CN1552776A - Preparing method for coating liquid of anti-static transparent and high-strength coating - Google Patents
Preparing method for coating liquid of anti-static transparent and high-strength coating Download PDFInfo
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- CN1552776A CN1552776A CNA031290477A CN03129047A CN1552776A CN 1552776 A CN1552776 A CN 1552776A CN A031290477 A CNA031290477 A CN A031290477A CN 03129047 A CN03129047 A CN 03129047A CN 1552776 A CN1552776 A CN 1552776A
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Abstract
A coating liquid for generating antistatic, transparent and high-strength film on the surface of CRT is prepared through preparing the hydroxide sol of electric conducting metal oxide doped by soluble metal salt, preparing the inorganic filming sol from alkoxy silicate or alkyl titanate through hydrolytic polymerizing, mixing at 15-60 deg.C, taking hydrolysis and polycondensation.
Description
Technical field
The present invention relates to a kind of technical field for preparing the coating liquid production method of antistatic, transparent, high-strength coating, this coating liquid is coated on glass or other transparent substrates, prepares antistatic, transparent, high-intensity film.
Background technology
Be commonly used to do cathode ray tube (CRT), insulating material surface resistivitys such as the glass of liquid-crystal display (LCD) or plastics are very high, static charge is easy to build up in the above, the accumulation of electric charge makes koniology, materials such as fiber are attached on the surface of display screen, the result causes display screen to tarnish, the resolving power that shows image reduces, and the people who touches this display screen can be shocked by electricity, the glass bulb transmitance for preparing CRT simultaneously is than higher, the contrast gradient that is unfavorable for showing image improves, need cathode tube outer on glass coat layer of surface resistance lower have antistatic property and a clear films.
The preparation of electro-conductive material is one of key of coating liquid preparation.Electro-conductive material is divided into inorganic and organic two kinds.Polyaniline, polypyrrole and Polythiophene are the representatives of organic conductive polymkeric substance, they have good conductivity, but they are bad to heat, air and ultraviolet stability, United States Patent (USP) 5412279 and 4959162 forms with antistatic coating disclose a kind of polymer application of polypyrrole, though reach electroconductibility preferably, but the coating transparency of manufacturing is lower and be subjected to the corrosion of chemical substances such as ammoniacal liquor easily.Inorganic conductive material is then with the metal oxide (FTO of semiconductor doping; ATO; ITO; ZTO) be main; United States Patent (USP) 5376308; 4945282; 5291097 disclose a kind of antistatic coating solution; wherein electro-conductive material is tin-antimony oxide ATO particle or indium tin oxide ITO particle; the metal oxide suspension preparation of this coating solution is refinement and the dispersion that reaches metal oxide through mechanical means such as grindings; this preparation method's process complexity is (as hydrolysis; filter; clean; baking; pulverize; dealkalize or the like); inefficiency; the cost height; and conductivity and its stability can not be satisfactory, surface resistivity only 10
9-10Ohm/.These need us to develop new processing method to produce coating liquid antistatic, transparent, high-strength coating.
Summary of the invention
Primary technical problem to be solved by this invention is to provide a kind of coating liquid production method antistatic, transparent, high-strength coating that is used to prepare at existing background technology, it can avoid preparing the loaded down with trivial details process of solid nano particulate, method is simple, production efficiency is high, can reduce production costs greatly, and the film that forms with this coating liquid its superperformance is arranged.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind ofly be used to prepare coating liquid production method antistatic, transparent, high-strength coating, it is characterized in that: the hydroxide sol of the conducting metal oxide that adulterated soluble metallic salt makes with form by alkoxyl silicone acid esters or alkyl titanic acid ester hydrolytic polymerization inorganicly become film sol under temperature 15-60 ℃ condition, to mix, and be hydrolyzed and polycondensation has obtained this coating liquid; Above-mentioned its quality of soluble metallic salt that is used for obtaining hydroxide sol will account for the 1-10% of coating liquid total mass, the hydroxide sol its preparation method of conducting metal oxide is a kind of basic solution under agitation to be added in a kind of ethanolic soln of above-mentioned metal soluble salt obtain hydroxide hydrate solution, water and adulterated oxide compound join in this solution then, heated and stirred, temperature remains on 80-90 ℃, reaction can obtain the hydroxide sol of this conductive oxide in 3-4 hour, wherein basic solution adopts ammoniacal liquor or sodium hydroxide or potassium hydroxide solution, its consumption remains between the 9-11 pH value of whole solution, the consumption of water is less than 1% of solution quality, adulterated oxide compound consumption is the 1-10% that is doped the molar weight of thing, and the etoh solvent consumption is to account for 20～50% of coating liquid total mass; Above-mentioned alkoxyl silicone acid esters or alkyl titanic acid ester will account for the 10-20% of coating liquid total mass, inorganic one-tenth film sol its preparation method is alkoxyl silicone acid esters, alkyl titanic acid ester or their mixture to be joined in the alcoholic solvent stir, add then and account for coating liquid total mass 1-7% acidic aqueous solution, its sour content is fully promptly prepared a kind of SiO behind the stirring reaction in mass percent 0.1～0.5%
2Colloidal sol or TiO
2Inorganic sol solution, alcoholic solvent consumption are 20～50% of coating liquid total mass.
The hydroxide sol of above-mentioned conducting metal oxide is the stable dispersions of oxyhydroxide in alcoholic solvent of conducting metal oxide, wherein the oxyhydroxide of conducting metal oxide comprise stannic hydroxide, the stannic hydroxide of mixing antimony of mixing fluorine, the indium hydroxide of mixing tin one or more, be nano-scale particle; This dispersion liquid directly is prepared from from metal salt solution through sol-gel method.
Above-mentioned metal soluble salt comprises stannide, indium thing, Zinc compounds or stibnide, is used for adulterated conductive compound to include stannide, indium thing, Zinc compounds or stibnide.
Above-mentioned alcoholic solvent preferably contains the alcohol of 1～3 carbon atom, and these alcohol can be used alone, but also also mix together, and alcoholic solvent is to mix when using, and contains mass percent 50% or more methyl alcohol under the preferable case in alcohol mixture.
The preferred hydrochloric acid of above-mentioned acidic aqueous solution, nitric acid, sulfuric acid or acetic acid water solution.
It adds 1～5% amide solvent that accounts for the coating liquid total mass above-mentioned inorganic one-tenth film sol in preparation process, the preferred free methane amide of described amide solvent, N-methylformamide, N, dinethylformamide, ethanamide, N-methylacetamide, N, N-N,N-DIMETHYLACETAMIDE, N-methyl propanamide or their mixture.
Above-mentioned alkoxyl silicone acid esters comprises methoxy silane, Ethoxysilane or their mixture, and the titan-alkoxide acid esters comprises titanium ethanolate, butyl (tetra) titanate or their mixture.
Compared with prior art, the invention has the advantages that: can avoid preparing the loaded down with trivial details process of solid nano particulate, can reduce production costs greatly, improved efficient, and processing method is simple, with low cost, it has transmitance greater than 90% film that forms with this coating liquid, and 1 * 10
7-1 * 10
9The surface resistivity of ohm/, and film toughness 200 rear film surface resistivitys under 1 kgf are constant, and have good chemical stability.Film is simply effective, implements easily.
Description of drawings
The structure sectional view of Fig. 1 indicating meter.
Embodiment
Describe in further detail below in conjunction with the drawings and Examples invention.
Fig. 1 is a cross sectional representation, and coating liquid forms antistatic coating 2 on CRT display screen 1 surface.
Electro-conductive material conducting metal oxide of the present invention is to be selected from fluorine doped tin oxide FTO, antimony doped tin oxide ATO, tin-doped indium oxide FTO, to mix among the tin zinc oxide ZTO one or more, wherein, hydroxide sol is to be hydrolyzed and to prepare the stable nano-level conducting hydroxide particles that is scattered in the alcoholic solution by adding a spot of basic solution in the aqueous solution of sol-gel method by the aqueous solution of the solution of these metal soluble salt such as tin tetrachloride, indium chloride.Wherein used alkali comprises ammoniacal liquor NH
3H
2O, sodium hydroxide, potassium hydroxide, its consumption should make the pH value of whole solution between 9～11, and the consumption of water is less than the mass percent 1% of solution.The concentration of this dispersion liquid and the particle diameter of oxide particle are to realize by temperature and stirring velocity, the reaction starting point concentration of control sol gel reaction time, the too low colloidal sol that can not form of stirring velocity is that the hydroxide particles granularity is bigger, and the transparency of solution is very low.Here, the most handy following form of soluble metal salt and organic solvent is used.For example, described solvable mineral compound comprises stannide, as the hydrate (SnCl of stannide
4NH
2O); The indium thing is as indium nitrate hydrate (In (NO
3)
3NH
2O) or indium chloride hydrate (InCl
3NH
2O), Zinc compounds such as zinc chloride (ZnCl
2NH
2O).The usage quantity scope of soluble metallic salt is 1～10% of a gross weight, and as greater than 10% o'clock, the transparency of colloidal sol can reduce when add-on was too much, if be lower than 1%, does not then reach the ideal antistatic effect.Simultaneously, if when compounds such as Sn, In, Zn, Sb are impregnated in wherein, can use antimony chloride (SbCl
3), indium chloride hydrate (InCl
3NH
2O) or tin chloride hydrate (SnCl
4NH
2O), zinc chloride hydrate (ZnCl
2NH
2O).The amount ranges of doped compound be doped thing molar weight 1～10%, if doping is too high, conductivity can reduce on the contrary, doping then can not be improved the conductivity of colloidal sol inadequately.
A kind of inorganic sol that the present invention mentioned is SiO
2Colloidal sol, TiO
2Colloidal sol or their mixture are formed.This colloidal sol is formed by alkoxyl silicone acid esters, alkyl titanic acid ester or their mixture solution and the abundant hydrolysis of acidic aqueous solution.Wherein the alkoxyl silicone acid esters comprises methoxy silane, Ethoxysilane and their mixture; The alkyl titanic acid ester comprises titanium ethanolate, butyl (tetra) titanate.Wherein the consumption of alkyl silicate or alkyl titanic acid ester accounts for 10～20% of gross weight.If silicon ester or titanic acid ester consumption are less than 10% then the intensity of prepared coating is not high, and consumption surpasses at 20% o'clock, the viscosity of whole colloidal sol is excessive, is unfavorable for the coating of coating.Acidic aqueous solution is hydrochloric acid, nitric acid, sulfuric acid or acetic acid water solution, its consumption accounts for 1%～7% of total amount, if the acidic aqueous solution consumption is lower than 1%, then fully hydrolysis of silicon ester or titanic acid ester, film strength is not enough, and consumption surpasses at 7% o'clock, and excessive water can make dissolved adhesiveness stability reduce.Its shelf time shortens.Wherein Suan content is 0.1～0.5%.Solvent for use is the alcohol that contains 1-3 carbon atom, for example methyl alcohol, ethanol, Virahol, n-propyl alcohol.These alcohol can be used alone, but also also mix together.When two kinds of alcoholic solvents mix use, consider dispersing property, contain 50% mass percent or more methyl alcohol in the alcohol mixture under the preferable case.With a spot of acidic aqueous solution join be dissolved in the organic solvent can hydrolysis silicate or titanate material in carry out complete hydrolysis, to form a kind of film forming inorganic sol.
For obtaining quality rete preferably, in this colloidal sol, add a kind of amide solvent and contain intramolecularly amide group (N (R)-C=O, R are alkyl) simultaneously.The used amide solvent of the present invention contains lactan group (N (R)-C=O, R are alkyl).The example of amide solvent comprises methane amide (DMF), ethanamide (AA), N-methylacetamide (NMAA), N,N-dimethylacetamide (DMA), N-methyl propanamide (NMPA) and N-Methyl pyrrolidone (NMP).The amount of institute's amide containing is for accounting for coating liquid mass percent 1-5%.The adding of acid amides can improve conductivity and help the integrity of coating.If amide solvent is lower than 1%, can not improve conductivity, film forming there is not influence.When amide solvent is higher than 5%, can obtain the ideal conductivity, and help the integrity of coating, still, the high boiling point of acid amides makes it still have considerable part to remain in the coating after 150 ℃ of roastings, and is harmful to the stability of coating.
The following description of preparation method of above-mentioned inorganic sol solution, add in the alcoholic solvent and stir accounting for the alkoxyl silicone acid esters, alkyl titanic acid ester of coating liquid quality 10～20% or their mixture, general 1～2 hour, add a kind of coating liquid quality 1～5% amide solvent that accounts for, add the acidic aqueous solution that accounts for coating liquid quality 1～7%, fully stir after 12 hours and promptly prepare a kind of SiO
2Or TiO
2Inorganic sol solution.
Above-mentioned hydroxide sol is inorganicly become the film sol Hybrid Heating to stir to be hydrolyzed and polycondensation forms the composition of coating liquid with above-mentioned.
The present invention may be better understood for following examples of implementation, and these embodiment are used for explaining the present invention, and can not be used for limiting the present invention.
The specified coating coating liquid of table 1 prepares as follows.In one 1 liter glass flask, under violent stirring as 500 rev/mins of speed, a kind of alkoxyl silicone acid esters or the adding of alkyl titanic acid ester are met in the alcoholic solvent of above-mentioned requirements, stir mixed in 1-2 hour after, the acidic aqueous solution that dropwise adds concentration 1% at room temperature stirs after 12 hours and to add a kind of amide solvent and stir and obtain a kind of one-tenth film sol.Under violent stirring, add in a kind of ethanolic soln of above-mentioned soluble salt certain density alkaline aqueous solution, make the pH value of solution reach 9-11, obtain hydroxide hydrate solution, water and adulterated compound join in this solution then, and heated and stirred, temperature remain on 80-90 ℃, reaction can obtain the hydroxide sol of this conductive oxide in 3-4 hour, two kinds of colloidal sols are mixed stirring 2-3 hour, temperature of reaction 15-60 ℃, promptly obtain this coating coating liquid.
The preparation method of coating as follows, the glass screen of cathode tube is cleaned with sanitising agent, use deionized water rinsing, the back alcohol flushing, preheating is 1.5 hours in 40 ℃ baking oven, through form the coating of about 100 nano thickness after the spin coating on the glass screen, this coating was cured under 160 ℃ 30 minutes, took out to be cooled to the every physicals that records this coating after the room temperature.The results are shown in Table 2.
Table 1
| Example | Component | ||||||
| Inorganic sol | The conducting metal hydroxide sol | ||||||
| Alkyl silicate | Acidic aqueous solution | Alcoholic solvent | Amide reagent | SnCl·5H 2O | ?SbCl 3·4H 2O | Alcoholic solvent | |
| ??1 | ????15.5(A) | ????3.2 | ??34(C) | ??2.3(B) | ????6.4 | ????0.2 | ??38.4(C) |
| ??2 | ????18(A) | ????6.1 | ??25.6(E) | ??2.0(B) | ????9.3 | ????0.3 | ??38.7(C) |
| ??3 | ??2(A)+12.6(D) | ????5.4 | ??30.4(C) | ??3.1(B) | ????8.3 | ????0.4 | ??37.8(C) |
| ??4 | ????10.8(D) | ????5.9 | ??43.2(G) | ??1.6(B) | ????5.2 | ????0.1 | ??33.2(C) |
| ??5 | ????12(A) | ????4.5 | ??34.2(G) | ??3.6(F) | ????8.9 | ????0.4 | ??36.4(C) |
| ??6 | ????14(D) | ????4 | ??31.8(C) | ??4.8(F) | ????5.3 | ????0.3 | ??39.8(C) |
| ??7 | ????20(D) | ????4.7 | ??20(C) | ??1.1(F) | ????10 | ????0.9 | ??43.3(C) |
| ??8 | ????14(D) | ????3.4 | ??50(G) | ??3.0(F) | ????3.5 | ????0.1 | ??26.0(C) |
| ??9 | ????17(D) | ????4.0 | ??50(G) | ??2.5(B) | ????1.5 | ????0.1 | ??25.0(C) |
Wherein A-tetraethyl silicate, D-methyl silicate;
B-N, dinethylformamide, F-N, N-N,N-DIMETHYLACETAMIDE;
C-ethanol, E-methyl alcohol, G-n-propyl alcohol;
Table 2
| Example | Test event | ||
| Surface resistivity (ohm/) | Transmitance (%) | Film toughness (1 kilogram force, and resistance after 200 times (ohm/ )) | |
| ????1 | ????3.2×10 8 | ????92.2 | ????3.3×10 8 |
| ????2 | ????2×10 8 | ????93.5 | ????5×10 8 |
| ????3 | ????8.3×10 8 | ????90.2 | ????6.1×10 7 |
| ????4 | ????3.3×10 9 | ????94.4 | ????5×10 9 |
| ????5 | ????4.5×10 7 | ????95.3 | ????7.2×10 9 |
| ????6 | ????1.2×10 9 | ????94.3 | ????2.2×10 9 |
| ????7 | ????3.0×10 9 | ????90.6 | ????5×10 9 |
| ????8 | ????8.5×10 8 | ????97.4 | ????1.0×10 9 |
| ????9 | ????8.0×10 9 | ????93.5 | ????8.2×10 9 |
The mensuration of performance
Surface resistivity: measure by Insulation Resistance Tester device NF2511A
Transmitance: measure at 550 nano wave lengths with ultraviolet-visible pectrophotometer
Film toughness: survey surface resistivity with behind the common eraser 200 times by pressure warning unit control.
Comprehensively described, coating coating liquid of the present invention can be used for outer glass and its transparent substrate of CRT, and the surface resistivity of coating is 1 * 10
7-1 * 10
9Ohm/, transmitance is greater than 90%, and under 1 kgf effect, behind the eraser 200 times, surface resistivity is constant substantially.
Preamble describes the present invention in mode intuitively, is construed as, and described term is to be used for explaining rather than being used for limiting of the present invention.So, should think the protection domain of request of the present invention to the technique means variation that the present invention carries out various further improvement or is equal to.
Claims (9)
1, a kind ofly is used to prepare coating liquid production method antistatic, transparent, high-strength coating, it is characterized in that: the hydroxide sol of the conducting metal oxide that adulterated soluble metallic salt makes with form by alkoxyl silicone acid esters or alkyl titanic acid ester hydrolytic polymerization inorganicly become film sol under temperature 15-60 ℃ condition, to mix, and be hydrolyzed and polycondensation has obtained this coating liquid; Above-mentioned its quality of soluble metallic salt that is used for obtaining hydroxide sol will account for the 1-10% of coating liquid total mass, the hydroxide sol its preparation method of conducting metal oxide is a kind of basic solution under agitation to be added in a kind of ethanolic soln of above-mentioned metal soluble salt obtain hydroxide hydrate solution, water and adulterated oxide compound join in this solution then, heated and stirred, temperature remains on 80-90 ℃, reaction can obtain the hydroxide sol of this conductive oxide in 3-4 hour, wherein basic solution adopts ammoniacal liquor or sodium hydroxide or potassium hydroxide solution, its consumption remains between the 9-11 pH value of whole solution, the consumption of water is less than 1% of solution quality, adulterated oxide compound consumption is the 1-10% that is doped the molar weight of thing, and the etoh solvent consumption is to account for 20～50% of coating liquid total mass; Above-mentioned alkoxyl silicone acid esters or alkyl titanic acid ester will account for the 10-20% of coating liquid total mass, inorganic one-tenth film sol its preparation method is alkoxyl silicone acid esters, alkyl titanic acid ester or their mixture to be joined in the alcoholic solvent stir, add then and account for coating liquid total mass 1-7% acidic aqueous solution, its sour content is fully promptly prepared a kind of SiO behind the stirring reaction in mass percent 0.1～0.5%
2Colloidal sol or TiO
2Inorganic sol solution, alcoholic solvent consumption are 20～50% of coating liquid total mass.
2, coating liquid production method according to claim 1, the hydroxide sol that it is characterized in that described conducting metal oxide is the stable dispersions of oxyhydroxide in alcoholic solvent of conducting metal oxide, wherein the oxyhydroxide of conducting metal oxide comprise stannic hydroxide, the stannic hydroxide of mixing antimony of mixing fluorine, the indium hydroxide of mixing tin one or more, be nano-scale particle; This dispersion liquid directly is prepared from from metal salt solution through sol-gel method.
3, coating liquid production method according to claim 1 is characterized in that described metal soluble salt comprises stannide, indium thing, Zinc compounds or stibnide, is used for adulterated conductive compound to include stannide, indium thing, Zinc compounds or stibnide.
4, coating liquid production method according to claim 1 is characterized in that described alcoholic solvent is the alcohol that contains 1～3 carbon atom, and these alcohol can be used alone, but also also mix together.
5, coating liquid production method according to claim 4 is characterized in that described alcoholic solvent is to mix when using, and contains mass percent 50% or more methyl alcohol under the preferable case in alcohol mixture.
6, coating liquid production method according to claim 1 is characterized in that described acidic aqueous solution is hydrochloric acid, nitric acid, sulfuric acid or acetic acid water solution.
7, coating liquid production method according to claim 1, it is characterized in that described inorganic one-tenth film sol it adds 1～5% amide solvent that accounts for the coating liquid total mass in preparation process, and described amide solvent is selected from by methane amide, N-methylformamide, N, dinethylformamide, ethanamide, N-methylacetamide, N, N-N,N-DIMETHYLACETAMIDE, N-methyl propanamide or their mixture.
8, coating liquid production method according to claim 1 is characterized in that described alkoxyl silicone acid esters comprises methoxy silane, Ethoxysilane or their mixture.
9, coating liquid production method according to claim 1 is characterized in that described titan-alkoxide acid esters comprises titanium ethanolate, butyl (tetra) titanate or their mixture.
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|---|---|---|---|
| CNA031290477A CN1552776A (en) | 2003-05-30 | 2003-05-30 | Preparing method for coating liquid of anti-static transparent and high-strength coating |
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|---|---|---|---|
| CNA031290477A CN1552776A (en) | 2003-05-30 | 2003-05-30 | Preparing method for coating liquid of anti-static transparent and high-strength coating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747670B (en) * | 2008-11-28 | 2012-03-07 | 富港电子（东莞）有限公司 | Preparation method of composite paint and product thereof |
| CN103881430A (en) * | 2014-03-20 | 2014-06-25 | 南京倍立达新材料系统工程股份有限公司 | Dustproof antistatic inorganic composite coating and preparation method thereof |
| CN108884574A (en) * | 2016-03-30 | 2018-11-23 | 东京应化工业株式会社 | The manufacturing method of metal oxide film formation smears and the matrix with metal oxide film |
| CN115247002A (en) * | 2022-08-08 | 2022-10-28 | 安徽锦华氧化锌有限公司 | Preparation method of static conductive zinc oxide |
-
2003
- 2003-05-30 CN CNA031290477A patent/CN1552776A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747670B (en) * | 2008-11-28 | 2012-03-07 | 富港电子（东莞）有限公司 | Preparation method of composite paint and product thereof |
| CN103881430A (en) * | 2014-03-20 | 2014-06-25 | 南京倍立达新材料系统工程股份有限公司 | Dustproof antistatic inorganic composite coating and preparation method thereof |
| CN108884574A (en) * | 2016-03-30 | 2018-11-23 | 东京应化工业株式会社 | The manufacturing method of metal oxide film formation smears and the matrix with metal oxide film |
| CN108884574B (en) * | 2016-03-30 | 2022-10-14 | 东京应化工业株式会社 | Coating agent for forming metal oxide film and method for producing substrate having metal oxide film |
| CN115247002A (en) * | 2022-08-08 | 2022-10-28 | 安徽锦华氧化锌有限公司 | Preparation method of static conductive zinc oxide |
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