CN100383196C - Method for preparing conducting particles for composite electrically-conducting paint using microemulsion technology - Google Patents
Method for preparing conducting particles for composite electrically-conducting paint using microemulsion technology Download PDFInfo
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- CN100383196C CN100383196C CNB2006100400705A CN200610040070A CN100383196C CN 100383196 C CN100383196 C CN 100383196C CN B2006100400705 A CNB2006100400705 A CN B2006100400705A CN 200610040070 A CN200610040070 A CN 200610040070A CN 100383196 C CN100383196 C CN 100383196C
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Abstract
The present invention discloses a method for preparing electric conduction particles for a composite electric conduction coating by using micro emulsion technology. The present invention is characterized in that W/O type micro emulsion technology is used, and substances with large dielectric constants, such as mica powder or quartz powder, etc., are used for core substances; stannous chloride dihydrate is used as a main coating substance, antimony chloride is used as adulterant, hydrogen peroxide is used as oxidant, ammonia water is used as a precipitation agent, and uniform sediment is prepared in micro emulsion; composite electric conduction particles are obtained through filtration, washing, desiccation and calcination. The composite electric conduction particles of the present invention are homogeneously and completely coated, and have the uniform diameter and stable electric conduction performance. The electric conduction service life of an electric conduction coating is long.
Description
Technical field
The present invention relates to a kind of method of utilizing microemulsion technology to prepare conducting particles for composite electrically-conducting paint.
Background technology
Early stage preparation coating is to utilize microemulsion technology to prepare with the technology of conducting particles, mainly is pure metal or metal oxide (TiO for example
2) nanoparticle, pure metal or metal oxide nanoparticles be as conducting particles, and the one, price comparison is expensive; The 2nd, because its density is bigger, phenomenon also takes place to extract out in the use of electrically conducting coating or storage process easily, cause the conductivity shakiness, in order to solve pure metal or metal oxide above-mentioned shortcoming as conducting particles, the technician adopts the regular solution legal system to be equipped with composite conducting particle technology, but with the prepared composite conducting particle of regular solution method, though its diameter also can be in the nano level scope (100-10nm). absorption property is also better. and price is more much lower than pure metal or metal oxide, density is also much smaller, also is not prone to conducting particles and extracts problem out.But the particle dia of this method preparation is not of uniform size, is difficult to control, and coats imperfectly, and covered effect is bad, so that conductivity is still unstable, the conduction life-span is shorter.
Summary of the invention
The objective of the invention is to overcome metal simple-substance, life-span short, conductivity unsettled shortcoming uneven in the prior art, a kind of method of utilizing microemulsion technology to prepare conducting particles for composite electrically-conducting paint is provided as conducting particles cost height and coating.
The present invention realizes with following technical scheme: utilize the w/o type microemulsion technology, with the bigger material of specific inductivity such as mica powder or silica powder is the core material, with tin protochloride is main coating, with the antimony chloride is hotchpotch, be oxygenant with the hydrogen peroxide, be precipitation agent with ammoniacal liquor, the throw out of preparation homogeneous in microemulsion, after filtration, washing, drying and calcining obtain the composite conducting particle.
It may further comprise the steps:
(1) preparation of microemulsion: under the normal temperature (20-30 ℃), in the deionized water adding 55-65% organic solvent with weight ratio 10-20% (referring to account for the weight percent of microemulsion, as follows), mix; Add tensio-active agent, the 15-20% cosurfactant middle rank alcohols of 3-5% then successively, stirring promptly gets microemulsion;
(2) preparation of composite conducting particle: get 50% of above-mentioned microemulsion, add 60%-80% (accounting for the per-cent that coating adds core material gross weight, as follows) tin protochloride, butter of antimony, hydrogen peroxide under the normal temperature successively, stir and make mixed liquor A; In remaining microemulsion, add 20%-40% core material mica powder, and constantly stir, form mixed liquid B; At last mixed liquor A is constantly added in the mixed liquid B, continuously stirring simultaneously, the reinforced back dropping ammonia of finishing is regulated pH value to 7-9, then the mixed solution throw out is filtered, dry, calcine and make finished product.
The proportioning of above-mentioned tin protochloride, butter of antimony, hydrogen peroxide and core material is: tin protochloride, butter of antimony, hydrogen peroxide account for the 60%-80% of four gross weights, the core material accounts for 7.89% of four gross weights, wherein the mol ratio of tin protochloride and butter of antimony is 9-10: 1, and the mol ratio of hydrogen peroxide and tin protochloride is 1-1.1: 1.
Above-mentioned organic solvent is the naphthenic technical grade product, as hexanaphthene, pentamethylene.
Above-mentioned tensio-active agent is anion surfactant or nonionogenic tenside, and anion surfactant is the alkyl polyoxyethylene ether sulfate class, alkylbenzene sulfonate; Nonionogenic tenside is alkyl polyoxyethylene ether, alkylphenol polyoxyethylene.
Above-mentioned cosurfactant is intermediate alcohols technical grade product, as butanols, amylalcohol.
Above-mentioned tin protochloride, butter of antimony, hydrogen peroxide, ammoniacal liquor are technical grade product.
Above-mentioned core material is technical grade mica powder, silica powder product, and granularity is the 325-600 order.
The composite conducting particle of the present invention preparation is according to the difference of processing condition, appearance color by ivory buff to light gray-white.
The invention has the beneficial effects as follows:
Microemulsion in the present technique is the microemulsion of water-in-oil-type, and wherein water nuclear is for the microreactor of physical change and chemical transformation takes place.The composite conducting particle of this invention coats even, complete, and diameter homogeneous (50-10nm), conductivity are stablized, the conduction life-span of electrically conducting coating is longer.Its advantage at first is both to have solved that pure metal simple substance is too high as the conducting particles cost, density is excessive, in use is easy to the problem of extracting out; Next is to have solved the composite conducting particle to coat inequality, conductivity shakiness, the problem that work-ing life is short; Moreover coating can be the compound of high oxidation state, can be the compound of low-oxidation-state also, and raw material sources are extensive, reduce cost greatly on original basis.
Embodiment
Further illustrate the solution of the present invention and effect below in conjunction with embodiment.
Under the normal temperature (20-30 ℃),, add the nonionogenic tenside alkyl polyoxyethylene ether of 5g, slightly stir the beaker of technical grade hexalin 200ml injection 600ml.Add the 30-40ml deionized water then, add the butanols of measuring slightly again and make solution become the microemulsion of clear, be divided into two parts of A, B by 50%.
The hydrogen peroxide that in A part microemulsion, adds 12g tin protochloride, 1.35g butter of antimony, 10ml, and transfer pH value between 3-4 with dilute hydrochloric acid; In B part microemulsion, add 325 purpose mica powder 2g, and stirring suspension constantly.
B part solution is warmed to 30 degrees centigrade less, and A part blended microemulsion adds B part lentamente and mixes in the microemulsion, regulates pH value to 7.2 with ammoniacal liquor then, keeps temperature to keep 30 minutes for 30 degrees centigrade.After 36 hours, filtration, washing, drying, calcining get product the throw out that forms through ageing.
This composite conducting particle coats even, complete, and diameter homogeneous (50-10nm), conductivity conduction life-span stable, electrically conducting coating prolong greatly.
Claims (8)
1. method of utilizing microemulsion technology to prepare conducting particles for composite electrically-conducting paint, it is characterized in that utilizing the w/o type microemulsion technology, with mica powder or the bigger material of silica powder specific inductivity is the core material, with tin protochloride is main coating, with the antimony chloride is hotchpotch, be oxygenant with the hydrogen peroxide, be precipitation agent with ammoniacal liquor, the throw out of preparation homogeneous in microemulsion, after filtration, washing, drying and calcining obtain the composite conducting particle; Concrete steps are as follows:
(1) preparation of microemulsion: be controlled under normal temperature 20-30 ℃, the deionized water that accounts for weight of microemulsion 10-20% is added in the 55-65% organic solvent, mix; Add tensio-active agent, the 15-20% cosurfactant of 3-5% then successively, stirring promptly gets microemulsion;
(2) preparation of composite conducting particle: get 50% of above-mentioned microemulsion, add successively by the load weighted tin protochloride of proportioning, butter of antimony, hydrogen peroxide under the normal temperature, stir and make mixed liquor A, and transfer its pH value between 3-4 with dilute hydrochloric acid; In remaining microemulsion, add the core material that weighs by proportioning, and constantly stir, form mixed liquid B; At last mixed liquor A is constantly added in the mixed liquid B, the while continuously stirring, dropping ammonia is regulated pH value to 7-9 after reinforced the finishing, and then the ageing of mixed solution throw out, filtration, drying, calcining is made finished product;
The proportioning of tin protochloride, butter of antimony, hydrogen peroxide and core material is: tin protochloride, butter of antimony, hydrogen peroxide account for the 60%-80% of four gross weights, the core material accounts for 7.89% of four gross weights, wherein the mol ratio of tin protochloride and butter of antimony is 9-10: 1, and the mol ratio of hydrogen peroxide and tin protochloride is 1-1.1: 1.
2. prepare the conducting particles for composite electrically-conducting paint method according to claim 1 is described with microemulsion technology, it is characterized in that described organic solvent is the naphthenic technical grade product.
3. describedly prepare the conducting particles for composite electrically-conducting paint method according to claim 1 or 2, it is characterized in that described naphthenic organic solvent is hexanaphthene, pentamethylene with microemulsion technology.
4. prepare the conducting particles for composite electrically-conducting paint method according to claim 1 is described with microemulsion technology, it is characterized in that described tensio-active agent is anion surfactant or nonionogenic tenside, anion surfactant is the alkyl polyoxyethylene ether sulfate class, alkylbenzene sulfonate; Nonionogenic tenside is alkyl polyoxyethylene ether, alkylphenol polyoxyethylene.
5. prepare the conducting particles for composite electrically-conducting paint method according to claim 1 is described with microemulsion technology, it is characterized in that described cosurfactant is intermediate alcohols technical grade product.
6. describedly prepare the conducting particles for composite electrically-conducting paint method according to claim 1 or 5, it is characterized in that described intermediate alcohols cosurfactant is butanols, amylalcohol with microemulsion technology.
7. prepare the conducting particles for composite electrically-conducting paint method according to claim 1 is described with microemulsion technology, it is characterized in that described tin protochloride, butter of antimony, hydrogen peroxide, ammoniacal liquor are technical grade product.
8. prepare the conducting particles for composite electrically-conducting paint method according to claim 1 is described with microemulsion technology, it is characterized in that described core material is technical grade mica powder, silica powder product, granularity is the 325-600 order.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100400705A CN100383196C (en) | 2006-04-25 | 2006-04-25 | Method for preparing conducting particles for composite electrically-conducting paint using microemulsion technology |
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| CNB2006100400705A CN100383196C (en) | 2006-04-25 | 2006-04-25 | Method for preparing conducting particles for composite electrically-conducting paint using microemulsion technology |
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| CN1865359A CN1865359A (en) | 2006-11-22 |
| CN100383196C true CN100383196C (en) | 2008-04-23 |
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| CN102198951B (en) * | 2010-03-26 | 2013-01-23 | 南京理工大学 | Surface coating method of ammonium salts |
| CN106085114A (en) * | 2016-06-28 | 2016-11-09 | 郭迎庆 | A kind of preparation method of anticorrosion ground connection coating material |
| CN110591503A (en) * | 2019-09-24 | 2019-12-20 | 徐州金亚粉体有限责任公司 | Preparation method of anti-static floor coating |
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| US4621024A (en) * | 1984-12-31 | 1986-11-04 | Paper Applications International, Inc. | Metal-coated hollow microspheres |
| JPS62216105A (en) * | 1986-03-17 | 1987-09-22 | 大塚化学株式会社 | Conductive mica and manufacture of the same |
| JPS62275186A (en) * | 1986-05-23 | 1987-11-30 | Aarefu:Kk | Production of white conductive composite powder |
| JPH05294632A (en) * | 1992-03-27 | 1993-11-09 | Mitsubishi Materials Corp | Production of electrically-conductive powder coated with tin oxide doped with antimony oxide |
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| CN1190645A (en) * | 1997-10-17 | 1998-08-19 | 中国科学院固体物理研究所 | Surface clad nm zinc ferrite corpuscle and corpuscle cooloidal sol preparation method |
| CN1328064A (en) * | 2001-07-16 | 2001-12-26 | 复旦大学 | nm Microspheres of magnetic polymer synthesized by one-step method and its preparing process |
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2006
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4621024A (en) * | 1984-12-31 | 1986-11-04 | Paper Applications International, Inc. | Metal-coated hollow microspheres |
| JPS62216105A (en) * | 1986-03-17 | 1987-09-22 | 大塚化学株式会社 | Conductive mica and manufacture of the same |
| JPS62275186A (en) * | 1986-05-23 | 1987-11-30 | Aarefu:Kk | Production of white conductive composite powder |
| JPH05294632A (en) * | 1992-03-27 | 1993-11-09 | Mitsubishi Materials Corp | Production of electrically-conductive powder coated with tin oxide doped with antimony oxide |
| CN1165782A (en) * | 1997-01-22 | 1997-11-26 | 中国人民解放军国防科学技术大学 | Method for preparing superfined Cr2O3 |
| CN1190645A (en) * | 1997-10-17 | 1998-08-19 | 中国科学院固体物理研究所 | Surface clad nm zinc ferrite corpuscle and corpuscle cooloidal sol preparation method |
| CN1328064A (en) * | 2001-07-16 | 2001-12-26 | 复旦大学 | nm Microspheres of magnetic polymer synthesized by one-step method and its preparing process |
Non-Patent Citations (3)
| Title |
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| Preparation of nanometer-sized (1-x) SnO2 and Sb2O3conductive pigment powders and the hydrolysis behavior ofurea. Tan, Junru, Shen, Lazhen, Fu, Xiansong, Hou, Wenxiang,Chen, Xiuzeng.Dyes and Pigments,Vol.61 No.1. 2004 * |
| 浅色复合导电涂料的开发与应用. 彭德厚等.化学工程师，第10期. 2005 * |
| 聚合物基纳米无机复合材料的最新研究进展. 张艳辉等.化学工业与工程技术，第25卷第6期. 2004 * |
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