CN103571302A - Water-based fluorine-containing epoxy paint - Google Patents
Water-based fluorine-containing epoxy paint Download PDFInfo
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- CN103571302A CN103571302A CN201310463815.9A CN201310463815A CN103571302A CN 103571302 A CN103571302 A CN 103571302A CN 201310463815 A CN201310463815 A CN 201310463815A CN 103571302 A CN103571302 A CN 103571302A
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Abstract
The invention discloses water-based fluorine-containing epoxy paint. A preparation method of the water-based fluorine-containing epoxy paint comprises the following steps of (1) uniformly mixing absolute ethyl alcohol, amino siloxane and fluorine-containing siloxane under the condition of magnetic-force stirring, adjusting the pH value to 3-5, reacting for 45min to 65min at room temperature, thus obtaining the fluorine-containing and amino-containing siloxane sol, wherein the amino siloxane contains -NH2 or -NH-, and the fluorine-containing siloxane contains -CF2- or -CF3; (2) at room temperature, mixing the fluorine-containing and amino-containing siloxane sol with water-based epoxy resin emulsion, reacting for 0.5h to 1h under the condition of magnetic-force stirring, thus obtaining the modified water-based epoxy emulsion after the reaction; (3) at room temperature, adding polyamine curing agent into the modified epoxy emulsion and reacting for 10min to 20min under the condition of magnetic-force stirring, thus obtaining the water-based fluorine-containing epoxy paint. A coating prepared from the fluorine-containing epoxy paint has excellent hydrophobicity, chemical resistance, acid-alkali resistance and stain resistance and strong substrate combining force; the preparation method is simple, the cost is low, and the industrial production can be realized.
Description
Technical field
The present invention relates to technical field of coatings, particularly a kind of aqueous fluorine-containing epoxy coating.
Background technology
Fluorocarbon coating has extremely low surface energy and the highest theoretical water droplet contact angle, makes it in fields such as water proof anti-soil freezings, obtain paying close attention to widely.Yet the fluorocarbon coating FEVE of main flow films with the contact angle of water generally at 85～95 ° in the market, and shows according to research, contact angle is greater than the surface of 98 ° and just has anti-fouling effect, so in fact commercially available fluorocarbon coating does not have anti-fouling effect.In addition, existing fluorocarbon coating is expensive, and solvent for use also belongs to high malicious type.
Aqueous epoxy coating because its source is abundant, cheap, environmental friendliness, transparency is high, physical and mechanical properties is excellent, and (hardness is high, strong with substrate caking power) is widely used.But epoxy coating film coated surface can be high, water droplet contact angle low (30～50 °), does not possess waterproof freezing performance.In addition, epoxy coat is weather-proof, wear resistance is also poor.And these, fluorocarbon coating possesses just.If epoxy coating and fluorocarbon coating are combined, comprehensively the two advantage, will bring novel material and new application.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of novel aqueous fluorine-containing epoxy coating, this fluorine-containing epoxy coating fluorine-containing chain in solidification process easily moves to coating surface, makes coating have excellent hydrophobic performance, chemically-resistant, acid and alkali-resistance, anti-pollution characteristic and very strong substrate caking power; This fluorine-containing epoxy coating preparation method is simple simultaneously, and cost is low, and suitability for industrialized is produced.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
An epoxy coating, its preparation method comprises following concrete steps:
(1) dehydrated alcohol, aminosiloxane, flucride siloxane are mixed under magnetic agitation, regulate left and right, pH value to 3～5, at room temperature react obtain after 45～60min fluorine-containing and containing aminosiloxane colloidal sol; In described aminosiloxane, contain-NH
2or-NH-, in described flucride siloxane, contain-CF
2-or-CF
3; The volume ratio that feeds intake of described dehydrated alcohol, aminosiloxane, flucride siloxane is 20～40:0.5～1:0.2～0.4;
(2) at room temperature, by fluorine-containing and mix with aqueous epoxy resin emulsion containing aminosiloxane colloidal sol, under magnetic agitation, at room temperature react 0.5～1h, after reaction, obtain the aqueous epoxy emulsion of modification; Fluorine-containing and be 2～6:10～30 containing the volume ratio that feeds intake of aminosiloxane colloidal sol and aqueous epoxy resin emulsion;
(3) at room temperature, get polyamine curing agent and join in modified epoxy emulsion, under magnetic agitation, react 10～20min, obtain aqueous fluorine-containing epoxy coating; Described polyamine curing agent is 1.5～2.5:10 with the volume ratio that feeds intake of the aqueous epoxy resin emulsion that the described modified epoxy emulsion of preparation is used.
In described step (1), aminosiloxane is contain-NH of end group
2or the siloxanes of contain in segment-NH-, can be selected from following a kind of or several combination arbitrarily: γ-aminopropyl triethoxysilane, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, γ-aminopropyltrimethoxysilane, N-β-(aminoethyl)-γ aminopropyl trimethoxysilane, γ-aminopropyl methyldiethoxysilane etc.
In described step (1), flucride siloxane is contain-CF of the end of the chain
3or contain in segment-CF
2-silicon fluoride, can be selected from following a kind of or several combination arbitrarily: 17 fluorine decyl triethoxyl silanes, ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyl group Trimethoxy silanes, 4-methyl-(perfluor is base ethyl) propyl trimethoxy silicane, ten difluoro heptyl propyl group methyl dimethoxysilanes etc.
In described step (1), use pH to 3～5 of the mixed system of hydrochloric acid adjusting dehydrated alcohol, aminosiloxane, flucride siloxane, the preferred 30-50% of concentration of hydrochloric acid.
In described step (2), epoxy resin latex is bi-component aqueous epoxy Resin A component, in its molecular chain, with epoxide group, is preferably bisphenol A type epoxy resin.The solid content of described epoxy resin latex is preferably 49-51%.
In described step (3), solidifying agent is polyamine curing agent, can self-vulcanizing, can be selected from following a kind of or several combination arbitrarily: quadrol, diethylenetriamine, triethylene tetramine, two propylene triamines, diethyl amino propylamine, trimethylammonium is diamines, T31 solidifying agent, AB-HGF, 810 epoxy curing agents, G328 epoxy hardener, T2-500 pnenolic aldehyde amine hardener, cashew nut oil modified amine hardener, 703 solidifying agent etc.
The prepared aqueous fluorine-containing epoxy emulsion coating method of the present invention can be selected a kind of in spraying, showering, spin coating, dip-coating, roller coating and brushing, is preferably spraying method.Solidification value can be carried out between 10～180 ℃, and temperature is higher, and required time is shorter.Preferred consolidation temperature is between 50～120 ℃.
The present invention compared with prior art has following outstanding advantage and beneficial effect:
(1) first the present invention prepares a kind ofly containing amino fluorine silicon alcosol, and generation fluorine-containing epoxy resin then reacts this colloidal sol and epoxy resin.This fluorine-containing silanol is incorporated in epoxy systems, not only as solidifying agent, forms Si-O-Si network, has increased mechanics, the thermal property of coating, and due to fluorine-containing chain hydrophobic, make it in coating drying process, more easily move to coatingsurface, coatingsurface fluorine content is greater than inner fluorine content greatly.Thereby, add on a small quantity fluorochemicals and can make prepared coating there is excellent hydrophobicity, chemically-resistant, acid and alkali-resistance, anti-pollution characteristic and very strong substrate caking power.
(2) low, the production of aqueous fluorine-containing epoxy coating production technique of the present invention simple (can make on the basis of existing commercialization aqueous epoxy coating), cost and the equal environmental friendliness of coating process, suitability for industrialized is produced.
Accompanying drawing explanation
Fig. 1 be when aminosiloxane be γ-aminopropyl triethoxysilane, flucride siloxane fluorine-containing epoxy coating preparation and the application schematic diagram while being 17 fluorine decyl triethoxyl silane.
Fig. 2 is the water contact angle after epoxy coating (a), fluorine silicon colloidal sol (b) and fluorine-containing epoxy coating (c) solidify in different base.
Embodiment
Technical scheme in the embodiment of the present invention is carried out to clear, complete description below, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
(1) 17 fluorine decyl triethoxyl silanes (FAS) of the γ-aminopropyl triethoxysilane (KH-550) of the dehydrated alcohol of 20 parts by volume, 0.5 parts by volume, 0.2 parts by volume are mixed under magnetic agitation, hydrochloric acid with 50% slowly regulates pH value to 4 left and right, obtains flucride siloxane colloidal sol after at room temperature reacting 45min.
(2) at normal temperatures, by the above-mentioned colloidal sol of 4 parts by volume and 10 parts by volume aqueous epoxy resin emulsions (the Zhejiang novel material company limited that stablizes the country, AB-EP-51, solid content 49-51%) mix, under magnetic agitation, react at normal temperatures 0.5h, after reaction, containing amine silanol, be grafted on epoxy, obtain the aqueous epoxy emulsion of modification.
(3) at normal temperatures, get 1.5 parts of modified amine curing agents (Zhejiang novel material company limited that stablizes the country, AB-HGF, solid content 39-41%) join in above-mentioned modified epoxy emulsion, under magnetic agitation, react 10min, obtain aqueous fluorine-containing epoxypaint, wherein, the volume * 100%=0.24v% of the volume/prepared aqueous fluorine-containing epoxypaint of 17 fluorine decyl triethoxyl silanes of the consumption of FAS-17 (v%)=add.
By the aqueous fluorine-containing epoxypaint making after glass surface dip-coating, curing reaction 1 h at 120 ℃, coating performance is as shown in table 1.
Table 1 coating property indices
| Production code member | Epoxypaint | Fluorine-containing organic silicon colloidal sol | Fluorine-containing epoxy resin coating |
| Outward appearance | Emulsion | Clear solution | Emulsion |
| Paint film appearance | Transparent | Transparent | Substantially transparent |
| Sticking power (level) | 0-1 | 0-1 | 0-1 |
| Hardness (H) | 5 | 5 | 5 |
| Contact angle (°) | 33.6 | 120 | 115 |
| Water tolerance (7 days) | Without bubbling, peel off | Without bubbling, peel off | Without bubbling, peel off |
| Acid resistance (50g/L sulfuric acid, 7 days) | Without bubbling, peel off | Without bubbling, peel off | Without bubbling, peel off |
| Alkali resistance (50g/LNaOH, 7 days) | Without bubbling, peel off | Without bubbling, peel off | Without bubbling, peel off |
| Solidification value (℃) | Room temperature | 50-120 | 120 |
| Set time (min) | 20 | 5-15 | 60 |
From above table, can find, the epoxy resin contact angle after modification has risen to 115 ° from 33.6 °, and now silicon fluoride add-on is only 0.24v%, with low cost.
The fluorine-contained surface amount of having analyzed coating with X-ray fluorescence spectra, its result is as shown in table 2.
Embodiment 2
The consumption (v%) that changes 17 fluorine decyl triethoxyl silanes (FAS), is 0.12v%, and other conditions, with embodiment 1, make aqueous fluorine-containing epoxypaint.
By the aqueous fluorine-containing epoxypaint making, after glass surface dip-coating, at 120 ℃, curing reaction 1h, obtains top coat, has analyzed the fluorine-contained surface amount of coating with X-ray fluorescence spectra, and its result is as shown in table 2.
The consumption (v%) that changes 17 fluorine decyl triethoxyl silanes (FAS), is 0.36v%, and other conditions, with embodiment 1, make aqueous fluorine-containing epoxypaint.
By the aqueous fluorine-containing epoxypaint making, after glass surface dip-coating, at 120 ℃, curing reaction 1h, obtains top coat, has analyzed the fluorine-contained surface amount of coating with X-ray fluorescence spectra, and its result is as shown in table 2.
Table 2 coatingsurface fluorine content and contact angle
A: the preparation method of the epoxy coat of processing with FAS is: first process glass surface with the aqueous epoxy resin emulsion in embodiment 1 and obtain epoxy coat, then epoxy coat is immersed in to hexane solution (FAS volume fraction is 0.5%) the processing 1h of 17 fluorine decyl triethoxyl silanes (FAS), at 120 ℃, dry 1h again, obtain the epoxy coat of processing with FAS.
B: film on slide glass with the FAS-KH550 colloidal sol of embodiment 1 preparation, dry 1h at 120 ℃, obtain the coating of processing with colloidal sol.
From table 2, with silicon fluoride (FAS), directly process epoxy coat fluorine-contained surface amount the highest, but this method is not suitable for suitability for industrialized production.Directly fluorine-containing material is added in epoxypaint to effect also clearly, while only adding volume 0.36%, coatingsurface fluorine content is close with the coating of directly processing with FAS, and contact angle reaches 116 °, can be used as water proof anti-soil protection against corrosion freezing surperficial.
Embodiment 2
(1) ten trifluoro octyltri-ethoxysilane of the γ-aminopropyl triethoxysilane of the dehydrated alcohol of 20 parts by volume, 0.5 parts by volume, 0.3 parts by volume are mixed under magnetic agitation, hydrochloric acid with 50% slowly regulates pH to 4 left and right, obtains flucride siloxane colloidal sol after at room temperature reacting 45min.
(2) at normal temperatures, by the above-mentioned colloidal sol of 4 parts by volume and 10 parts by volume aqueous epoxy resin emulsions (the Zhejiang novel material company limited that stablizes the country, AB-EP-51, solid content 49-51%) mix, under magnetic agitation, react at normal temperatures 0.5h, after reaction, containing amine silanol, be grafted on epoxy, obtain the aqueous epoxy emulsion of modification.
(3) at normal temperatures, get 1.5 parts of modified amine curing agents (Zhejiang stablize the country novel material company limited, AB-HGF, solid content 39-41%) and join in above-mentioned modified epoxy emulsion, under magnetic agitation, react 10min, obtain aqueous fluorine-containing epoxypaint.
After applying and be dried with embodiment 1, top coat character is similar to example 1.
(1) dehydrated alcohol of 20 parts by volume, 0.7 parts by volume γ-aminopropyl methyldiethoxysilane, 0.3 parts by volume 17 fluorine decyl triethoxyl silanes are mixed under magnetic agitation, hydrochloric acid with 50% slowly regulates pH to 4 left and right, obtains flucride siloxane colloidal sol after at room temperature reacting 50min.
(2) at normal temperatures, by 3 parts by volume prepolymers and 10 parts by volume aqueous epoxy resin emulsions (the Zhejiang novel material company limited that stablizes the country, AB-EP-51, solid content 49-51%) mix, under magnetic agitation, react at normal temperatures 0.5h, after reaction, containing amine silanol, be grafted on epoxy, obtain the aqueous epoxy emulsion of modification.
(3) at normal temperatures, get 2 parts of modified amine curing agents (Zhejiang stablize the country novel material company limited, AB-HGF, solid content 39-41%) and join in above-mentioned modified epoxy emulsion, under magnetic agitation, react 10min, obtain aqueous fluorine-containing epoxypaint.
After applying and be dried with embodiment 1, top coat character is similar to example 1.
Embodiment 4
(1) 17 fluorine decyl triethoxyl silanes of γ-aminopropyl methyl dimethoxysilane of the dehydrated alcohol of 20 parts by volume, 0.7 parts by volume, 0.2 parts by volume are mixed under magnetic agitation, hydrochloric acid with 50% slowly regulates pH to 4 left and right, obtains flucride siloxane colloidal sol after at room temperature reacting 45min.
(2) at normal temperatures, by 3 parts by volume prepolymers and 10 parts by volume aqueous epoxy resin emulsions (the Zhejiang novel material company limited that stablizes the country, AB-EP-51, solid content 49-51%) mix, under magnetic agitation, react at normal temperatures 0.5h, after reaction, containing amine silanol, be grafted on epoxy, obtain the aqueous epoxy emulsion of modification.
(3) at normal temperatures, get 2 parts of modified amine curing agents (Zhejiang stablize the country novel material company limited, AB-HGF, solid content 39-41%) and join in above-mentioned modified epoxy emulsion, under magnetic agitation, react 10min, obtain aqueous fluorine-containing epoxypaint.
After applying and be dried with embodiment 1, top coat character is similar to example 1.
Embodiment 5
(1) dehydrated alcohol of 20 parts by volume, 0.6 parts by volume γ-aminopropyl methyl dimethoxysilane, 0.3 parts by volume ten trifluoro octyltri-ethoxysilane are mixed under magnetic agitation, hydrochloric acid with 50% slowly regulates pH to 4 left and right, obtains flucride siloxane colloidal sol after at room temperature reacting 45min.
(2) at normal temperatures, by 4 parts by volume prepolymers and 10 parts by volume aqueous epoxy resin emulsions (the Zhejiang novel material company limited that stablizes the country, AB-EP-51, solid content 49-51%) mix, under magnetic agitation, react at normal temperatures 0.5h, after reaction, containing amine silanol, be grafted on epoxy, obtain the aqueous epoxy emulsion of modification.
(3) at normal temperatures, get 1.5 parts of modified amine curing agents (Zhejiang stablize the country novel material company limited, AB-HGF, solid content 39-41%) and join in fluorine-containing epoxy emulsion, under magnetic agitation, react 10min, obtain aqueous fluorine-containing epoxypaint.
After applying and be dried with embodiment 1, top coat character is similar to example 1.
Embodiment 6
Get the prepared fluorine-containing epoxy coating of above-described embodiment 1, dip-coating, on slide glass, is inquired into the impact of its curing mode on coating performance.Discovery is dried 1h at 120 ℃, its surface contact angle reaches 115 °, and along with temperature raises, its required time shortens, at 180 ℃, dry 30min and can reach surface elevation hydrophobization (contact angle～115 °), at 50 ℃, extend to 2h its set time.Moreover, this coating at room temperature also can complete curing, under 20 ℃ of room temperatures, places after 7 days, and its contact angle also rises greatly, has become highly hydrophobic (contact angle～115 °).It is curing to be that this coating can complete in a very wide scope.
Embodiment 7
Get the prepared fluorine-containing epoxy coating of above-described embodiment 1, adopt respectively mode film forming in substrate of glass such as spraying, showering, spin coating, dip-coating, roller coating and brushing, after finding film forming, film is smooth, light, and water droplet contact angle all reaches 115 °.Film on a large scale and adopt spraying to be advisable, be easy to industrialization operation.
Embodiment 8
Get the prepared fluorine-containing epoxy coating of above-described embodiment 1, by its dip-coating (marble in various substrates, plasterboard, paper, metal, cloth etc.), observe their water droplet contact angle, find that the basic and various types of substrates of this coating has good sticking power (0 grade), and contact angle generally become highly hydrophobicly from hydrophilic, what have has even approached super-hydrophobic (as shown in Fig. 2, table 3).Prove that this coating can be used as water proof anti-soil anticorrosive coating.
Concrete contact angle data are as shown in table 3:
Contact angle after the surface treatment of table 3 different base/°
Claims (5)
1. an aqueous fluorine-containing epoxy coating, its preparation method comprises following concrete steps:
(1) dehydrated alcohol, aminosiloxane, flucride siloxane are mixed under magnetic agitation, regulate left and right, pH value to 3～5, at room temperature react obtain after 45～60min fluorine-containing and containing aminosiloxane colloidal sol; In described aminosiloxane, contain-NH
2or-NH-, in described flucride siloxane, contain-CF
2-or-CF
3; The volume ratio that feeds intake of described dehydrated alcohol, aminosiloxane, flucride siloxane is 20～40:0.5～1:0.2～0.4;
(2) at room temperature, by fluorine-containing and mix with aqueous epoxy resin emulsion containing aminosiloxane colloidal sol, under magnetic agitation, at room temperature react 0.5～1h, after reaction, obtain the aqueous epoxy emulsion of modification; Fluorine-containing and be 2～6:10～30 containing the volume ratio that feeds intake of aminosiloxane colloidal sol and aqueous epoxy resin emulsion;
(3) at room temperature, get polyamine curing agent and join in modified epoxy emulsion, under magnetic agitation, react 10～20min, obtain aqueous fluorine-containing epoxy coating; Described polyamine curing agent is 1.5～2.5:10 with the volume ratio that feeds intake of the aqueous epoxy resin emulsion that the described modified epoxy emulsion of preparation is used.
2. aqueous fluorine-containing epoxy coating as claimed in claim 1, is characterized in that: described aminosiloxane is selected from following a kind of or several combination arbitrarily: γ-aminopropyl triethoxysilane, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, γ-aminopropyltrimethoxysilane, N-β-(aminoethyl)-γ aminopropyl trimethoxysilane, γ-aminopropyl methyldiethoxysilane; Described flucride siloxane is selected from following a kind of or several combination arbitrarily: 17 fluorine decyl triethoxyl silanes, ten trifluoro octyltri-ethoxysilane, 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyl group Trimethoxy silanes, 4-methyl-(perfluor is base ethyl) propyl trimethoxy silicane, ten difluoro heptyl propyl group methyl dimethoxysilanes.
3. aqueous fluorine-containing epoxy coating as claimed in claim 1, is characterized in that: in step (2), the solid content of described epoxy resin latex is 49-51%.
4. the aqueous fluorine-containing epoxy coating as described in one of claim 1～3, is characterized in that: in step (2), described aqueous epoxy resins is bisphenol A type epoxy resin.
5. the aqueous fluorine-containing epoxy coating as described in claim 1～3, is characterized in that: the polyamine curing agent described in step (2) is selected from following a kind of or several combination arbitrarily: quadrol, diethylenetriamine, triethylene tetramine, two propylene triamines, diethyl amino propylamine, trimethylammonium is diamines, T31 solidifying agent, AB-HGF, 810 epoxy curing agents, G328 epoxy hardener, T2-500 pnenolic aldehyde amine hardener, cashew nut oil modified amine hardener, 703 solidifying agent.
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Application publication date: 20140212 |