photocatalyst

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