CN100378181C - Inorganic coating composition regulated by pH value and its preparation method and use - Google Patents

Inorganic coating composition regulated by pH value and its preparation method and use Download PDF

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CN100378181C
CN100378181C CNB200610058599XA CN200610058599A CN100378181C CN 100378181 C CN100378181 C CN 100378181C CN B200610058599X A CNB200610058599X A CN B200610058599XA CN 200610058599 A CN200610058599 A CN 200610058599A CN 100378181 C CN100378181 C CN 100378181C
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coating composition
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金贞夏
李镕珍
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Korea Fine Ceramic Paint Co., Ltd.
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金贞夏
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/05—Alcohols; Metal alcoholates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
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    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/80—Processes for incorporating ingredients
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates

Abstract

The present invention provides an inorganic coating composition capable of drying at ordinary temperatures which has an increased pot life as compared to that of an inorganic coating composition formed by the hydrolysis of an alkoxysilane, and a decreased curing time as compared to that of the inorganic composition, and can be dried at an ordinary temperature, and further can be dried by any one without particular restriction, a process for its production and its use. The inorganic coating composition capable of drying at ordinary temperatures containing 1-40 wt.% of an organoalkoxysilane shown by the general formula: R<SUB>n</SUB>Si(OR<SUP>1</SUP>)<SUB>4-n</SUB>, 0.5-20 wt.% of a colloid oxide converted as a solid in water or an organic solvent as a dispersing medium, 0.1-70 wt.% of an aliphatic lower alcohol, 0.1-3 wt.% of an organic or an inorganic acid, 0.01-20 wt.% of an inorganic filler, 0.01-40 wt.% of an inorganic pigment, and 0.1-5 wt.% of a pH stabilizer which is composed of an alkaline solution and/or a buffer solution.

Description

Inorganic coating composition and compound method and the purposes of utilizing the pH value to regulate
Technical field
The present invention relates to exsiccant inorganic coating composition and compound method and the application at normal temperatures of a kind of employing pH value control method, relate in particular to and a kind ofly form inorganic coating composition and compound method and the application that fine inside/outside decorative material for building is filmed by being coated on surfaces such as metal, nonmetal, glass, plastics, cement, slabstone.
Background technology
Generally, attractive in appearance ornamental, the thermotolerance that provides by coating on product surfaces such as metal such as stainless steel, aluminium alloy and cement, glass, plastics, paper, sclerosis inorganic paint, weathering resistance, stain resistance, high rigidity, water tolerance, adhibit quality, solidity to corrosion, weather resistance, cold-resistant hot etc. functional coating have been popularized and have been applied in each field, openly announce at Japanese Patent in " 51-2736 ", " 53-130732 ", " 64-168 " and the Korea S " special 2000-0010246 " etc. and introduce.
But, the inorganic coating composition of being introduced is as if the perfect physical properties that will obtain as inorganic coating film, just must heat-treat (more than at least 50 ℃), therefore need expand extra Special Equipment in order to dry (thermal treatment) operation, thereby cause that equipment is restricted, production cost rises.
Though also introduced in Korea S's publication number " special 1990-0009898 " by dropping into the serial inorganic coating composition of metal alkoxide (alkoxide) that organic and inorganic acid changes colloid pH value and is hydrolyzed, but, this method becomes acid owing to only being confined to drop into the ripe liquid coating that organic and inorganic acid causes hybrid agent and stiffening agent, thereby because of polycondensation makes effective storage life short, and owing to the pH value influence of basic color or stopping composition causes being easy at several days inner gels (GEL) and rotten.And because this method is to be hydrolyzed with main body after, the mineral acid organic by adding in stiffening agent, therefore other maturation time and the stirring of needs grasped maturation time and use so be not suitable for general tyro.
Japanese Patent openly announce " 1998-268772 " also stated silicon alkoxide (silicone alkoxide) as main component near under the room temperature by the hardened coating-forming agent, but only use hardening catalyst also can cause the bad preservation of coating simply and make coated membrane be easy to generate crackle.And humidity slightly changes setting time is just had a significant impact.
Korea S " special 1999-0007963 " also stated room temperature vulcanizing and heat hardening all can coating composition, and introduced the using method of the multipolymer acrylic resin of the oligomer solution of hydrolyzable alkoxy TMOS (alkoxy silane) and acrylate and methacrylic ester, but this method causes effective storage life short because of the variation of pH value, and owing to comprising large amount of organic matter hardness, weathering resistance and thermotolerance is reduced.
Have the pH value of acidity-slightly acidic scope as the coating major part of hydrolyzable alkoxy TMOS in the above-mentioned inorganic coating composition, this will cause continuing polycondensation takes place and the effective storage life that shortens coating, bring difficulty to construction thus.
Summary of the invention
The present invention is in order to solve as above problem and propose, its purpose is to provide a kind of inorganic coating composition of exsiccant at normal temperatures and compound method and application, wherein, the pH value of keeping and regulating coating by more than one solution that in the inorganic coating composition of hydrolyzable alkoxy TMOS, add selection from basic solution or buffered soln (buffer solution), not only increased effective storage life thus and shortened setting time, but also can in Air drying, not have special restriction and can make anyone apply operation.
Description of drawings
Fig. 1 is the block diagram of expression blending process of the present invention.
Embodiment
Coating composition provided by the present invention comprises: with general formula R nSi (OR ') 4-nThe organoalkoxysilane of (R is that carbon number is 1～6 alkyl in the formula, and R ' is that carbon number is that 1～5 alkyl or carbon number are 1～4 acyl group) expression, weight percent is 1～40; With water or the organic solvent colloid oxide compound as dispersion medium, the weight percent that is scaled solid shape powder is 0.5～20; The rudimentary aliphatic alcohol of more than one that from the group that comprises methyl alcohol, ethanol, propyl alcohol, Virahol, n-butanols, isopropylcarbinol composition, select, weight percent is 0.1～70; The organic/inorganic acid of more than one that from the group that comprises phosphoric acid, hydrochloric acid, sulfuric acid, nitric acid, acetate, formic acid composition, select, weight percent is 0.1～3; The inorganic fillings of more than one that from the micropowder of the whisker that comprises potassium titanate, aluminium borate whisker, aluminum oxide, silicon nitride, silicon carbide, silicon-aluminium and glass fibre, carbon fibre and antibiotic micropowder of porous inorganic and inorganic inhibitor, select, weight percent is 0.01～20; More than one mineral dyes of in the nontoxicity pearly pigment of the titanium oxide pigments of rutile structure and mica-titanium oxide base, selecting, weight percent is 0.01～40; The pH value is become the pH value stabilization agent of neutral range, and weight percent is 0.1～3.
Below describe the present invention with reference to the accompanying drawings in detail, Fig. 1 is the block diagram of expression blending process of the present invention.The present invention reacts it put into colloid oxide compound and organic and inorganic acid in organoalkoxysilane after, and use ball mill (ball mill), sand mill pulverizers such as (sand mill) to stir after in above-mentioned reaction solution, adding alcohol, stopping composition and pigment, so that its mean particle size reaches below the 10 μ m, then with pour basic solution into after the alcohol wash, buffered soln makes the pH value stabilization, stir then and use so that it does not produce throw out.
Aforesaid the present invention substantially with single liquid type as the basis, but the two liquid mixed type inorganic paints that can utilize pigment portion and resin portion to separate as required come hydrolysis metal alkoxide silane, and be used alone or as a mixture as buffered soln (buffer solution) in the basic solution between pH value=7.5～10 of pH value stabilization agent or pH value=6.5～7.3 scopes formed by conjugate acid and conjugate base thereof and the weight percent that adds to be 0.1～5, can to stablize the pH value thus.Promptly, can be divided into the alcohol type solvent and with ball mill, sand mill and stir the pigment portion of stopping composition and pigment and by adding the resin portion of pouring basic solution and buffered soln after organic, mineral acid reacts it in organoalkoxysilane and the colloid oxide compound, can use with two liquid mixed types, and the preservation period of aforesaid two liquid mixed type inorganic paints is longer.
Above-mentioned organoalkoxysilane general formula R nSi (OR ') 4-n(R is that carbon number is 1～8 alkyl in the formula; R ' is that carbon number is that 1～5 alkyl or carbon number are 1～4 acyl group) expression; the exemplary of organoalkoxysilane has methyltrimethoxy silane (methyl trimethoxysilane); Union carbide A-162 (methyltriethoxysilane); ethyl trimethoxy silane (ethyltrimethoxysilane); ethyl triethoxysilane (ethyl triethoxysilane); n-propyl-triethoxysilicane (propyltriethoxysilane); I-propyl trimethoxy silicane (propyltrimethoxysilane); phenyltrimethoxysila,e (phenyltrimethoxysilane); phenyl triethoxysilanes (phenyltriethoxysilane) etc. use more than one above-mentioned organoalkoxysilane.
Above-mentioned colloid oxide compound adds for the hydrolyzable alkoxy TMOS, utilizes water and/or organic solvent as dispersion medium, and in addition, this colloid has wear resistance and is divided into acidic gum and alkaline colloid.
Even that above-mentioned acidic gum does not add in addition is organic, mineral acid also can the hydrolyzable alkoxy TMOS, thereby use pH value and the adjusting setting rate that more than one basic solutions or buffered soln can stable composition after the hydrolysis, the ST-0 that the daily output chemistry is arranged as typical acidic gum, 0-33, Al 2O 3Zol-100, Al 2O 3Zol-200, NAYCOL 2034DI, LUDOX SK, TMA, CL, the SN of Japanese Catalysts ﹠ Chem Ind Co etc.
Composition is acidity when using this acidic gum.The coating composition of the hydrolysis of acid, weakly acidic organoalkoxysilane is owing to continue to take place polycondensation, thereby shortens the effective storage life of coating.And because of the effect of pigment, inorganic fillings etc. changes its pH value easily, thereby the effective storage life of hydrolysis composition is shorter.If surpass the effective storage life of coating, then film is difficult to sclerosis, and variety of issues such as coating, gloss, physical properties reduction occur.These problems can overcome by adding more than one solution in selected basic solution or the buffered soln and regulating the pH value.
Above-mentioned alkaline colloid is different with acidic gum, and the needs interpolation is organic, mineral acid is hydrolyzed.At this moment the organic and inorganic acid of Tian Jiaing has acetate, formic acid, carbonic acid, phosphoric acid, oxalic acid, sulfuric acid, nitric acid, hydrochloric acid, tosic acid (para-toluenesulfonic acid) etc., and wherein acetate, formic acid especially are fit to use volatility preferably.The weight percent of addition is 0.01～3, is not easy to be hydrolyzed less than 0.01% o'clock, violent reaction takes place and add 3% when above, thereby shortens effective storage life and pungency is arranged because of the distinctive taste of organic acid.As above-mentioned alkaline colloid daily output chemical ST-20, ST-30, ST-40LUDOX HS-30, HS-40, the SI-45P of Japanese Catalysts ﹠ Chem Ind Co, SI-80 etc. are arranged.
In above-mentioned alkaline colloid, put into organic and inorganic acid and make the reaction that is hydrolyzed of itself and organoalkoxysilane after forcing to make acidic gum, pour basic solution, buffered soln then into.Utilize basic solution, buffered soln to make it stable, the Air drying method is identical with acidic gum.
Above-mentioned buffered soln adds for stable, whole compositions of cold setting.Weak acid and mixed salt solution thereof or weakly alkaline and mixed salt solution thereof etc. have such characteristic, that is, also can change hardly even add the pH value of small amount of acid or alkali or its solution of thin up.Sort buffer solution is neutral or approaches neutrality, thereby prevents coating from further polycondensation taking place and increase considerably the effective storage life of coating.And, because the volatilization rapidly in filming of the organic acid in the buffered soln, thereby make to film and become alkalescence and make it can be at normal temperatures dry during coating composition.
PH value=6.5～7.3 of above-mentioned buffered soln, preferably pH value=6.8～7.When the pH value less than 6.5 the time because coating continues to take place polycondensation, thereby shorten the effective storage life of coating, when pH value greater than 7.3 the time, because reaction carries out with particle state, thereby easy gel (GEL).
Use the reason of above-mentioned buffered soln to have two kinds substantially, one of its reason is for as mentioned above, thereby prevents that by stablizing the pH value by the basic color in the coating or stopping composition, colloid oxide compound coating pH value being changed makes coating rotten; It is former two to be that the conjugate acid of buffered soln volatilizees easily when the application composition therefore.If conjugate acid volatilizees rapidly, then the function of pH value stablize in buffered soln forfeiture, and makes the alkalize of filming because of only remaining basic salt or conjugate base.The filming easy gel (GEL) of alkalize and make the sclerosis of filming, thereby be suitable for Air drying type coating.Even there is not other drying unit, under normal temperature (10～30 ℃), just can be in the hardening state that available hand touches through 30 minutes after the application, spend five days approximately and afterwards can obtain complete hardened coating film.
The acid that is used for described buffered soln has acetate, formic acid, carbonic acid, phosphoric acid, oxalic acid, sulfuric acid, nitric acid, hydrochloric acid, tosic acid etc., preferably uses weak acid (pH=3～6.5).If use strong acid (pH=1～3), then be difficult to obtain buffered soln pH=6.5 of the presently claimed invention～7.2, and owing to be easy to exceed buffering range (buffer region), thereby be easy to make the stability of coating to be affected.And most of strong acid (hydrochloric acid, sulfuric acid, nitric acid) is therefore preferably avoided using even adopt the amount of a little also harmful and pungency arranged.Preferably use human body nonirritant and evaporable acetate or formic acid easily.
The alkaline metal salt or the alkaline earth salt that add with acid during preparation buffered soln have lime acetate, potassium acetate, lithium acetate, sodium acetate, magnesium acetate, formic acid calcium, potassium formate, formic acid lithium, sodium formate, formic acid magnesium, potassiumphosphate, calcium phosphate, Trilithium phosphate, sodium phosphate, trimagnesium phosphate, nitrocalcite, SODIUMNITRATE, lithium nitrate, saltpetre, magnesium nitrate, sal epsom, calcium sulfate, sodium sulfate, Lithium Sulphate, vitriolate of tartar, yellow soda ash, lime carbonate, salt of wormwood, magnesiumcarbonate, Quilonum Retard etc.Wherein, volatility better and be easy to become neutral acetate metal-salt and formic acid metal-salt to be fit to use buffer preparation.Vitriol or Nitrates use sulfuric acid, nitric acid as conjugate acid, but harmful because of it, thereby are not suitable for using.
Preferably that alkyl is less acetate (CH 3COOH) and conjugate base potassium acetate (CH 3COOK) salt mixes and is dissolved in the ionized water and uses, perhaps formic acid (HCOOH) and conjugate base sodium formiate (HCOONa) thereof or potassium formiate (HCOOK) salt are mixed and be dissolved in the ionized water, the weight percent that buffered soln adds in the whole coating composition is in 0.1～5, and the weight percent of interpolation is preferably 0.1～3.When weight percent less than 0.1 the time, can not stablize and fixed pH value, and because of the alkalescence of pigment or stopping composition makes the pH value of whole coating change easily, when weight percent surpasses 5, the water tolerance variation of filming, and influence job morale because of the organic acid smell of uniqueness.
The kind of buffered soln is innumerablely many in the reality, according to embodiment these buffered soln is described exemplarily below.
Embodiment 1
Suppose to utilize the H about pKa value=6.1 2CO 3(carbonic acid) comes the buffered soln of secure ph=6.8, and then carbonic acid is that benchmark is with H with pKa value=6.1 2CO 3And HCO 3 -Two kinds of forms exist, here H 2CO 3Be conjugate acid, HCO 3 -It is conjugate base.
Acid with above-mentioned relation is called conjugate acid, and acid group is called conjugate base.When conjugate acid (proton can be offered the chemical seed (ion or neutral molecule) of acid group) that mixes same amount and conjugate base (can accept the chemical seed (neutral molecule or ion) of proton), the pH value of buffered soln is identical with the pKa value.That is H, 2CO 3And HCO 3 -Amount when identical, it is identical with the pKa value 6.1 that the pH value becomes, and for the buffered soln of secure ph=6.8, conjugate base is more than conjugate acid.What specifically will have more can be obtained according to Henderson-Hasellbach equation.
PH=pKa+log (conjugate base/conjugate acid)
PKa=6.1, because needed pH value=6.8, so 6.8=6.1+log (conjugate base/conjugate acid)
About log (conjugate base/conjugate acid)=0.7, about (conjugate base/conjugate acid)=5.
Therefore, utilize the carbonic acid can be according to conjugate base (HCO 3 -): conjugate acid (H 2CO 3After mixing, the ratio of)=5: 1 obtains the carbonate buffer solution of needed pH value=6.8.
Embodiment 2
Can utilize organic acid+basic metal or alkaline-earth metal as another kind of buffered soln.Suppose to utilize the buffered soln of acetate and salt secure ph=6.8 thereof, be after the sodium acetate solution 100ml of the acetic acid solution 100ml of 0.1M and salt 0.1M thereof then, any one solution slowly poured in the remaining solution and with the pH value as reference solution be adjusted to 6.8 by the preparation conjugate acid.
The solution that contains above-mentioned two kinds of materials can be with the pigment of slowly discharging from coating or the acid or the acid group neutralization of stopping composition.
If add acid in the coating of interpolation buffered soln again, then because the H that is added +With CH 3COO -React and generate CH 3COOH, so the pH value of solution is almost constant.
CH 3COO -+H +→CH 3COOH
If acid group is added in the buffered soln, then the OH that is added -With H 3O +Neutralization reaction takes place make H 3O +Reduce, thereby balance moves to the right and make the pH value of solution almost constant.
CH 3COOH+OH -→CH 3COO -+H 2O
The purpose of adding above-mentioned basic solution is, thereby the pH value of coating is adjusted to neutrality increase effective storage life, when using the acidic gum compositions formulated, the meeting appearance only is difficult to be adjusted to the situation (strongly-acid) of neutrality (pH value=6.5～7.2) with a spot of buffered soln, this moment a spot of by adding in addition (weight percent is 0.01～5, preferably 0.01～2) basic solution (pH value=7.5～10) thus carry out neutralization reaction increase effective storage life.Above-mentioned typical basic solution has ammonia soln, sodium carbonate solution, calcium carbonate soln, magnesium hydroxide solution, sodium hydroxide solution, potassium hydroxide solution, barium hydroxide solution, lithium hydroxide solution etc.At this moment because strong alkali solution is not only harmful, even and add minute quantity and also can make the variation easily of pH value, ammonia soln or sodium carbonate solution as weakly alkaline solution are preferably used in thereby the bad adjustment of the neutral range of coating thus.
Though the pH value that described basic solution or buffered soln can stable compositions, the better effects if of buffered soln.Its reason is, have the factor that much is subjected to the influence of pigment or stopping composition and makes the pH value variation of coating in the composition, but buffered soln is subjected to the influence of these pigment or stopping composition hardly, thereby can keeps the pH value.
Above-mentioned alcohol uses as dispersion solvent, and it comprises methyl alcohol, ethanol, propyl alcohol, Virahol, n-butanols, isopropylcarbinol etc., selects a kind of or two or more uses therein.
Adding above-mentioned inorganic fillings is the hardness of filming in order to improve, prevent to film split, coating precipitation etc., usually use the whisker of potassium titanate, aluminium borate whisker, aluminum oxide, silicon nitride, silicon carbide, silicon-aluminum oxide etc. and micropowder and the antibiotic micropowder of porous inorganic (Korean Patent " the 145990th ") and the inorganic inhibitor etc. of glass fibre, carbon fibre etc., wherein a kind of or two or more of use.
It is nontoxicity pearly pigment, aluminum paste, the Stainless Steel Powder slurries (Stainless Steel Paste) etc. such as mineral dyes such as titanium oxide, mica-titanium oxide base of rutile (Rutile) structure of 0.03～20 μ m that above-mentioned mineral dye uses the average particle diameter of extensively being sold, and generally selects a kind of or two or more uses therein.
Be contained on the product made as the metal that is coated object, nonmetal, cement, by cement, glass, plastics, the paper etc. by being coated with as the above-mentioned present composition, thereby be applicable on all material that requires heat-resisting, weather-proof, water-fast, anti-corrosion, high rigidity, durable, anti-pollution, decorative effect aluminium and aluminium alloy, Stainless Steel Alloy, hot melt zinc/gold-plated steel plate, hot melt aluminium/gold-plated steel plate, titanium steel plate etc. are arranged as typical metal object.
Followingly describe the present invention in detail according to embodiment.
Embodiment 3
In organoalkoxysilane, put into colloid silica, be hydrolyzed after colloid aluminum oxide and the organic acid, add whole alcohol (methyl alcohol, Virahol, ethanol) then two minutes one, and put into and use ball mill, sand mill etc. to stir after stopping composition (inorganic antibacterial material, inorganic inhibitor, other stopping composition) and the pigment to make it mean particle size less than 10 μ m, use then after 1/2nd remaining alcohol clean, pour in the buffered soln and fully stir and make it not produce throw out.If mean particle size reaches more than the 10 μ m, can reduce ornamental and stain resistance, so stir during the application composition and make it not produce throw out.
Embodiment 4
In organoalkoxysilane, put into colloid silica, be hydrolyzed after colloid aluminum oxide and the acid, add 1/3rd of whole alcohol then, pour buffered soln into afterwards and generate resin portion,
In 1/3rd alcohol of whole alcohol amounts, put into after stopping composition (inorganic antibacterial material, inorganic inhibitor, other stopping composition) and the pigment, use stirrings such as ball mill, sand mill to make it mean particle size less than 10 μ m, utilize 1/3rd alcohol that are left to clean and generate pigment portion then, afterwards, described resin portion of uniform mixing and pigment portion carry out application then when using coating.
The composition ratio of the inorganic paint coating composition that generates according to the foregoing description 3 and embodiment 4 has been shown, in [table 1] shown in the experimental result following [table 2] of the effective storage life of these compositions pH value and setting time.
[table 1]
Embodiment
Form (portion) A B C D E F G H I
Organoalkoxysilane 15.9 37.9 24.7 32.3 35.7 19.6 25.5
Tetraalkoxysilane 4 22.8 6.6 5 36.5
Colloid silica 14.4 *1) 31.9 *2) 16.0 *3) 18 *4) 8.8 *5) 15.7 *6) 27.9 *2) 20.0 *3)
The colloid aluminum oxide *a) 5.0 1.5 *1) 1.1 16.4
Methyl alcohol 12.6 12.0 18.3 19.2 12 12.0
Virahol 20.8 16.0 17.0 12 14.1 34.8 23.4 17.8
Organic and inorganic acid *b) 0.1 *b) 0.2 *g) 0.1 *b) 0.6 *g) 0.2 *g) 0.1 *b)
The inorganic antibacterial material *c) 1.2 0.4 2.1 0.4
Inorganic inhibitor *d) 1.0 2.6 4.2
Other inorganic fillings *e) 2.2 0.01 6.8 6 0.8 4.4 2.2 0.01 0.8
Mineral dye 21.8 0.01 32.9 16.2 14 24.1 21.8 0.01 32.9
Basic solution 0.1 *C) 0.1 *D)
Buffered soln 1 *A) 2 *A) 2.5 *A) 1 *A) 2 *A) 2.5 *A) 1 *A) 2 *A) 2.5 *A)
Add up to 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0
Embodiment
Form (portion) J K L M N O P Q R
Organoalkoxysilane 25.9 5.8 22.3 22.3 35.7 15.9
Tetraalkoxysilane 25.2 21.5 25.8 6 4 36.3
Colloid silica 18 *4) 10.8 *5) 9.6 *6) 14.4 *1) 16.0 *3) 28 *4) 14.4 * 5) 9.6 *6)
The colloid aluminum oxide *a) 19.4 15.2 5.0
Methyl alcohol 12.0 20.3 19.2 12 9.6
Virahol 24.8 16.0 25.0 12 14.1 24.8 13
Organic and inorganic acid *b) 0.1 *b) 0.3 *g) 0.1 *b) 0.6 *g) 0.1 *b)
The inorganic antibacterial material *c) 1.2 0.8 2.1 3.2 1.2 1
Inorganic inhibitor *d) 1.0 2.6 1.0
Other inorganic fillings *e) 6.2 5.5 1.8 6 2.8 4.4 9 2.2 19
Mineral dye 21.8 28.4 32.9 18.6 20 23.5 24 21.8 21
Basic solution 0.1 *C) 0.1 *D) 0.1 *c) 0.1 *D)
Buffered soln 1 *A) 2 *A) 2.5 *A) 0 0 0 0 0 0
Add up to 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0
*A) Al of Japanese Nissan chemical industry Co., Ltd. 2O 3Zol-100
*B) formic acid ((HCOOH=46.03))
*C) Korean Patent " No. 145990 " multi-hole type inorganic antibacterial micropowder
*d)GERMANY NYCO MINERALS，INC.Wollastonite
*E) big tomb timosu-D of pharmaceutical chemicals Co., Ltd. of Japan and German Degussa Al 2O 3Oxcide-C
*F) Al of Japanese Nissan chemical industry Co., Ltd. 2O 3Zol-200
*G) acetate ((CH 3COOH=60.05)
*1) SNOWTEX-30 of Japanese Nissan KCC
*2) SNOWTEX-40 of Japanese Nissan KCC
*3)USA DuPont Ludox collidal silica HS-40
*4)USA DuPont Ludox collidal silica CL-X
*5) the Japanese SN of Catalysts ﹠ Chem Ind Co
*6) the Japanese OSCAL IPA-ST of Catalysts ﹠ Chem Ind Co
*A) HCOOH+HCOOK+H 2O buffered soln
*B) CH 3COOH+CH 3COOK+H 2O buffered soln
*C) 3% NH 4The OH basic solution
*D) 3% Na 2CO 3Basic solution
[table 2]
The preparation composition Effective storage life Time of drying Complete setting time Coating pH value Remarks
A 79 days 30 minutes 5 days pH＝6.8
B 86 days 35 minutes 5 days pH＝7
C 77 days 28 minutes 5 days pH＝7
D 68 days 35 minutes 5 days pH＝7
E 86 days 30 minutes 5 days pH＝7
F 73 days 30 minutes 5 days pH＝7
G 54 days 43 minutes 5 days pH＝6.7
H 94 days 18 minutes 5 days pH＝7
I 78 days 26 minutes 5 days pH＝7
J 87 days 30 minutes 5 days pH＝7
K 103 days 31 minutes 5 days pH＝7
L 73 days 30 minutes 5 days pH＝7
M 6 days 2 hours 9 days pH＝5.8 No buffered soln
N 8 days 2 hours 8 days pH＝6.1 No buffered soln
O 5 days 2 hours 20 minutes 14 days pH＝5.1 No buffered soln
P 65 days 34 minutes 7 days pH＝6.9 No buffered soln adds basic solution
Q 77 days 31 minutes 8 days pH＝7 No buffered soln adds basic solution
R 21 days 1 hour 7 days pH＝6.5 No buffered soln
As above-mentioned [table 2] as can be known, the effective storage life of coating and setting time are subjected to the influence of coating pH value bigger.Though it is different according to kind, but as shown in table 2, add the composition of basic solution, buffered soln and can preserve 2.5 months at dark cold place, can preserve 3 months at most, during longer if desired storage life described resin portion and pigment portion are separately preserved, then can preserve more than 6 months.On the contrary, by showing can confirm not pour into the M of buffered soln, N, O, R composition not only effective storage life are short, and sclerosis is also slower.And only put into the composition of basic solution, though the pH value of coating is more stable, compare with the composition of pouring buffered soln into or pouring basic solution+buffered soln into, at normal temperatures slow-drying.
And, having carried out physical property test after the composition according to the method application described [table 1] of [table 3] below, its result is shown in [table 4].
[table 3]
NO Use the composition title Title material Coating process Curing condition
a Table 1, preparation composition A The gold-plated steel plate of heavy wall hot melt zinc Spraying Normal temperature/10 day
b Preparation composition B The gold-plated steel plate of heavy wall hot melt aluminium Spraying Normal temperature/10 day
c Preparation composition C Stainless steel Spraying Normal temperature/10 day
d The preparation components D Aluminium alloy Spraying Normal temperature/10 day
e Preparation composition E Slabstone Cylinder Normal temperature/10 day
f Preparation composition F Plasterboard Cylinder Normal temperature/10 day
g Preparation composition G Glass Spraying Normal temperature/10 day
h Preparation composition H Titanium steel plate Spraying Normal temperature/10 day
i Preparation composition I Concrete Cylinder Normal temperature/10 day
j Preparation composition J The gold-plated steel plate of heavy wall hot melt zinc Spraying Normal temperature/10 day
k Preparation composition K The gold-plated steel plate of heavy wall hot melt aluminium Spraying Normal temperature/10 day
l Preparation composition L Stainless steel Spraying Normal temperature/10 day
m Preparation composition M Aluminium alloy Spraying Normal temperature/30 day
n Preparation composition N Slabstone Cylinder Normal temperature/30 day
o Preparation composition O Plasterboard Cylinder Normal temperature/30 day
p Preparation composition P Glass Spraying Normal temperature/10 day
q Preparation composition Q Titanium steel plate Spraying Normal temperature/10 day
r Preparation composition R Concrete Cylinder Normal temperature/30 day
[table 4]
a b c d e f g h i
Pencil hardness 8H 7H 9H 9H 8H 7H 7H 9H 9H
Glossiness 45 53 52 56 32 38 60 59 36
Adhesion 100/1 00 100/1 00 100/1 00 100/1 00 100/1 00 100/1 00 100/1 00 100/10 0 100/10 0
Bendability ○ ○ ○ ○ - - ○ △ -
Shock-resistance ○ ○ ○ ○ △ ○ ○ ○ △
Thermotolerance ○ ○ ○ ○ ○ ○ ○ ○ ○
Stain resistance I ○ ○ ○ △ ○ ○ ○ ○ ○
Stain resistance II ○ ○ ○ ○ ○ ○ ○ ○ △
Alkali resistance ○ ○ ○ ○ ○ ○ ○ ○ ○
Acid resistance ○ ○ ○ ○ ○ ○ ○ ○ ○
CAS S ○ ○ ○ ○ ○ ○ ○ △ △
Resistance to salt water ○ ○ ○ ○ ○ ○ ○ ○ ○
Pin hole ○ ○ ○ ○ ○ ○ ○ ○ ○
Weather-proof ○ ○ ○ ○ ○ ○ ○ ○ ○
The property
Flame resistivity Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level
Resistance to boiling water ○ ○ ○ ○ ○ ○ ○ ○ ○
Water tolerance ○ ○ ○ ○ ○ ○ ○ ○ ○
Dissolubility resistent ○ ○ ○ ○ ○ ○ ○ ○ ○
j k l m n o p q r
Pencil hardness 8H 7H 7H 8H 8H 8H 7H 9H 8H
Glossiness 48 56 46 54 30 35 56 61 33
Adhesion 100/1 00 100/1 00 100/1 00 100/1 00 100/1 00 100/1 00 100/1 00 100/10 0 100/10 0
Bendability ○ ○ ○ ○ - - ○ △ -
Shock-resistance ○ △ ○ ○ △ ○ ○ ○ △
Thermotolerance ○ ○ ○ ○ ○ ○ ○ ○ ○
Stain resistance I ○ ○ ○ △ ○ ○ ○ ○ ○
Stain resistance II ○ ○ ○ ○ ○ ○ ○ ○ ○
Alkaline-resisting ○ ○ ○ ○ ○ ○ ○ ○ ○
The property
Acid resistance ○ △ ○ ○ ○ ○ ○ ○ ○
CAS S ○ ○ ○ ○ ○ ○ ○ ○ ○
Resistance to salt water ○ ○ ○ ○ ○ ○ ○ ○ ○
Pin hole ○ ○ △ ○ ○ ○ ○ ○ ○
Weathering resistance ○ ○ ○ ○ ○ ○ ○ ○ ○
Flame resistivity Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level Anti-combustion one-level
Resistance to boiling water ○ ○ ○ ○ ○ ○ ○ ○ ○
Water tolerance ○ ○ ○ ○ ○ ○ △ ○ ○
Dissolubility resistent ○ ○ ○ ○ ○ ○ ○ ○ ○
Zero: the no abnormal △ of appearance of film: trickle crackle or slight corrosion
*: crack, exfoliation corrosion (substandard products)-: cannot do experiment or meaningless
*Test method and relevant specification
*Pencil hardness: (JIS K 56008.4.1 (5) (b) for the test pencil hardness
*Glossiness test: 60 ° of mirror surface lusters (JIS H 40016.6, JIS K 54008.4)
*Adhesion test: by utilizing adhesive plaster to peel off (KS D 67116.3, JIS K 40016.3) after the 1mm spacing 100/100
*Bendability: crooked 7/16 Ψ utilizes adhesive plaster release coated film surface (JIS H 40016.4) afterwards for 180 °
*Shock-resistance: from the high place of 50cm to film coated surface landing 500g steel ball (KS D 67116.5, JIS H 4,001 6.5)
*Thermotolerance: utilize electric furnace to do 200 ℃/one hour test (JIS K 54008.13)
*Stain resistance: cleaned with flowing water afterwards in 80 ℃/24 hours with [carbon/water] coating
*Stain resistance: clean with flowing water after coating [carbon/Vaseline/BC] solution
*Alkali resistance: 24 hours (JIS K 56008.21) of deposition in 5% yellow soda ash
*Acid resistance: 24 hours (JIS K 56008.22) of deposition in 5% sulfuric acid
*CASS:Salt spray Nacl 5%, CuCl 20.26g/l 0.1ml acetate is 48 hours (JIS H 8681) of spraying continuously
*Resistance to salt water: 240 hours (JIS K 5,600 8.23) of deposition in 5% NaCI
*Pin hole:25 ℃ of RH60 ± 5%Pin hole solution drop/ one hour
*Weathering resistance: Sunshine Weather Meter 1000 hours (JIS K 56009.8)
*Flame resistivity; Coefficient (CA) the electric heating 1.5KW (KS F 2271) of propane flammable gas 350cc/min spontaneous combustion in 10 minutes
*Resistance to boiling water: in four hours (JIS 5,600 8.20) of deposition, boiling water (distilled water) lining
*Water tolerance: 720 hours (JIS K 5,600 8.19) of deposition in tap water
*Dissolubility resistent: in benzene, toluene, precipitate 240 hours with 12/15
As mentioned above, the pH value of physical properties and effective storage life, coating is irrelevant, and performance is good.That is, the basic solution or the buffered soln that add for the pH value of stablizing coating influence physical properties hardly, and have only influenced the effective storage life of coating and the time of drying of filming.
The present invention is not limited to the foregoing description, under the condition that does not exceed the claims of the present invention main idea, the any staff with general knowledge in field can carry out various distortion under the present invention, and these changes also will belong to the scope that this claim is put down in writing.
Utilizability on the industry
In sum, the invention provides a kind of functional coating, this functional coating provides ornamental, heat resistance attractive in appearance, weatherability, stain resistance, high rigidity, resistance to water, adhibit quality, corrosion resistance, durability, cold-resistant hot etc. by being coated in the surfaces such as metal, nonmetal, cement, slabstone, thereby the inside/outside decorative material for building that not only can form high-quality is filmed, but also any one ordinary people just can be broken a seal and use immediately without special equipment.
End reaction thing of the present invention is formed inorganic coating film by potteryization, formed inorganic coating film is not only more stable on physical properties, chemical property, and different with organic coating be, distribute harmful Environmental Hormone or volatile organic matter (VOCs) hardly, thereby possessed the environmental protection effect.And the present invention has obtained TVOC (mg/m in " authentication of Green environmental-protection building material " of Korea S air cleaning association on January 27th, 2005 2H): 0.007HCHO (mg/m 2H) effect, thus fitst water grade (authentication code: HB165F05-01) obtained.And with the far infrared irradiation rate: 0.916, radiant (W/m six): 7.89 * 10 2Ratio emit far infrared rays in a large number to the human body beneficial, and at the anti-mould test of the graduate coating of Korea S's raw yarn cloth testing (KS M 5000, test method 3431) is acknowledged as fitst water 10 grades in, and in flame resistance test, also be acknowledged as anti-combustion one-level etc., can confirm to have good physical properties and characteristic thus.
And the present invention has stablized the pH value of composition and has increased substantially hold capacity by adding buffered soln, and because of its drying at normal temperatures, so do not need existing in order to obtain that inorganic compositions is filmed and heat embrittlement (oven dry) process of carrying out.Thus, from human consumer's angle, also has the effect that to create high-level efficiency etc. with the low price cost.

Claims (9)

1. one kind is adopted pH value control method exsiccant inorganic coating composition at normal temperatures, it is characterized in that comprising:
With general formula R nSi (OR ') 4-nThe organoalkoxysilane of expression, weight percent is 1～40;
Water or organic solvent are as the colloid oxide compound of dispersion medium, and the weight percent that is scaled solid shape powder is 0.5～20;
Rudimentary aliphatic alcohol, weight percent are 0.1～70;
Organic/inorganic acid, weight percent are 0.1～3;
Inorganic fillings, weight percent are 0.01～20;
Mineral dye, weight percent are 0.01～40;
Being used alone or as a mixture pH value as the agent of pH value stabilization and being 7.5～10 basic solution, pH value is the buffered soln of 6.5～7.3 scopes, and weight percent is 0.1～5;
In the formula, R is that carbon number is 1～6 alkyl, and R ' is that carbon number is that 1～5 alkyl or carbon number are 1～4 acyl group.
2. employing pH value control method according to claim 1 is the exsiccant inorganic coating composition at normal temperatures, it is characterized in that:
Described buffered soln is the solution of being made up of conjugate acid and conjugate base thereof.
3. employing pH value control method according to claim 1 is the exsiccant inorganic coating composition at normal temperatures, it is characterized in that:
Described lower alcohol selects more than one to use from the group of being made up of methyl alcohol, ethanol, propyl alcohol, Virahol, n-butanols, isopropylcarbinol.
4. employing pH value control method according to claim 1 is the exsiccant inorganic coating composition at normal temperatures, it is characterized in that:
Described organic acid or mineral acid select more than one to use from the group of being made up of phosphoric acid, hydrochloric acid, sulfuric acid, nitric acid, acetate, formic acid.
5. employing pH value control method according to claim 1 is the exsiccant inorganic coating composition at normal temperatures, it is characterized in that:
Described inorganic fillings selects more than one to add from the micropowder of the whisker of potassium titanate, aluminium borate whisker, aluminum oxide, silicon nitride, silicon carbide, silicon-aluminium and glass fibre, carbon fibre and antibiotic micropowder of porous inorganic and inorganic inhibitor.
6. employing pH value control method according to claim 1 is the exsiccant inorganic coating composition at normal temperatures, it is characterized in that:
Described mineral dye selects more than one to add from the nontoxicity pearly pigment of the titanium oxide pigments of rutile structure and mica-titanium oxide base.
7. the described employing of the claim 1 pH value control method compound method of exsiccant inorganic coating composition at normal temperatures is characterized in that comprising step:
Reaction is hydrolyzed after interpolation colloid oxide compound and organic acid or the mineral acid in organoalkoxysilane;
In described reaction solution, put into after alcohol, stopping composition and the pigment to stir and make it mean particle size and reach below the 10 μ m with pulverizer;
Finish after the described stirring, clean with alcohol;
Finish after the alcohol wash, pour separately or use with pH value stabilization agent the stablizing coating pH value of basic solution, buffered soln into.
8. the described employing of the claim 1 pH value control method compound method of exsiccant inorganic coating composition at normal temperatures is characterized in that comprising step:
In organoalkoxysilane, add the reaction that is hydrolyzed after colloid oxide compound and organic acid or the mineral acid, in the reaction solution of described hydrolysis, add alcohol, and pour into independent or use the pH value stabilization agent of basic solution, buffered soln with and form resin portion;
In alcohol, put into after inorganic fillings, the pigment to stir and make it granularity and reach below the 10 μ m, generate pigment portion with alcohol wash then with pulverizer;
Mix described resin portion and pigment portion.
9. one kind is adopted pH value control method exsiccant inorganic coating composition at normal temperatures, by utilizing the described inorganic coating composition of claim 1, forms on the surface of inside/outside decorative material for building and films.
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