CN102838894A - Preparation method for high performance coating - Google Patents
Preparation method for high performance coating Download PDFInfo
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- CN102838894A CN102838894A CN2011101702474A CN201110170247A CN102838894A CN 102838894 A CN102838894 A CN 102838894A CN 2011101702474 A CN2011101702474 A CN 2011101702474A CN 201110170247 A CN201110170247 A CN 201110170247A CN 102838894 A CN102838894 A CN 102838894A
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Abstract
本发明涉及一种含有SixOx-1(OH)y(OR)z醇溶胶高性能涂料的制备方法，具体步骤为搅拌下将醇溶液滴加到正硅酸有机酯Si(OR)4中获得含有结构式为SixOx-1(OH)y(OR)z物质的醇溶胶、将SixOx-1(OH)y(OR)z醇溶胶、成膜组分、颜料和填料以及助剂在溶剂中混合、出料、包装。本发明的高性能涂料，由于二氧化硅以粒径为约1-10nm的没有完全水解的缩合SixOx-1(OH)y(OR)z微细粒子形式存在，其与涂料溶剂的相容性很好，因此可均匀地分散在涂料中，原料存在的悬浮稳定性差、触变性差、光洁度不高等问题也得到很好的解决。The present invention relates to a kind of preparation method that contains Six O x-1 (OH) y (OR) z alcohol sol high-performance paint, and concrete step is to drop alcohol solution to orthosilicate organic ester Si (OR) 4 under stirring Obtaining containing structural formula is the alcohol sol of Six O x-1 (OH) y (OR) z material, with Six O x-1 (OH) y (OR) z alcohol sol, film-forming component, pigment and filler And the additives are mixed, discharged and packaged in the solvent. In the high-performance coating of the present invention, since silicon dioxide exists in the form of incompletely hydrolyzed condensed Six O x-1 (OH) y (OR) z fine particles with a particle diameter of about 1-10 nm, its phase with the coating solvent Capacitance is very good, so it can be evenly dispersed in the paint, and the problems of poor suspension stability, poor thixotropy and poor finish of raw materials have also been well resolved.
Description
Technical field
The present invention relates to a kind of preparation method for coating, relate more specifically to contain Si
xO
X-1(OH)
y(OR)
zThe preparation method of the high-performance coating of alcosol.
Background technology
Nano silicon adds in the coating, both can coating have good hardness and scratch resistance, can keep the transparency of filming again simultaneously.The scrub resistance of raising coating, intensity, hardness etc.; Take into account the anti-ultraviolet aging experimental performance that improves coating, reduce time of drying significantly, and the suspension stability that raw material exists is poor, thixotropy is poor, smooth finish is not high etc., and problem also is well solved.
At present, the nanoparticle in the nano paint often directly adds in the resin matrix with the form of auxiliary agent.Because the particle diameter of nano silicon is little, specific surface energy is big, and it is very easy to reunite in coating or can be dispersed in the coating by pigment, filler embedding.
Summary of the invention
The objective of the invention is to solve above-mentioned deficiency, a kind of preparation method of high-performance coating is provided.The technical scheme that realizes the object of the invention is: a kind of preparation method of high-performance coating may further comprise the steps:
1) stirring is mixed into organic alcohol down positive silicic acid organic ester Si (OR) is housed
4Reactor drum in, dripping dilute acid or diluted alkaline are controlled at room temperature with circulated refrigerated water with temperature of reaction to solution again, stir 10-20min, obtaining to contain structural formula is Si
xO
X-1(OH)
y(OR)
zThe alcosol of sol particles, wherein:
X is the integer greater than 0;
Z is the integer greater than 0;
2x+2=y+z; With
R representes to have the straight or branched alkyl of 2-9 carbon atom, preferably has the straight or branched alkyl of 3-6 carbon atom, more preferably ethyl;
2) with Si
xO
X-1(OH)
y(OR)
zAlcosol, film-forming components, pigment and filler and auxiliary agent mix in solvent;
3) discharging, packing.
The preparation method of above-mentioned high-performance coating, positive silicic acid organic ester Si (OR) in the described step 1)
4Be tetraethoxy, positive isopropyl silicate, a kind of in the positive silicon ester of the tetrabutyl.
The preparation method of above-mentioned high-performance coating, organic alcohol is a kind of in ethanol, propyl alcohol or the butanols in the described step 1).
The preparation method of above-mentioned high-performance coating; Diluted acid is Hydrogen chloride or dilute sulphuric acid in the described step 1), and diluted alkaline is a weak ammonia, and the volumetric molar concentration of Hydrogen chloride or dilute sulphuric acid or weak ammonia is: 0.001-1mol/L; Preferably: 0.01-0.5mol/L, more preferably: 0.05-0.1mol/L.
The preparation method of above-mentioned high-performance coating, in the described step 1) in positive silicic acid organic ester and diluted acid or the diluted alkaline mol ratio of water be 1: 0.1-5 is preferably 1: 0.2-4, more preferably 1: 0.3-3.
The preparation method of above-mentioned high-performance coating, diluted acid or diluted alkaline rate of addition are 0.2-8ml/min in the described step 1), are preferably 0.3-6ml/min, more preferably 0.5-3ml/min.
The preparation method of above-mentioned high-performance coating, Si in the described step 1)
xO
X-1(OH)
y(OR)
zThe structural formula of alcosol is Si
xO
X-1(OH)
y(OR)
zThe particle diameter of sol particles be 1-10nm.
The present invention has positive effect:
(1) preparation method of the present invention is simple, and is easy to operate; (2) the accurate control of the rate of addition through diluted acid or diluted alkaline effectively realizes suppressing the too fast purpose of hydrolysis.Sol particles particle diameter yardstick is controlled below 10nm, and size distribution is even relatively, Si
xO
X-1(OH)
y(OR)
zThe colloidal sol stable performance, do not reunite.
Embodiment
Coating of the present invention comprises following component: A) Si
xO
X-1(OH)
y(OR)
zAlcosol, wherein: x is the integer greater than 0; Z is the integer greater than 0; 2x+2=y+z; Represent to have the straight or branched alkyl of 2-9 carbon atom with R, preferably have the straight or branched alkyl of 3-6 carbon atom, more preferably ethyl; And B) film-forming components; Wherein in the Si of silicon-dioxide
xO
X-1(OH)
y(OR)
zThe weight ratio of alcosol and film-forming components is 1: 15-85 is preferably 1: 20-65, more preferably 1: 25-50.
Si
xO
X-1(OH)
y(OR)
zAlcosol makes through stirring down organic alcohol is added drop-wise in the positive silicic acid organic ester, and the mol ratio of water is 1 in wherein positive silicic acid organic ester and diluted acid or the diluted alkaline: 0.1-5 is preferably 1: 0.2-4, more preferably 1: 0.3-3; Rate of addition is 0.2-8ml/min, is preferably 0.3-6ml/min, more preferably 0.5-3ml/min.Stirring velocity is generally 200-250rpm, for example 200rpm or 250rpm.Organic alcohol is ethanol, propyl alcohol or butanols, drips to carry out at normal temperatures usually.The Si of said alcosol
xO
X-1(OH)
y(OR)
zThe particle diameter of minuteness particle is 1-10nm, for example 1-6nm or 3-9nm.
The film-forming components of in coating of the present invention, using can be any film-forming components that those skilled in the art know, the example is fluorocarbon resin, urethane resin, Synolac, thermosetting acrylic resin, resol, nitro-cotton, chlorinated rubber, pitch, modified rosin resin, thermoplastic acrylic resin etc.Being preferably membrane component is fluorocarbon resin.Be used for fluorocarbon resin of the present invention and be well known to those skilled in the art, the example is PVF, pvdf, vinylidene fluoride-hexafluoropropylene copolymer, hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers, tetrafluoroethylene propylene copolymer, tetrafluoroethylene-vinylidene-PEMULEN TR2 etc.The preferred used fluorocarbon resin of the present invention is selected from pvdf, vinylidene fluoride-hexafluoropropylene copolymer, hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers, tetrafluoroethylene-vinylidene-PEMULEN TR2.
Coating of the present invention also comprises solvent.Solvent for use is common solvent or its mixture, includes but not limited to aromatic hydrocarbons such as YLENE, toluene etc.; Ester class such as ETHYLE ACETATE, butylacetate, Isoamyl Acetate FCC etc.; Alcohols such as butanols, isopropylcarbinol, phenylcarbinol etc.; Ethers such as ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, Ucar 35 diethyl ether etc.; Ketone such as MIBK, methyl phenyl ketone, isophorone etc.Those skilled in the art can be according to the present invention the amount of definite solvent for use such as coating desired properties such as coating property.
Coating of the present invention also can comprise other component that those skilled in the art know, for example pigment; Filler, for example talcum powder, lime carbonate, permanent white, silicon-dioxide etc.; Auxiliary agent, for example skimmer, wetting agent, dispersion agent, emulsifying agent, anti-settling agent, stablizer, anti, flow agent, siccative, anti-sagging agent, softening agent, matting agent, fire retardant, mould inhibitor, sterilant, trapping agent etc.Those skilled in the art can be according to the present invention coating desired properties such as bactericidal property etc. confirm the concrete kind and the consumption thereof of used other component.
With the Si that makes as stated
xO
X-1(OH)
y(OR)
zAlcosol, film-forming components, optional pigment and filler and optional adjuvants are mixed in solvent and are obtained coating of the present invention, wherein in the Si of silicon-dioxide
xO
X-1(OH)
y(OR)
zThe weight ratio of alcosol and film-forming components is 1: 15-85 is preferably 1: 20-65, more preferably 1: 25-50.
Used film forming component, solvent and optional pigment, filler and the auxiliary agent that uses are all as stated.
Can the coating of the present invention that make as stated be sealed, and in dry environment, preserve.Certainly, as far as coating of the present invention, preferred now-making-now-using.
Any appropriate method that can be known by one of skill in the art with application of paints of the present invention in material surface to be coated, for example roller coat, spraying, dip-coating, brushing, blade coating etc.With said application of paints after on the material surface to be coated, choose the Si that in the presence of weak acid, makes in filming wantonly
xO
X-1(OH)
y(OR)
zThe further hydrolysis of minuteness particle, wherein weak acid can for example be formic acid, acetate, propionic acid or oxalic acid, its concentration is 0.1-10 weight %, is preferably 0.5-6 weight %.In further hydrolytic process, because Si
xO
X-1(OH)
y(OR)
zHomodisperse and basic fixed are in filming for minuteness particle, so the condensation degree of hydrolysis gained Nano particles of silicon dioxide can not improve basically, promptly continues to remain about 1-10nm, obtains Nano particles of silicon dioxide uniform distribution final coating therein thus.
(embodiment 1)
Tetraethoxy is added in the reaction kettle; Then; Under the stirring velocity of 250rpm, ethanol is added in the reaction kettle, the Hydrogen chloride that drips 0.05mol/L with the rate of addition of 3ml/min again dropwises continued and stirred 15 minutes in reaction kettle; Temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2O (OH)
2(OR)
4, Si
3O
2(OH)
2(OR)
6, Si
3O
2(OH)
3(OR)
5The water white Si that sol particles is formed
xO
X-1(OH)
y(OR)
zThe alcosol mixture.The particle size analyzer measuring result shows gained Si
xO
X-1(OH)
y(OR)
zThe Si of alcosol
xO
X-1(OH)
y(OR)
zThe particle diameter of minuteness particle is 1-6nm.The weight ratio that pvdf is dispersed in YLENE, butylacetate and isophorone is to form the fluorocarbon resin dispersion system in 7: 2: 1 the mixed solvent, and its solid content is 40 weight %.With gained Si
xO
X-1(OH)
y(OR)
zAlcosol adds in the fluorocarbon resin dispersion system, adds skimmer (commercially available, German Bi Ke BYK-141) again, and flow agent (commercially available, German Bi Ke BYK-333) and mixing obtain coating of the present invention.The gained paint spay-coating is obtained thickness on steel be about 30 microns filming, treat the coating surface drying after, with concentration be the acetic acid aqueous solution of 1.5% (weight) be sprayed at film on, and will film and be placed in the envrionment conditions, so that Si wherein
xO
X-1(OH)
y(OR)
zMinuteness particle further is hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and the gained result sees table 1.
(embodiment 2)
Silicic acid four isopropyl esters are added in the reaction kettle; Then; Under the stirring velocity of 200rpm, propyl alcohol is added in the reaction kettle, the Hydrogen chloride that drips 0.06mol/L with the rate of addition of 6ml/min again dropwises continued and stirred 10 minutes in reaction kettle; Temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2O (OH)
2(OR)
4, Si
3O
2(OH)
2(OR)
6, Si
3O
2(OH)
3(OR)
5The water white Si that sol particles is formed
xO
X-1(OH)
y(OR)
zThe alcosol mixture.The particle size analyzer measuring result shows gained Si
xO
X-1(OH)
y(OR)
zThe Si of alcosol
xO
X-1(OH)
y(OR)
zThe particle diameter of minuteness particle is 2-8nm.The weight ratio that the 2.32kg vinylidene fluoride-hexafluoropropylene copolymer is dispersed in YLENE, butylacetate and isophorone is to form the fluorocarbon resin dispersion system in 7: 2: 1 the mixed solvent, and its solid content is 40 weight %.With gained Si
xO
X-1(OH)
y(OR)
zAlcosol adds in the fluorocarbon resin dispersion system, adds skimmer (commercially available, German Bi Ke BYK-141) again, and flow agent (commercially available, German Bi Ke BYK-333) and mixing obtain coating of the present invention.The gained paint spay-coating is obtained thickness on steel be about 30 microns filming, treat the coating surface drying after, with concentration be the aqueous formic acid of 6% (weight) be sprayed at film on, and will film and be placed in the envrionment conditions, so that Si wherein
xO
X-1(OH)
y(OR)
zMinuteness particle further is hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and the gained result sees table 1.
(embodiment 3)
Silicic acid four positive butyl esters are added in the reaction kettle; Then; Under the stirring velocity of 250rpm, propyl alcohol is added in the reaction kettle, the rate of addition with 0.3ml/min drips 0.1mol/L Hydrogen chloride in reaction kettle again, dropwises continued and stirs 20 minutes; Temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2O (OH)
2(OR)
4, Si
3O
2(OH)
2(OR)
6, Si
3O
2(OH)
3(OR)
5The water white Si that sol particles is formed
xO
X-1(OH)
y(OR)
zThe alcosol mixture.The particle size analyzer measuring result shows gained Si
xO
X-1(OH)
y(OR)
zThe Si of alcosol
xO
X-1(OH)
y(OR)
zThe particle diameter of minuteness particle is 1-10nm.The volume ratio that hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers is dispersed in YLENE, butylacetate and isophorone is to form the fluorocarbon resin dispersion system in 7: 2: 1 the mixed solvent, and its solid content is 40 weight %.With gained Si
xO
X-1(OH)
y(OR)
zAlcosol adds in the fluorocarbon resin dispersion system, adds skimmer (commercially available, German Bi Ke BYK-141) again, and flow agent (commercially available, German Bi Ke BYK-333) and mixing obtain coating of the present invention.The gained paint spay-coating is obtained thickness on steel be about 30 microns filming, treat the coating surface drying after, with concentration be the oxalic acid aqueous solution of 0.6% (weight) be sprayed at film on, and will film and be placed in the envrionment conditions, so that Si wherein
xO
X-1(OH)
y(OR)
zMinuteness particle further is hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and the gained result sees table 1.
(embodiment 4)
Silicic acid four isopropyl esters are added in the reaction kettle; Then; Under the stirring velocity of 200rpm, butanols is added in the reaction kettle, the Hydrogen chloride that drips 0.07mol/L with the rate of addition of 0.5ml/min again dropwises continued and stirred 20 minutes in reaction kettle; Temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2O (OH)
2(OR)
4, Si
3O
2(OH)
2(OR)
6, Si
3O
2(OH)
3(OR)
5The water white Si that sol particles is formed
xO
X-1(OH)
y(OR)
zThe alcosol mixture.The particle size analyzer measuring result shows gained Si
xO
X-1(OH)
y(OR)
zThe Si of alcosol
xO
X-1(OH)
y(OR)
zThe particle diameter of minuteness particle is 3-9nm.The volume ratio that tetrafluoroethylene-vinylidene-PEMULEN TR2 is dispersed in YLENE, butylacetate and isophorone is to form the fluorocarbon resin dispersion system in 7: 2: 1 the mixed solvent, and its solid content is 40 weight %.With gained Si
xO
X-1(OH)
y(OR)
zAlcosol adds in the fluorocarbon resin dispersion system, adds skimmer (commercially available, German Bi Ke BYK-141) again, and flow agent (commercially available, German Bi Ke BYK-333) and mixing obtain coating of the present invention.The gained paint spay-coating is obtained thickness on steel be about 30 microns filming, treat the coating surface drying after, with concentration be the propionic acid aqueous solution of 2% (weight) be sprayed at film on, and will film and be placed in the envrionment conditions, so that Si wherein
xO
X-1(OH)
y(OR)
zMinuteness particle further is hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and the gained result sees table 1.
Performance test
Test event: anti-wiping examination performance, Ginkgo Biloba Leaf Extract
Test result: as shown in table 1 below
Table 1
| The outward appearance of coating | Anti-wiping examination performance improves multiple | The Ginkgo Biloba Leaf Extract time (h) | |
| Embodiment 1 | Smooth | 9 | 600 |
| Embodiment 2 | Smooth | 4 | 350 |
| Embodiment 3 | Smooth | 11 | 660 |
| Embodiment 4 | Smooth | 7 | 450 |
Table 1 shows by coating gained coatingsurface smooth of the present invention, and shows the scrub resistance that improves coating, intensity, hardness etc.; Take into account the anti-ultraviolet aging experimental performance that improves coating.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
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|---|---|---|---|
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|---|---|---|---|
| CN201110170247.4A CN102838894B (en) | 2011-06-23 | 2011-06-23 | Preparation method for high performance coating |
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| CN102838894B CN102838894B (en) | 2014-05-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590209A (en) * | 2015-10-16 | 2017-04-26 | 江苏考普乐新材料有限公司 | Aqueous fluorocarbon coating material and preparation method thereof |
| CN106634563A (en) * | 2016-11-09 | 2017-05-10 | 东南大学 | Non-toxic anticorrosive mildew-proof nano coating as well as preparation and application methods thereof |
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| CN87107834A (en) * | 1986-10-03 | 1988-07-27 | Ppg工业公司 | Organo-siloxane/metal oxide coating |
| US5035745A (en) * | 1990-06-29 | 1991-07-30 | Ppg Industries, Inc. | Ion-exchanged abrasion resistant coatings |
| CN101368066A (en) * | 2008-10-13 | 2009-02-18 | 南京大学 | Organosilane Zinc Rich Coatings |
| CN101985536A (en) * | 2010-10-25 | 2011-03-16 | 江苏考普乐新材料股份有限公司 | Fluorocarbon paint and preparation method thereof |
| CN102079949A (en) * | 2010-12-22 | 2011-06-01 | 李志� | Preparation method of nanometer aerogel heat-insulation coating |
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2011
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| CN87107834A (en) * | 1986-10-03 | 1988-07-27 | Ppg工业公司 | Organo-siloxane/metal oxide coating |
| US5035745A (en) * | 1990-06-29 | 1991-07-30 | Ppg Industries, Inc. | Ion-exchanged abrasion resistant coatings |
| CN101368066A (en) * | 2008-10-13 | 2009-02-18 | 南京大学 | Organosilane Zinc Rich Coatings |
| CN101985536A (en) * | 2010-10-25 | 2011-03-16 | 江苏考普乐新材料股份有限公司 | Fluorocarbon paint and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590209A (en) * | 2015-10-16 | 2017-04-26 | 江苏考普乐新材料有限公司 | Aqueous fluorocarbon coating material and preparation method thereof |
| CN106634563A (en) * | 2016-11-09 | 2017-05-10 | 东南大学 | Non-toxic anticorrosive mildew-proof nano coating as well as preparation and application methods thereof |
| CN106634563B (en) * | 2016-11-09 | 2020-10-23 | 科派股份有限公司 | Nontoxic anticorrosion mildew-proof nano coating and preparation and application methods thereof |
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|---|---|
| CN102838894B (en) | 2014-05-14 |
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Address after: No.1, Binjiang 2nd Road, Binjiang Economic Development Zone, Xinbei District, Changzhou City, Jiangsu Province Patentee after: JIANGSU KFCC NEW MATERIALS Co.,Ltd. Address before: No.1, Binjiang 2nd Road, Binjiang Economic Development Zone, Xinbei District, Changzhou City, Jiangsu Province Patentee before: JIANGSU KFCC NEW MATERIALS CO.,LTD. |
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Address after: No.1, Binjiang 2nd Road, Binjiang Economic Development Zone, Xinbei District, Changzhou City, Jiangsu Province Patentee after: JIANGSU KFCC NEW MATERIALS CO.,LTD. Country or region after: China Address before: No.1, Binjiang 2nd Road, Binjiang Economic Development Zone, Xinbei District, Changzhou City, Jiangsu Province Patentee before: JIANGSU KFCC NEW MATERIALS Co.,Ltd. Country or region before: China |