CN101759145A - Preparation method of ZnO/TiO2 composite nanoparticles - Google Patents
Preparation method of ZnO/TiO2 composite nanoparticles Download PDFInfo
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- CN101759145A CN101759145A CN201010100047A CN201010100047A CN101759145A CN 101759145 A CN101759145 A CN 101759145A CN 201010100047 A CN201010100047 A CN 201010100047A CN 201010100047 A CN201010100047 A CN 201010100047A CN 101759145 A CN101759145 A CN 101759145A
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- znso
- zno
- tetra
- molar ratio
- butyl titanate
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 20
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract 2
- 238000000227 grinding Methods 0.000 claims abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000001782 photodegradation Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 28
- 239000011787 zinc oxide Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- 238000005303 weighing Methods 0.000 description 8
- 241000370738 Chlorion Species 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002331 protein detection Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种ZnO/TiO2复合纳米粒子的制备方法，1)、按ZnSO4·7H2O与NaCl或KCl的摩尔比为：1∶5～1∶15在室温下混合均匀，研磨5-10min，成白色膏状形态；2)、按ZnSO4·7H2O与NaOH或KOH的摩尔比为：1∶2～1∶3，加入NaOH或KOH，继续室温下研磨15-25min，形成淡黄色的细粉末；3)、按ZnSO4·7H2O与钛酸四正丁酯的摩尔比为：1∶1～1∶0.1，加入钛酸四正丁酯，混合均匀成膏状，并且继续研磨10-20min，得到白色的固体粉末；将到白色的固体粉末用二次水搅拌混合，并且超声8-10min，离心分离直到上层清液中检测不出有氯离子存在，将分离产物置于真空干燥箱中，75℃下干燥数小时，即得到了ZnO/TiO2复合纳米粒子。该复合纳米粒子具有优异的紫外吸收性能，在光催化，光降解等应用中显示出巨大的应用前景。The invention discloses a preparation method of ZnO/TiO 2 composite nanoparticles. 1) According to the molar ratio of ZnSO 4 7H 2 O to NaCl or KCl: 1:5-1:15, mix uniformly at room temperature, grind 5-10min, into a white paste form; 2), according to the molar ratio of ZnSO 4 7H 2 O to NaOH or KOH: 1:2～1:3, add NaOH or KOH, continue grinding at room temperature for 15-25min, Form pale yellow fine powder; 3) According to the molar ratio of ZnSO 4 7H 2 O to tetra-n-butyl titanate: 1:1～1:0.1, add tetra-n-butyl titanate, mix well to form a paste , and continue to grind for 10-20min to obtain a white solid powder; stir and mix the white solid powder with secondary water, and ultrasonically 8-10min, and centrifuge until no chloride ions are detected in the supernatant, then separate The product was placed in a vacuum drying oven and dried at 75° C. for several hours to obtain ZnO/TiO 2 composite nanoparticles. The composite nanoparticles have excellent ultraviolet absorption properties and show great application prospects in photocatalysis, photodegradation and other applications.
Description
Technical field
The present invention relates to a kind of ZnO/TiO
2The preparation method of composite nanoparticle.
Background technology
In numerous nano-metal-oxides, ZnO has the band gap (3.37eV) of broad and higher exciton binding energy (60meV) as important II-VI family semi-conducting material, and nontoxic, cheap, environmental stability is good, exactly because these excellent performances of zinc oxide, the ZnO nano semiconductor material has been widely used in every field: electrooptical device, sensor, photovoltaic material, piezoelectric, cell marking, protein detection, ultraviolet light detection etc.At present, the main synthetic method of ZnO nano material has: microwave method, sol-gal process, hydro-thermal method, coprecipitation, solution calcination method, thermal decomposition method, gas-phase condensation method, thermal evaporation, direct polishing and chemical mechanical pulping or the like. but all in liquid phase, finish mostly in the above cited method, however solid phase is synthetic relatively, and liquid phase is synthesized the weak point that itself is arranged, such as: the nucleating growth process has notable difference and some reaction speed is too fast, process is difficult to control, and the trickle change on the dynamics will cause structure, modal great variety.
Summary of the invention
The purpose of this invention is to provide a kind of ZnO/TiO
2The preparation method of composite nanoparticle.
The objective of the invention is to realize in the following way: 1, a kind of ZnO/TiO
2The preparation method of composite nanoparticle: it is characterized in that:
1), presses ZnSO
47H
2The mol ratio of O and NaCl or KCl is: at room temperature mixed in 1: 5～1: 15, and ground 5-10min, become white paste form;
2), press ZnSO
47H
2The mol ratio of O and NaOH or KOH is: 1: 2～1: 3, add NaOH or KOH, and continue to grind 15-25min under the room temperature, form flaxen fine powder;
3), press ZnSO
47H
2The mol ratio of O and tetra-n-butyl titanate is: 1: 1～1: 0.1, add tetra-n-butyl titanate, and be mixed into paste, and continue to grind 10-20min, obtain the pressed powder of white; The pressed powder that will arrive white mixes with secondary water, and ultrasonic 8-10min, and centrifugation can not detect chlorion and exists in supernatant liquor, separated product is placed vacuum drying chamber, 75 ℃ of down dry a few hours, has promptly obtained ZnO/TiO
2Composite nanoparticle.
The present invention has following beneficial effect: 1, technological process is simple, and the reaction time is short, and is with low cost; 2, whole process of preparation need not any organic solvent, and reaction temperature only needs room temperature to get final product, and need not last handling processes such as high annealing; 3, the advantage in the reactive matrix system continues as next step doping system service, form the compound system 4 of two kinds of nano particles, prepared composite nanoparticle particle diameter comparatively meticulous (3～20nm), favorable dispersibility, be dispersed in the organic solvent such as methyl alcohol and do not see a sedimentation yet in month, reunite; 5, by regulating ZnSO in the compound system
47H
2The mol ratio that O is different with tetra-n-butyl titanate is (1: 1～1: 0.1), and its performance can obtain raising in various degree; 6, composite nanoparticle significantly strengthens UV Absorption, can be used for photocatalysis, light degradation etc.;
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
At first, with the ZnSO of 1.0g
47H
2The NaCl of O and 2.5g at room temperature mixes, and grinds 10min, becomes white paste form.Then, the NaOH powder of 0.28g is joined in the above mixed system, continue to grind 20min under the room temperature, form flaxen fine powder.At last, accurately pipette 1.19ml tetra-n-butyl titanate (ZnSO with pipette
47H
2The mol ratio of O and tetra-n-butyl titanate is: 1: 1) join in the above mixed-powder, be mixed into paste, and continue to grind 10-20min, obtain the pressed powder of white.End product is mixed with secondary water, and ultrasonic 8-10min, centrifugation repeats for several times, can not detect chlorion and exist in supernatant liquor, and separated product is placed vacuum drying chamber, 75 ℃ of down dry a few hours, has promptly obtained ZnO and TiO
2Composite nanoparticle.
Embodiment 2
Take by weighing the ZnSO of 1.0g
47H
2The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 1.19ml (ZnSO with pipette
47H
2The mol ratio of O and tetra-n-butyl titanate is: 1: 1) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO
2Composite nanoparticle.
Embodiment 3
Take by weighing the ZnSO of 1.0g
47H
2The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 0.60ml (ZnSO with pipette
47H
2The mol ratio of O and tetra-n-butyl titanate is: 1: 0.3) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO
2Composite nanoparticle.
Embodiment 4
Take by weighing the ZnSO of 1.0g
47H
2The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 0.30ml (ZnSO with pipette
47H
2The mol ratio of O and tetra-n-butyl titanate is: 1: 0.2) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO
2Composite nanoparticle.
Embodiment 5
Take by weighing the ZnSO of 1.0g
47H
2The KCl of O and 3.0g mixes, griding reaction 10min.Then, take by weighing the KOH of 0.39g and join in the above mixed-powder, mix, continue griding reaction 20min, form the fine powder of little Huang.At last, accurately pipette tetra-n-butyl titanate 0.12ml (ZnSO with pipette
47H
2The mol ratio of O and tetra-n-butyl titanate is: 1: 0.1) add wherein, griding reaction is complete to the tetra-n-butyl titanate hydrolysis, forms meticulous white powder.With product for several times with the ultrasonic cleaning of secondary water, no chlorion existence in centrifugal clear liquid, 70 ℃ of vacuum drying 5 hours obtain ZnO and TiO
2Composite nanoparticle.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010100047 CN101759145B (en) | 2010-01-22 | 2010-01-22 | A kind of preparation method of ZnO/TiO2 composite nanoparticles |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010100047 CN101759145B (en) | 2010-01-22 | 2010-01-22 | A kind of preparation method of ZnO/TiO2 composite nanoparticles |
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| Publication Number | Publication Date |
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| CN101759145A true CN101759145A (en) | 2010-06-30 |
| CN101759145B CN101759145B (en) | 2013-03-20 |
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|---|---|---|---|
| CN 201010100047 Expired - Fee Related CN101759145B (en) | 2010-01-22 | 2010-01-22 | A kind of preparation method of ZnO/TiO2 composite nanoparticles |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103263963A (en) * | 2013-04-22 | 2013-08-28 | 薛运河 | Wet-to-dry dispersant-free method for producing ultrafine nanoscale dry powder and involved device |
| CN103854865A (en) * | 2014-03-21 | 2014-06-11 | 武汉理工大学 | ZnO/TiO2 composite material for photoanode material and preparation method thereof |
| CN105152240A (en) * | 2015-09-16 | 2015-12-16 | 太仓市国峰纺织印染有限责任公司 | High-efficiency dyeing wastewater treating agent and preparation method thereof |
| CN108298576A (en) * | 2018-03-07 | 2018-07-20 | 福建工程学院 | A kind of preparation method of antibacterial granule activated carbon |
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2010
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Patent Citations (4)
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Non-Patent Citations (5)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103263963A (en) * | 2013-04-22 | 2013-08-28 | 薛运河 | Wet-to-dry dispersant-free method for producing ultrafine nanoscale dry powder and involved device |
| CN103263963B (en) * | 2013-04-22 | 2015-07-01 | 薛运河 | Wet-to-dry dispersant-free method for producing ultrafine nanoscale dry powder and involved device |
| CN103854865A (en) * | 2014-03-21 | 2014-06-11 | 武汉理工大学 | ZnO/TiO2 composite material for photoanode material and preparation method thereof |
| CN103854865B (en) * | 2014-03-21 | 2016-08-17 | 武汉理工大学 | ZnO/TiO2 composite material for photoanode material and preparation method thereof |
| CN105152240A (en) * | 2015-09-16 | 2015-12-16 | 太仓市国峰纺织印染有限责任公司 | High-efficiency dyeing wastewater treating agent and preparation method thereof |
| CN105152240B (en) * | 2015-09-16 | 2018-03-30 | 太仓市国峰纺织印染有限责任公司 | A kind of efficiently treatment of dyeing/printing wastewaters and preparation method thereof |
| CN108298576A (en) * | 2018-03-07 | 2018-07-20 | 福建工程学院 | A kind of preparation method of antibacterial granule activated carbon |
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|---|---|
| CN101759145B (en) | 2013-03-20 |
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