CN101125677A - Method for preparing high dispersity nano zinc oxide - Google Patents
Method for preparing high dispersity nano zinc oxide Download PDFInfo
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- CN101125677A CN101125677A CNA2007101394509A CN200710139450A CN101125677A CN 101125677 A CN101125677 A CN 101125677A CN A2007101394509 A CNA2007101394509 A CN A2007101394509A CN 200710139450 A CN200710139450 A CN 200710139450A CN 101125677 A CN101125677 A CN 101125677A
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Abstract
The invention relates to a method to produce highly dispersed nano-zinc oxide. Zinc source and ammonium salt are mixed according to molar ratio 1:0.5-10 between zinc and ammonium; according to the molar ratio 1:0.5-10 between zinc and ammonia in ammonia water, concentration of which is 10-25 percent, ammonia water is added into the mixture, stirred for 1-10 hours, aged for 1-2 days and filtered; filtrate is steamed under 60 DEG C - 95 DEG C until white precipitate comes out and white precipitate is obtained after filtering; the white precipitate is washed by deionized water until pH value is 6-8, dried under 50 DEG C -110 DEG C, roasted for 1-8 hours under 200 DEG C-800 DEG C to get the nano-zinc oxide. The invention has the advantages of simple production process, mild reaction condition and getting nano-zinc oxide with large specific surface area, good dispersion, non-aggregation and comparatively good photo-catalytic activity.
Description
Technical field
The invention belongs to a kind of method for preparing high dispersity nano zinc oxide, specifically a kind of preparation method with high dispersity nano zinc oxide of photocatalytic activity.
Background technology
Nano zine oxide has characteristics such as nontoxic, structure and stable performance as photocatalyst; its photocatalytic process uses air or oxygen as oxygenant; can directly make excitaton source with sunlight; at the organic and inorganic pollutant of degraded; the protection environment, to keep aspect such as the eubiosis significant, become the environmental type catalyzer with DEVELOPMENT PROSPECT.The preparation of industrialization nano zine oxide adopts chemical precipitation method more at present, the nano zine oxide bad dispersibility of preparation, agglomeration is serious, there is more problem (Zhan Guoping in the practical application, Huang Kelong, Liu Suqin. the technology of preparing of Nano-class zinc oxide and progress [J]. New Chemical Materials, 2001,29 (7): 15～18.).Along with further going deep into to the research of preparation nano zine oxide; by adding high-molecular polythene pyrrolidone (PVP) as coating materials; the nanometer Zinc oxide powder that makes; has good dispersiveness (Yang Qinglin; Guo Lin; Wuzhong China etc. the synthetic and sign [J] of nano zine oxide cenotype under the room temperature. SCI, 2003,24 (1): 82～85.).Adopt polyoxyethylene glycol PEG-400, unsaturated fatty acids Tween-60 and oligomeric acrylic acid sodium PAA as surface-modifying agent, investigated it to the nano granular of zinc oxide size of preparation and the influence of mode of appearance, the result shows that polyoxyethylene glycol can reduce particle size effectively, and adopt Tween-60 and PAAS can obtain the nano zine oxide (Min Huiling of favorable dispersity, Huang Yating, Wang Liming. nano zine oxide surface modification and applied research [J]. printing and dyeing, 2004,30 (16): 7～9.).But adopt the method for adding properties-correcting agent to prepare high-dispersibility zinc oxide and can make that cost greatly improves, and increased production operation, be unfavorable for suitability for industrialized production.
Summary of the invention
The present invention provides a kind of low cost, easy industrialized preparation has the method for the nanometer Zinc oxide powder of better photocatalytic activity.
The present invention is achieved in that under the room temperature in zinc, ammonium salt mixture, add certain amount of ammonia water, fully stir ageing under the room temperature, filter supernatant liquid, with clear liquid ammonia still process,, filter to a large amount of white precipitates appearance, washing, drying, roasting obtains good dispersity, does not have the nano zine oxide of reuniting and having photocatalytic activity.
Synthetic method of the present invention comprises the steps:
(1) molar ratio by zinc and ammonium is 1: 0.5～10, and zinc source and ammonium salt are made into mixture;
(2) be that the mol ratio of ammonia in 10～25% the ammoniacal liquor is 1: 0.5～10 by zinc and mass concentration, ammoniacal liquor be added in step (1) mixture that fully stirred 1 hour～10 hours, room temperature ageing 1～2 day is filtered;
(3) gained filtrate is occurred at 60 ℃～95 ℃ following ammonia still process to white precipitates, filter white depositions.
(4) with deionized water white depositions is washed to pH=6～8,50 ℃～110 ℃ dry down, 200 ℃～800 ℃ roastings 1～8 hour, obtain good dispersity, do not have the nano zine oxide of reuniting and having photocatalytic activity.
Used zinc source is: zinc oxide, zinc chloride, zinc sulfate, zinc nitrate or zinc acetate etc.
Used ammonium salt is: ammonium sulfate, bicarbonate of ammonia, volatile salt, ammonium oxalate, ammonium nitrate, ammonium chloride, ammonium phosphate or ammonium hydrogen phosphate etc.
The present invention compared with prior art has following advantage:
The present invention need not add any properties-correcting agent, directly the processing parameter by the control preparation process just can obtain that specific surface is big, good dispersity, nothing reunion and have the nano zine oxide of better photocatalytic activity, preparation technology is simple, and the reaction conditions gentleness is suitable for suitability for industrialized production.
Embodiment
Embodiment 1
Under the room temperature, zinc nitrate and volatile salt being made into mixture (mol ratio of zinc and ammonium is 1: 1.2), is that 10% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 4) in the mixture then with mass concentration, fully stirred 1 hour, room temperature ageing 1 day is filtered, and gets supernatant liquid, with clear liquid in 70 ℃ of ammonia still processs, filter, deionized water wash is to pH=6,50 ℃ of dryings, roasting is 2 hours in 200 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 2
Under the room temperature, zinc chloride and ammonium nitrate being made into mixture (mol ratio of zinc and ammonium is 1: 5), is that 15% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 2) in the mixture then with mass concentration, fully stirred 2 hours, room temperature ageing 1 day is filtered, and gets supernatant liquid, with clear liquid in 75 ℃ of ammonia still processs, filter, deionized water wash is to pH=7,60 ℃ of dryings, roasting is 2 hours in 300 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 3
Under the room temperature, zinc chloride and ammonium oxalate being made into mixture (mol ratio of zinc and ammonium is 1: 3), is that 15% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 8) in the mixture then with mass concentration, fully stirred 3 hours, room temperature ageing 2 days is filtered, and gets supernatant liquid, with clear liquid in 80 ℃ of ammonia still processs, filter, deionized water wash is to pH=7,65 ℃ of dryings, roasting is 1 hour in 400 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 4
Under the room temperature, zinc sulfate and bicarbonate of ammonia being made into mixture (mol ratio of zinc and ammonium is 1: 6), is that 15% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 3) in the mixture then with mass concentration, fully stirred 5 hours, room temperature ageing 2 days is filtered, and gets supernatant liquid, with clear liquid in 60 ℃ of ammonia still processs, filter, deionized water wash is to pH=8,80 ℃ of dryings, roasting is 3 hours in 500 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 5
Under the room temperature, zinc acetate and ammonium phosphate being made into mixture (mol ratio of zinc and ammonium is 1: 3), is that 20% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 6) in the mixture then with mass concentration, fully stirred 6 hours, room temperature ageing 1 day is filtered, and gets supernatant liquid, with clear liquid in 75 ℃ of ammonia still processs, filter, deionized water wash is to pH=7,90 ℃ of dryings, roasting is 6 hours in 600 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 6
Under the room temperature, zinc chloride and ammonium sulfate being made into mixture (mol ratio of zinc and ammonium is 1: 5), is that 25% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 5) in the mixture then with mass concentration, fully stirred 8 hours, room temperature ageing 2 days is filtered, and gets supernatant liquid, with clear liquid in 95 ℃ of ammonia still processs, filter, deionized water wash is to pH=8,85 ℃ of dryings, roasting is 5 hours in 700 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 7
Under the room temperature, zinc nitrate and ammonium chloride being made into mixture (mol ratio of zinc and ammonium is 1: 1.5), is that 20% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 3) in the mixture then with mass concentration, fully stirred 7 hours, room temperature ageing 2 days is filtered, and gets supernatant liquid, with clear liquid in 90 ℃ of ammonia still processs, filter, deionized water wash is to pH=6,95 ℃ of dryings, roasting is 7 hours in 800 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 8
Under the room temperature, zinc sulfate and volatile salt being made into mixture (mol ratio of zinc and ammonium is 1: 1.8), is that 10% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 3) in the mixture then with mass concentration, fully stirred 10 hours, room temperature ageing 1 day is filtered, and gets supernatant liquid, with clear liquid in 85 ℃ of ammonia still processs, filter, deionized water wash is to pH=8,110 ℃ of dryings, roasting is 3 hours in 650 ℃ of retort furnaces, obtains nano oxidized zinc product.
Embodiment 9
Under the room temperature, zinc oxide and bicarbonate of ammonia being made into mixture (mol ratio of zinc and ammonium is 1: 2), is that 25% ammoniacal liquor joins (mol ratio of zinc and ammonia is 1: 4) in the mixture then with mass concentration, fully stirred 5 hours, room temperature ageing 2 days is filtered, and gets supernatant liquid, with clear liquid in 80 ℃ of ammonia still processs, filter, deionized water wash is to pH=7,90 ℃ of dryings, roasting is 5 hours in 550 ℃ of retort furnaces, obtains nano oxidized zinc product.
Claims (3)
1. method for preparing high dispersity nano zinc oxide, its feature is comprising the steps:
(1) molar ratio by zinc and ammonium is 1: 0.5～10, and zinc source and ammonium salt are made into mixture;
(2) be that the mol ratio of ammonia in 10～25% the ammoniacal liquor is 1: 0.5～10 by zinc and mass concentration, ammoniacal liquor be added in step (1) mixture that fully stirred 1 hour～10 hours, room temperature ageing 1～2 day is filtered;
(3) gained filtrate is occurred at 60 ℃～95 ℃ following ammonia still process to white precipitates, filter white depositions;
(4) with deionized water white depositions is washed to pH=6～8,50 ℃～110 ℃ dry down, 200 ℃～800 ℃ roastings 1～8 hour, obtain nano zine oxide.
2. a kind of method for preparing high dispersity nano zinc oxide as claimed in claim 1, its feature is zinc oxide, zinc chloride, zinc sulfate, zinc nitrate or zinc acetate in described zinc source.
3. a kind of method for preparing high dispersity nano zinc oxide as claimed in claim 1, its feature is ammonium sulfate, bicarbonate of ammonia, volatile salt, ammonium oxalate, ammonium nitrate, ammonium chloride, ammonium phosphate or ammonium hydrogen phosphate at described ammonium salt.
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| CNB2007101394509A CN100554162C (en) | 2007-09-16 | 2007-09-16 | A kind of method for preparing high dispersity nano zinc oxide |
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| CNB2007101394509A CN100554162C (en) | 2007-09-16 | 2007-09-16 | A kind of method for preparing high dispersity nano zinc oxide |
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| CN101125677A true CN101125677A (en) | 2008-02-20 |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153062A (en) * | 2011-01-30 | 2011-08-17 | 广东光华科技股份有限公司 | Method for preparing electronic grade high-purity zinc pyrophosphate |
| CN102826591A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high purity nanometer zinc oxide by using electrolytic zinc acid leaching slag |
| CN102826588A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high-purity nanometer zinc oxide by using ammonia process decarburization of steel plant dust |
| CN102826586A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high purity nanometer zinc oxide by using steel plant dust |
| CN102826589A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high purity nanometer zinc oxide by using ammonia process of steel plant dust |
| CN102839282A (en) * | 2012-09-25 | 2012-12-26 | 四川巨宏科技有限公司 | Method for producing high-purity nano zinc oxide from low-grade zinc oxide ores |
| CN102863007A (en) * | 2012-09-25 | 2013-01-09 | 四川巨宏科技有限公司 | Method for producing high-purity nano-zinc oxide by ammonia method using electrolytic zinc acid-leaching residues |
| CN102863011A (en) * | 2012-09-25 | 2013-01-09 | 四川巨宏科技有限公司 | Method of using low-grade zinc oxide ore to produce high-purity nano zinc oxide by means of ammonia process |
| CN103318941A (en) * | 2012-09-12 | 2013-09-25 | 上海工程技术大学 | Synthetic method of porous ZnO three-dimensional superstructure assembled by nano-sheets |
| WO2014047760A1 (en) * | 2012-09-25 | 2014-04-03 | 四川巨宏科技有限公司 | Method for producing high-purity nanometer zinc oxide from electrolytic zinc acid-leaching residues by ammonia decarburization |
| CN104495911A (en) * | 2015-01-05 | 2015-04-08 | 安徽省特种设备检测院 | Method for preparing nano-ZnO powder |
| RU2580731C2 (en) * | 2014-06-11 | 2016-04-10 | Андрей Петрович Ларьков | Method of producing ultrafine zinc oxide |
| CN106006712A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparing method for nanometer zinc oxide |
| CN108622926A (en) * | 2018-05-23 | 2018-10-09 | 四川理工学院 | A kind of preparation method of surface photovoltage signal enhancing type ZnO |
| CN109935705A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | Hole-injecting material and preparation method thereof and QLED device |
| CN110217813A (en) * | 2019-07-11 | 2019-09-10 | 江苏千品新材料科技有限公司 | A kind of preparation method of nano zine oxide |
| CN110857221A (en) * | 2018-08-24 | 2020-03-03 | 义乌倍肯新材料科技有限公司 | Nano zinc oxide emulsion and preparation method thereof |
-
2007
- 2007-09-16 CN CNB2007101394509A patent/CN100554162C/en not_active Expired - Fee Related
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153062A (en) * | 2011-01-30 | 2011-08-17 | 广东光华科技股份有限公司 | Method for preparing electronic grade high-purity zinc pyrophosphate |
| CN103318941A (en) * | 2012-09-12 | 2013-09-25 | 上海工程技术大学 | Synthetic method of porous ZnO three-dimensional superstructure assembled by nano-sheets |
| CN102826586B (en) * | 2012-09-25 | 2014-06-18 | 四川锌鸿科技有限公司 | Method for producing high purity nanometer zinc oxide by using steel plant dust |
| WO2014047760A1 (en) * | 2012-09-25 | 2014-04-03 | 四川巨宏科技有限公司 | Method for producing high-purity nanometer zinc oxide from electrolytic zinc acid-leaching residues by ammonia decarburization |
| CN102826591A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high purity nanometer zinc oxide by using electrolytic zinc acid leaching slag |
| CN102839282A (en) * | 2012-09-25 | 2012-12-26 | 四川巨宏科技有限公司 | Method for producing high-purity nano zinc oxide from low-grade zinc oxide ores |
| CN102863007A (en) * | 2012-09-25 | 2013-01-09 | 四川巨宏科技有限公司 | Method for producing high-purity nano-zinc oxide by ammonia method using electrolytic zinc acid-leaching residues |
| CN102863011A (en) * | 2012-09-25 | 2013-01-09 | 四川巨宏科技有限公司 | Method of using low-grade zinc oxide ore to produce high-purity nano zinc oxide by means of ammonia process |
| CN102826588A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high-purity nanometer zinc oxide by using ammonia process decarburization of steel plant dust |
| CN102826586A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high purity nanometer zinc oxide by using steel plant dust |
| CN102826588B (en) * | 2012-09-25 | 2014-06-18 | 四川锌鸿科技有限公司 | Method for producing high-purity nanometer zinc oxide by using ammonia process decarburization of steel plant dust |
| US9394183B2 (en) | 2012-09-25 | 2016-07-19 | Sichuan Xinhong Technology Co., Ltd | Method for producing a high-purity nanometer zinc oxide from electrolytic zinc acid leaching residues by ammonia decarburization |
| CN102826589A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high purity nanometer zinc oxide by using ammonia process of steel plant dust |
| CN102826589B (en) * | 2012-09-25 | 2014-06-18 | 四川锌鸿科技有限公司 | Method for producing high purity nanometer zinc oxide by using ammonia process of steel plant dust |
| CN102826591B (en) * | 2012-09-25 | 2014-06-18 | 四川锌鸿科技有限公司 | Method for producing high purity nanometer zinc oxide by using electrolytic zinc acid leaching slag |
| RU2580731C2 (en) * | 2014-06-11 | 2016-04-10 | Андрей Петрович Ларьков | Method of producing ultrafine zinc oxide |
| CN104495911B (en) * | 2015-01-05 | 2016-06-01 | 安徽省特种设备检测院 | A kind of method preparing nano ZnO powder |
| CN104495911A (en) * | 2015-01-05 | 2015-04-08 | 安徽省特种设备检测院 | Method for preparing nano-ZnO powder |
| CN106006712A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparing method for nanometer zinc oxide |
| CN109935705A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | Hole-injecting material and preparation method thereof and QLED device |
| CN109935705B (en) * | 2017-12-15 | 2020-09-04 | Tcl科技集团股份有限公司 | Hole injection material, preparation method thereof and QLED device |
| CN108622926A (en) * | 2018-05-23 | 2018-10-09 | 四川理工学院 | A kind of preparation method of surface photovoltage signal enhancing type ZnO |
| CN108622926B (en) * | 2018-05-23 | 2020-06-26 | 四川理工学院 | Preparation method of surface photovoltage signal enhanced ZnO |
| CN110857221A (en) * | 2018-08-24 | 2020-03-03 | 义乌倍肯新材料科技有限公司 | Nano zinc oxide emulsion and preparation method thereof |
| CN110217813A (en) * | 2019-07-11 | 2019-09-10 | 江苏千品新材料科技有限公司 | A kind of preparation method of nano zine oxide |
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| CN100554162C (en) | 2009-10-28 |
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