CN1446862A - Aquosity pulp of tin dioxide with nano stibonium being adulterated to - Google Patents
Aquosity pulp of tin dioxide with nano stibonium being adulterated to Download PDFInfo
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- CN1446862A CN1446862A CN 03114873 CN03114873A CN1446862A CN 1446862 A CN1446862 A CN 1446862A CN 03114873 CN03114873 CN 03114873 CN 03114873 A CN03114873 A CN 03114873A CN 1446862 A CN1446862 A CN 1446862A
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Abstract
A nano Sb doped water SnO2 slurry for antistatic or antiradiation coated layer is prepared through dispersing the nano ATO powder in water, adding disperser and pH regulator, and blal grinding. It has long storage period (more than 5 months).
Description
Technical field
The present invention relates to a kind of nano antimony-doped tindioxide water paste and preparation method thereof.
Background technology
In recent years, development along with material science and technology, each fields that enter society day by day such as various macromolecular materials such as plastics, fiber, rubber, coating all are to be formed by these processing of high molecular material such as the housing and the surface of most of electronic instrument instruments, space flight and aviation aircraft, household electrical appliance.Because macromolecular material has insulativity, its surface is rubbed or is easily produced and accumulation static when clashing into, when accumulation of static electricity to a certain degree the time, will produce static discharge and cause malignant event.Along with the improving constantly of people's living standard, various display devices enter increasing family again, and these display devices all have very strong radiation to human body, and a lot of dusts are also usually adsorbed on its surface because of electrostatic interaction in addition.In order to eliminate the static of polymer surface, alleviate display device radiation and static, must be coated with the last layer antistatic coating to them, this makes the development of antistatic material come into one's own day by day.
ATO is the adulterated tindioxide of antimony (Antimony Doped Tin Oxide), be a kind of transparent conductive material, be mainly used in anti-static plastic, coating, fiber, the radioprotective antistatic coating on the indicating meter, the infrared absorption lagging material, gas sensitive and electrode materials etc.Nano ATO powder and other antistatic material are compared as carbon black, metal simple-substance, organic antistatic material etc., not only have high electroconductibility, also have the high-performance of nano material.But because the specific surface area of nano-powder is big, surface energy height, powder are in the thermodynamic instability state of height, very easily produce between the powder granule and reunite.The generation of reuniting has very big influence to the performance performance of nano-powder material.The method that suppresses the nano-powder reunion has two kinds, and the one, in the powder preparing process, control preparation technology stops the generation of powder reuniting; Another is after powder preparing is good, and powder is carried out dispersion treatment.
Adopt chemical coprecipitation to prepare the nano ATO powder at present mostly, the primary particle diameter of ATO powder, body that this method is prepared can reach tens nanometers, but the reunion of powder is very serious, and collective's granularity of coacervate reaches several microns.If powder directly is dispersed in the coating, make electrically conducting coating, powder can not be uniformly dispersed in coating on the one hand, and the powder granule of Tuan Juing is difficult to open on the other hand, thereby can't embody the characteristic of nano-powder.In order to address this problem, earlier powder is carried out dispersion treatment in certain medium usually, make slip, mix with coating with slip again, thereby reach the effect that mixes.
But because the surface energy height of nano-powder, in the nano-powder dispersion process, if do not add certain dispersion agent, powder will be difficult to also can reunite after dispersion or the dispersion, thereby dispersion system is difficult to stable.
Summary of the invention
One of technical issues that need to address of the present invention are to disclose a kind of nano antimony-doped tindioxide water paste, to overcome the very difficult stable defective of dispersion system that prior art exists;
The present invention needs two of technical solution problem to provide the preparation method of above-mentioned nano antimony-doped tindioxide water paste.
Design of the present invention is: utilizes wet ball grinding technology, the nano ATO powder is dispersed in the water medium, add certain amount of dispersant, and add a certain amount of pH value conditioning agent, and the pH value of regulation system, thus obtain high dispersing stabilized nano ATO water paste.
The nano ATO water paste of stably dispersing of the present invention is a kind of composition, is made up of the nano ATO powder, water, dispersion agent, the pH value conditioning agent that use significant quantity, and the weight ratio of dispersion agent and ATO is:
Dispersion agent: ATO=0.05～7.0% (wt.);
The add-on of pH value conditioning agent reaches 5.0～10.0 for making final pH value of slurry;
Said ATO powder is a kind of light blue inorganic conductive powder, it consists of the tindioxide of mixing antimony, can adopt the method for document and relevant patent disclosure to be prepared, as adopting special CN1317803A of China and U.S. Pat 9820502 disclosed methods to be prepared, its component and content comprise 2～50wt%Sb
2O
3+ Sb
2O
5, 50～98wt%SnO
2
The particle diameter of ATO powder is 80～130nm in the slurry;
For the convenience of using, the solid content of slurry is suitable with 10～50wt%;
Said dispersion agent comprises one or more in trolamine, triethylamine, thanomin, diisopropanolamine (DIPA), sodium-metaphosphate, Sodium hexametaphosphate 99, sodium polyphosphate, polyvinyl alcohol, polyvinylpyrrolidone, the methacryloxy silane;
Said pH value conditioning agent is acidity or alkaline matter, comprises in ammoniacal liquor, hydrochloric acid, the oleic acid one or more.
The preparation method of nano ATO water paste of the present invention may further comprise the steps successively:
(1) water and dispersion agent are mixed in ball grinder;
(2) the ATO powder is added in the above-mentioned ball grinder, stirs;
(3) add the pH regulator agent in above-mentioned ball grinder, the pH that regulates dispersion system is 5.0～10.0;
(4) ball-milling medium zirconium pearl is joined in the above-mentioned ball grinder, zirconium pearl volume is 4～6 times of powder volume;
(5) above-mentioned ball grinder is put on the ball mill, the ball milling time is 24～96 hours;
(6) take off ball grinder, pour out slurry, elimination zirconium pearl promptly obtains the nano ATO water paste.
The nano ATO water paste that makes according to the method described above, the median size of particle are less than 130nm, and pH value of slurry is 5～10, stablize the shelf-time greater than 5 months, can be widely used in various antistatic, the antiradiation coating materials.
Embodiment
Embodiment 1
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.05g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.03; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 102nm, pH value is 7.58 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 2
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.05; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 86.6nm, pH value is 7.5 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 3
In the ball grinder of 300ml, add the 90ml deionized water, add 0.2g trolamine and 0.2g PVA1750 (polyvinyl alcohol) again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.0; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 100nm, pH value is 8.22 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 4
In the ball grinder of 300ml, add the 90ml deionized water, add 0.1g PVA1750 (polyvinyl alcohol) again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 8.98; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 123nm, pH value is 6.65 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 5
In the ball grinder of 300ml, add the 90ml deionized water, add 0.7g PVA1750 (polyvinyl alcohol) again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 8.96; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 124nm, pH value is 6.61 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 6
In the ball grinder of 300ml, add the 90ml deionized water, add 0.1gPVP (polyvinylpyrrolidone) again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.05; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 124nm, pH value is 6.16 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 7
In the ball grinder of 300ml, add the 90ml deionized water, add 0.1g methacryloxy silane again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.0; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 126nm, pH value is 5.05 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 8
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g sodium polyphosphate again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.01; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 96.2nm, pH value is 6.97 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 9
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 7.04; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 102nm, pH value is 6.0 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 10
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.98; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 110nm, pH value is 9.44 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 11
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.01; Add 50ml zirconium pearl again, ball milling took off ball grinder after 24 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 106nm, pH value is 7.75 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 12
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.03; Add 50ml zirconium pearl again, ball milling took off ball grinder after 96 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 90.4nm, pH value is 7.58 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 13
In the ball grinder of 300ml, add the 90ml deionized water, add the 0.1g trolamine again, fully stir the back and add the 10gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 9.02; Add 50ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 92.9nm, pH value is 7.38 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Embodiment 14
In the ball grinder of 300ml, add the 120ml deionized water, add the 0.267g trolamine again, fully stir the back and add the 26.7gATO powder; Fully stir once more, add ammoniacal liquor and hydrochloric acid then, regulate pH value to 8.9; Add 135ml zirconium pearl again, ball milling took off ball grinder after 48 hours, poured out slurry, elimination zirconium pearl, and promptly getting median size is 102nm, pH value is 6.56 the stabilized aqueous slurry of nano ATO.This slurry was deposited 5 months, macroscopic precipitation do not occur.
Claims (9)
1. a nano antimony-doped tindioxide water paste is characterized in that being made up of the nano ATO powder, water, dispersion agent, the pH value conditioning agent that use significant quantity.
2. water paste according to claim 1 is characterized in that the weight ratio of dispersion agent and ATO is:
Dispersion agent: ATO=0.05～7.0% (wt.);
The add-on of pH value conditioning agent reaches 5.0～10.0 for making final pH value of slurry.
3. water paste according to claim 1, the median size that it is characterized in that ATO powder in the slurry is 80～130nm.
4. water paste according to claim 1, the solid content that it is characterized in that slurry is 10～50wt%.
5. water paste according to claim 1 is characterized in that said dispersion agent comprises one or more in trolamine, triethylamine, thanomin, diisopropanolamine (DIPA), sodium-metaphosphate, Sodium hexametaphosphate 99, sodium polyphosphate, polyvinyl alcohol, polyvinylpyrrolidone, the methacryloxy silane;
6. water paste according to claim 1 is characterized in that said pH value conditioning agent is acidity or alkaline matter.
7. according to the preparation method of each described water paste of claim 1～6, it is characterized in that may further comprise the steps successively:
(1) water and dispersion agent are mixed in ball grinder;
(2) the ATO powder is added in the above-mentioned ball grinder, stirs;
(3) in above-mentioned ball grinder, add the pH regulator agent;
(4) ball-milling medium zirconium pearl is joined in the above-mentioned ball grinder;
(5) above-mentioned ball grinder is put on the ball mill;
(6) take off ball grinder, pour out slurry, elimination zirconium pearl promptly obtains the nano ATO water paste.
8. method according to claim 7 is characterized in that, zirconium pearl volume is 4～6 times of powder volume.
9. according to claim 7 or 8 described methods, it is characterized in that the ball milling time is 24～96 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03114873 CN1446862A (en) | 2003-01-13 | 2003-01-13 | Aquosity pulp of tin dioxide with nano stibonium being adulterated to |
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| CN 03114873 CN1446862A (en) | 2003-01-13 | 2003-01-13 | Aquosity pulp of tin dioxide with nano stibonium being adulterated to |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100345764C (en) * | 2005-08-23 | 2007-10-31 | 浙江大学 | Two-step method for preparing stannic oxide nano material |
| CN100441646C (en) * | 2004-05-11 | 2008-12-10 | 长春迪高实业有限公司 | Sunlight controlled coating solution in low radiation, preparation method and application |
| CN101205419B (en) * | 2007-11-30 | 2010-05-19 | 华南理工大学 | Yb-doped nano aqueous ATO heat-proof slurry and preparation thereof |
| CN1865367B (en) * | 2005-05-17 | 2010-10-20 | 上海市建筑科学研究院有限公司 | Aqueous light color nanometer static-conductive coating for inner wall |
| CN1876289B (en) * | 2006-07-12 | 2010-12-22 | 华东理工大学 | Method for preparing antimony doped stannic oxide nanometer electricity-conductive powder |
| CN102108230A (en) * | 2011-02-28 | 2011-06-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Thermal-insulation coating and preparation method thereof |
| CN1827546B (en) * | 2006-02-16 | 2012-06-20 | 雷亚林 | Process for preparing conductive glass and ceramic film with infrared ray and far-infrared ray screen function |
| CN105259306A (en) * | 2015-10-13 | 2016-01-20 | 武汉工程大学 | Nanometer transition metal oxide sensitive slurry and preparing method and application thereof |
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| CN106519777A (en) * | 2016-10-31 | 2017-03-22 | 广州市建筑科学研究院有限公司 | Alcoholic nano transparent infrared thermal insulation anti-sedimentation slurry and preparation method thereof |
| CN109012482A (en) * | 2018-08-14 | 2018-12-18 | 合肥工业大学 | A method of dispersing antimony doped stannic oxide nanometer particle using small molecule amine |
| CN110003685A (en) * | 2019-04-15 | 2019-07-12 | 广西大学 | A kind of preparation method of antimony-doped stannic oxide nano pulp |
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2003
- 2003-01-13 CN CN 03114873 patent/CN1446862A/en active Pending
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| CN100441646C (en) * | 2004-05-11 | 2008-12-10 | 长春迪高实业有限公司 | Sunlight controlled coating solution in low radiation, preparation method and application |
| CN1865367B (en) * | 2005-05-17 | 2010-10-20 | 上海市建筑科学研究院有限公司 | Aqueous light color nanometer static-conductive coating for inner wall |
| CN100345764C (en) * | 2005-08-23 | 2007-10-31 | 浙江大学 | Two-step method for preparing stannic oxide nano material |
| CN1827546B (en) * | 2006-02-16 | 2012-06-20 | 雷亚林 | Process for preparing conductive glass and ceramic film with infrared ray and far-infrared ray screen function |
| CN1876289B (en) * | 2006-07-12 | 2010-12-22 | 华东理工大学 | Method for preparing antimony doped stannic oxide nanometer electricity-conductive powder |
| CN101205419B (en) * | 2007-11-30 | 2010-05-19 | 华南理工大学 | Yb-doped nano aqueous ATO heat-proof slurry and preparation thereof |
| CN102108230A (en) * | 2011-02-28 | 2011-06-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Thermal-insulation coating and preparation method thereof |
| CN102108230B (en) * | 2011-02-28 | 2013-06-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Thermal-insulation coating and preparation method thereof |
| CN105259306A (en) * | 2015-10-13 | 2016-01-20 | 武汉工程大学 | Nanometer transition metal oxide sensitive slurry and preparing method and application thereof |
| CN105259211A (en) * | 2015-10-13 | 2016-01-20 | 武汉工程大学 | Gas-sensor nanometer sensitive material, slurry with gas-sensor nanometer sensitive material, preparing method of gas-sensor nanometer sensitive material, preparing method of slurry and application of gas-sensor nanometer sensitive material |
| CN106519777A (en) * | 2016-10-31 | 2017-03-22 | 广州市建筑科学研究院有限公司 | Alcoholic nano transparent infrared thermal insulation anti-sedimentation slurry and preparation method thereof |
| CN106519777B (en) * | 2016-10-31 | 2019-05-07 | 广州市建筑科学研究院有限公司 | A kind of slurry and preparation method thereof of the infrared heat-insulated anti-settling of alcohol nanometer transparent |
| CN109012482A (en) * | 2018-08-14 | 2018-12-18 | 合肥工业大学 | A method of dispersing antimony doped stannic oxide nanometer particle using small molecule amine |
| CN110003685A (en) * | 2019-04-15 | 2019-07-12 | 广西大学 | A kind of preparation method of antimony-doped stannic oxide nano pulp |
| CN110003685B (en) * | 2019-04-15 | 2021-01-05 | 广西大学 | Preparation method of antimony-doped tin dioxide nano slurry |
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