CN105295583A - Preparation method for hydrophobic heat-reflective fluorocarbon coating - Google Patents
Preparation method for hydrophobic heat-reflective fluorocarbon coating Download PDFInfo
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Abstract
The invention discloses a preparation method for a hydrophobic heat-reflective fluorocarbon coating. According to the invention, a silane coupling agent KH550 and a silane coupling agent HMDS are respectively used for surface modification of nanometer TiO2 and nanometer SiO2 in another reaction system in advance, so an excess amount of an organic silicone resin component is effectively prevented from introducing into a final reaction system of the fluorocarbon coating; the prepared fluorocarbon coating has better adhesion performance on a substrate, corrosion resistance and mechanical strength compared with the prior art; and the problem of poor compatibility between organic silicone resin and other organic solvents is effectively overcome, so process control difficulty is reduced and the speed of chemical reaction is accelerated. The preparation method is simple; and the prepared fluorocarbon coating has sunshine reflectivity as high as more than 90% and a contact angle of more than 150 DEG, and the fluorocarbon coating has the advantages of excellent self-cleaning performance, good adhesion performance on the substrate, good corrosion resistance and long service life.
Description
Technical field
The present invention relates to a kind of method of modifying of fluorocarbon coating, particularly relate to a kind of preparation method of hydrophobic heat reflection fluorocarbon coating.
Background technology
Fluorocarbon coating has the features such as contamination resistance, weathering resistance be strong because of it, has the title of " coating king " in industry, is used widely.But fluorocarbon coating does not possess function of heat reflection, self-cleaning performance is poor, easily gathers greasy dirt and dust, needs manual cleaning.
In prior art, in order to give fluorocarbon coating heat reflection and/or self-cleaning performance, generally adopting in fluorocarbon coating, adding the method for titanium dioxide, silicon-dioxide and other functional inorganic filling, carrying out modified paint.
As: Chinese patent application CN103013243A discloses high self-cleaning solar heat reflection paint of a kind of nano modification and preparation method thereof, its feed composition (by mass percentage): fluorocarbon resin emulsion 40-50%, wetting dispersing agent (wilkinite) 0.5-1%, titanium dioxide 15-25%, nano silicon 0.2-1%, filler (barium sulfate) 0-25%, deionized water 3-10%, antimildew disinfectant 0.5-1%, film coalescence aid (alcohol ester 12) 0.5-2%, pH adjusting agent 0.1-0.5%, defoamer (modified polyorganosiloxane defoamer) 0.3-0.9%, flow agent (organic silicon surfactant) 0.2-0.5%, silicone resin 1-4.5% and auxiliary agent (thickening material) 0.1-0.5%.
Its preparation method: first add deionized water in stirred pot, then add wetting dispersing agent to stir, nano silicon, titanium dioxide, filler is added successively under the rotating speed of 400-600r/min, stir after 15 minutes, add defoamer, auxiliary agent, antimildew disinfectant again, high speed dispersion 20-30 minute under the rotating speed of 800-1200r/min, being then ground to fineness with sand mill is less than 10 microns, mill base; (in mill base) adds fluorocarbon resin emulsion, film coalescence aid, flow agent, silicone resin and pH adjusting agent again, stirs, and filters and get final product.
There is following problem or deficiency in the preparation method of this technical scheme: one is, complicated process of preparation.Reason is mainly, its in order to solve nano silicon aqueous phase system in the technical problem of bad dispersibility, the technical way adopted is, wetting dispersing agent (wilkinite) is introduced in system, as carrier, absorption nano silicon, and then in aqueous phase system, obtain required dispersion effect.This directly causes the grinding that must need to carry out slip in its subsequent step; Two are, in its reaction system, directly introduce the silicone resin of more amount.And those skilled in the art is known: silicone resin exist more weak, the resistance to various organic solvent-borne of physical strength poor, to shortcomings such as the bad adhesion of the base material such as metal and plastics and the poor compatibility of other organic solvents, this will the sticking power of obtained coating and the base material such as metal and plastics be caused not good enough etc. shortcoming or deficiency.
Summary of the invention
The object of the invention is, there is provided a kind of preparation method of hydrophobic heat reflection fluorocarbon coating, simple, the prepared fluorocarbon coating of its preparation technology has the technical characterstics such as sunlight reflectivity is high, self-cleaning performance is excellent, base material adhesive ability strong, corrosion resistance and good, long service life.
The technical scheme that the present invention is adopted for achieving the above object is, a kind of preparation method of hydrophobic heat reflection fluorocarbon coating, is characterized in that, comprise the following steps:
The first step, by mass fraction, gets nano-TiO respectively
24.0-12.0 part, Nano-meter SiO_2
22.0-6.0 part, fluorocarbon resin 55.0-63.1 part, butylacetate 24.2-27.8 part, hexamethylene diisocyanate 2.7-3.2 part, defoamer 0.1-1 part, wetting agent 0.1-1 part and dispersion agent 0.1-1 part are for subsequent use;
Second step, in above-mentioned fluorocarbon resin, first adds wetting agent and dispersion agent;
Then, slowly nano-TiO is added
2, use mechanical stirring device high-speed stirring, after 30min, then high-speed stirring limit, limit slowly adds Nano-meter SiO_2 simultaneously
2, defoamer and butylacetate;
Continue high-speed stirring 30min again;
Then, add hexamethylene diisocyanate, be placed in ultrasonic disperse instrument, ultrasonic disperse 15min, to obtain final product;
Above-mentioned nano-TiO
2be through KH550 silane coupler modified after to obtain;
Above-mentioned Nano-meter SiO_2
2obtain after being through HMDS silane coupling agent surface modification.
The technique effect that technique scheme is directly brought is, simple, the prepared fluorocarbon coating of preparation technology has sunlight reflectivity high (can reach more than 90%), self-cleaning performance is excellent, base material adhesive ability is strong, corrosion resistance and good, long service life.
Adopt fluorocarbon coating prepared by technique scheme on metal or plastic basis material after coating film forming, after testing, coating is in the wavelength region (200-2600nm) measured, luminous reflectance factor is more than 90%, and surface tension is very low, contact angle reaches more than 150 °, and greasy dirt etc. are difficult to, in its surface attachment, easily clean.
For understanding above-mentioned technical characterstic better, brief description is as follows:
In technique scheme, carry out nano-TiO by silicone resin (KH550 silane coupling agent and HMDS silane coupling agent) will be used
2and Nano-meter SiO_2
2surface modification, carries out in advance in another reaction system, thus effectively prevent in the final reaction system of fluorocarbon coating, introduces the silicone resin composition of excessive number; Prepared fluorocarbon coating is obtained relative to prior art better and the adhesion property of base material, corrosion resistance nature and physical strength.Further, in the preparation system of generation fluorocarbon coating subsequently, also efficiently avoid the problem of the poor compatibility of silicone resin and other organic solvents, this is conducive to the speed accelerating subsequent chemical reaction.
Further, (compared with prior art) does not need the carrier introducing polynite and so in reaction system, correspondingly, eliminates follow-up grinding steps, reduces complicacy and the operation easier of preparation technology.
Supplementary notes:
1, nano-TiO
2and Nano-meter SiO_2
2before surface modification, there is great amount of hydroxy group (-OH) in its surface, and general performance is polar hydrophilic oleophobic property, not easily disperses in non-polar organic solvent; Utilize silane coupling agent to nano-TiO
2and Nano-meter SiO_2
2after carrying out Surface coating respectively, hydroxyl (-OH) is reduced in a large number, surface is due to organic group in grafting, and entirety changes nonpolar lipophilic-hydrophobic property into, improves the dispersing property in fluorocarbon resin in subsequent reactions system; Its micro-shape is similar to the nanofeature pattern of lotus leaf surface, makes oil droplet and water droplet all not easily at its superficial residence, thus reaches very low, the easy cleaned effect of surface tension.
2, in technique scheme, hexamethylene diisocyanate (HB175) selected by solidifying agent, it has film forming good mechanical property, good, the resistance to rayed of chemical resistant properties, not yellowing, weathering resistance are good, and be far superior to the solidifying agent that aromatic isocyanate makes, be suitable for outdoor environment and use.
Be preferably, above-mentioned nano-TiO
2method of modifying, comprise the following steps:
Step one, is dissolved in propyl carbinol by KH550 silane coupling agent, uses magnetic agitation 10min, to mixing;
Step 2, pours in there-necked flask by the silane coupling agent-butanol solution after mixing, and uses mechanical stirrer to stir, and add Nano-meter SiO_2 under whipped state
2;
Then, there-necked flask is connect reflux, and under whipped state, be slowly warming up to 120 DEG C, after back flow reaction 2h, stop heating, carry out Temperature fall cooling;
Step 3, when cooling down to 60 DEG C, stops mechanical stirring, and there-necked flask is placed in ultrasonic disperse instrument ultrasonic disperse 30min;
Step 4, then there-necked flask is connect Vacuum filtration device and carry out vacuum decompression suction filtration, get filter residue and put into baking oven, at 120 DEG C, dry 8h, pulverizes after taking-up, to obtain final product.
The technique effect that this optimal technical scheme is directly brought is, at use KH550 silane coupling agent to nano-TiO
2in Process of Surface Modification, by adopting reflow method, accelerate speed of response, and by the employing of the series technique means such as ultrasonic disperse, effectively reduce nano-TiO
2the generation of the agglomeration in modifying process, reduces nano-TiO
2the control difficulty of particle diameter.
Further preferably, above-mentioned Nano-meter SiO_2
2method of modifying, comprise the following steps:
Step 1, is dissolved in propyl carbinol by HMDS silane coupling agent, uses magnetic agitation 10min, to mixing;
Step 2, pours in there-necked flask by the HMDS silane coupling agent-butanol solution after Homogeneous phase mixing, uses mechanical stirrer to stir, and add Nano-meter SiO_2 under whipped state
2;
Then, there-necked flask is connect reflux, and under whipped state, be slowly warming up to 120 DEG C, after back flow reaction 2h, stop heating, carry out Temperature fall cooling;
Step 3, when cooling down to 60 DEG C, stops mechanical stirring, there-necked flask is placed in ultrasonic disperse instrument ultrasonic disperse 30min.
Step 4, then there-necked flask is connect Vacuum filtration device and carry out vacuum decompression suction filtration, gets filter residue and puts into baking oven, dry 8h at 120 DEG C, after pulverize, to obtain final product.
The technique effect that this optimal technical scheme is directly brought is, at use HMDS silane coupling agent to Nano-meter SiO_2
2carrying out in Process of Surface Modification, by adopting reflow method, accelerating speed of response, and by the employing of the series technique means such as ultrasonic disperse, effectively reduce Nano-meter SiO_2
2in modifying process, the generation of agglomeration, reduces Nano-meter SiO_2
2the control difficulty of particle diameter.
Further preferably, above-mentioned nano-TiO
2and Nano-meter SiO_2
2average particle size particle size be 20-100nm.
The technique effect that this optimal technical scheme is directly brought is, nano-TiO
2and Nano-meter SiO_2
2average particle size particle size be 20-100nm, after paint film forming, its surface highly polished, planeness good.
Further preferably, above-mentioned defoamer is silicone antifoam agent;
Described wetting agent is BYK163;
Described dispersion agent is fatty acid dispersion agent.
The technique effect that this optimal technical scheme is directly brought is that raw material is commercially available prod, and its source is wide, and cost is low.
In sum, the present invention, relative to prior art, has simple, the prepared fluorocarbon coating of preparation technology and has the beneficial effects such as sunlight reflectivity is high, self-cleaning performance is excellent, base material adhesive ability strong, corrosion resistance and good, long service life.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Illustrate:
One, in following embodiment, the nano-TiO used
2be through KH550 silane coupler modified after to obtain;
The Nano-meter SiO_2 used
2obtain after being through HMDS silane coupling agent surface modification.
Wherein:
1, nano-TiO
2method of modifying, comprise the following steps:
Step one, is dissolved in propyl carbinol by KH550 silane coupling agent, uses magnetic agitation 10min, to mixing;
Step 2, pours in there-necked flask by the silane coupling agent-butanol solution after mixing, and uses mechanical stirrer to stir, and add Nano-meter SiO_2 under whipped state
2;
Then, there-necked flask is connect reflux, and under whipped state, be slowly warming up to 120 DEG C, after back flow reaction 2h, stop heating, carry out Temperature fall cooling;
Step 3, when cooling down to 60 DEG C, stops mechanical stirring, and there-necked flask is placed in ultrasonic disperse instrument ultrasonic disperse 30min;
Step 4, then there-necked flask is connect Vacuum filtration device and carry out vacuum decompression suction filtration, get filter residue and put into baking oven, at 120 DEG C, dry 8h, pulverizes after taking-up, to obtain final product.
2, Nano-meter SiO_2
2method of modifying, comprise the following steps:
Step 1, is dissolved in propyl carbinol by HMDS silane coupling agent, uses magnetic agitation 10min, to mixing;
Step 2, pours in there-necked flask by the HMDS silane coupling agent-butanol solution after Homogeneous phase mixing, uses mechanical stirrer to stir, and add Nano-meter SiO_2 under whipped state
2;
Then, there-necked flask is connect reflux, and under whipped state, be slowly warming up to 120 DEG C, after back flow reaction 2h, stop heating, carry out Temperature fall cooling;
Step 3, when cooling down to 60 DEG C, stops mechanical stirring, there-necked flask is placed in ultrasonic disperse instrument ultrasonic disperse 30min.
Step 4, then there-necked flask is connect Vacuum filtration device and carry out vacuum decompression suction filtration, gets filter residue and puts into baking oven, dry 8h at 120 DEG C, after pulverize, to obtain final product.
Two, defoamer is silicone antifoam agent, and wetting agent is BYK163, and dispersion agent is fatty acid dispersion agent; And defoamer, wetting agent and dispersion agent are commercially available prod.
Embodiment 1
The preparation method of fluorocarbon coating is as follows:
The first step, by mass fraction, gets nano-TiO respectively
24.0 parts, Nano-meter SiO_2
22.0 parts, fluorocarbon resin 55 parts, butylacetate 24.2 parts, hexamethylene diisocyanate 2.7 parts, defoamer 0.1 part, wetting agent 0.1 part and dispersion agent 0.1 part, for subsequent use;
Second step, in above-mentioned fluorocarbon resin, first adds wetting agent and dispersion agent;
Then, slowly nano-TiO is added
2, use mechanical stirring device high-speed stirring, after 30min, then high-speed stirring limit, limit slowly adds Nano-meter SiO_2 simultaneously
2, defoamer and butylacetate;
Continue high-speed stirring 30min again;
Then, add hexamethylene diisocyanate, be placed in ultrasonic disperse instrument, ultrasonic disperse 15min, to obtain final product.
Embodiment 2
The preparation method of fluorocarbon coating is as follows:
The first step, by mass fraction, gets nano-TiO respectively
28 parts, Nano-meter SiO_2
24 parts, fluorocarbon resin 58 parts, butylacetate 26 parts, hexamethylene diisocyanate 3 parts, defoamer 0.5 part, wetting agent 0.5 part and dispersion agent 0.5 part, for subsequent use;
All the other, all with embodiment 1.
Embodiment 3
The first step, by mass fraction, gets nano-TiO respectively
28 parts, Nano-meter SiO_2
25 parts, fluorocarbon resin 60 parts, butylacetate 25.8 parts, hexamethylene diisocyanate 3 parts, defoamer 1 part, wetting agent 1 part and dispersion agent 1 part, for subsequent use;
All the other, all with embodiment 1.
Embodiment 4
The first step, by mass fraction, gets nano-TiO respectively
210.0 parts, Nano-meter SiO_2
25.5 parts, fluorocarbon resin 63.1 parts, butylacetate 27.8 parts, hexamethylene diisocyanate 3.2 parts, defoamer 1 part, wetting agent 1 part and dispersion agent 1 part, for subsequent use;
All the other, all with embodiment 1.
Embodiment 5
The first step, by mass fraction, gets nano-TiO respectively
212.0 parts, Nano-meter SiO_2
26.0 parts, fluorocarbon resin 63.1 parts, butylacetate 27.8 parts, hexamethylene diisocyanate 3 parts, defoamer 0.8 part, wetting agent 0.8 part and dispersion agent 0.8 part, for subsequent use;
All the other, all with embodiment 1.
The detection of product performance and inspection:
The fluorocarbon coating obtained separately by embodiment 1-5, carries out stainless steel 304, acrylic plastering surface coated respectively, obtain coating:
1, surface highly polished, planeness good, to the strong adhesion (sticking power is one-level, GB/T1720-79) of base material.
2, adopt profile image analysis method to carry out contact angle detection respectively, the contact angle obtained is respectively: 151 °, 155 °, 153 °, 152 °, 152 °.
3, use Albedometer to carry out luminous reflectance factor test respectively, the wavelength region of light source used is 200-2600nm, and acquired results is respectively: 90%, 90.5%, 91%, 91,90.8%.
4, use percentage concentration be 10% dilute hydrochloric acid, percentage concentration be 10% dilute sodium hydroxide aqueous solution and toluene and sherwood oil (1:1) respectively erosion resistance test is carried out to coating; Testing standard is respectively: GB/T1763, GB/T9274-88, GB/T1734-93; Erosion resistance test result shows: in the test duration of 90 days, and coating all keeps complete, non-foaming, does not come off.
Salt-fog test test (testing standard is respectively: GB/T1771), test result shows: coating all can stand the salt-fog test test being greater than 600 hours, and coating keeps complete.
Claims (5)
1. a preparation method for hydrophobic heat reflection fluorocarbon coating, is characterized in that, comprise the following steps:
The first step, by mass fraction, gets nano-TiO respectively
24.0-12.0 part, Nano-meter SiO_2
22.0-6.0 part, fluorocarbon resin 55.0-63.1 part, butylacetate 24.2-27.8 part, hexamethylene diisocyanate 2.7-3.2 part, defoamer 0.1-1 part, wetting agent 0.1-1 part and dispersion agent 0.1-1 part are for subsequent use;
Second step, in above-mentioned fluorocarbon resin, first adds wetting agent and dispersion agent;
Then, slowly nano-TiO is added
2, use mechanical stirring device high-speed stirring, after 30min, then high-speed stirring limit, limit slowly adds Nano-meter SiO_2 simultaneously
2, defoamer and butylacetate;
Continue high-speed stirring 30min again;
Then, add hexamethylene diisocyanate, be placed in ultrasonic disperse instrument, ultrasonic disperse 15min, to obtain final product;
Above-mentioned nano-TiO
2be through KH550 silane coupler modified after to obtain;
Above-mentioned Nano-meter SiO_2
2obtain after being through HMDS silane coupling agent surface modification.
2. the preparation method of hydrophobic heat reflection fluorocarbon coating according to claim 1, is characterized in that, described nano-TiO
2method of modifying, comprise the following steps:
Step one, is dissolved in propyl carbinol by KH550 silane coupling agent, uses magnetic agitation 10min, to mixing;
Step 2, pours in there-necked flask by the silane coupling agent-butanol solution after mixing, and uses mechanical stirrer to stir, and add Nano-meter SiO_2 under whipped state
2;
Then, there-necked flask is connect reflux, and under whipped state, be slowly warming up to 120 DEG C, after back flow reaction 2h, stop heating, carry out Temperature fall cooling;
Step 3, when cooling down to 60 DEG C, stops mechanical stirring, and there-necked flask is placed in ultrasonic disperse instrument ultrasonic disperse 30min;
Step 4, then there-necked flask is connect Vacuum filtration device and carry out vacuum decompression suction filtration, get filter residue and put into baking oven, at 120 DEG C, dry 8h, pulverizes after taking-up, to obtain final product.
3. the preparation method of hydrophobic heat reflection fluorocarbon coating according to claim 1, is characterized in that, described Nano-meter SiO_2
2method of modifying, comprise the following steps:
Step 1, is dissolved in propyl carbinol by HMDS silane coupling agent, uses magnetic agitation 10min, to mixing;
Step 2, pours in there-necked flask by the HMDS silane coupling agent-butanol solution after Homogeneous phase mixing, uses mechanical stirrer to stir, and add Nano-meter SiO_2 under whipped state
2;
Then, there-necked flask is connect reflux, and under whipped state, be slowly warming up to 120 DEG C, after back flow reaction 2h, stop heating, carry out Temperature fall cooling;
Step 3, when cooling down to 60 DEG C, stops mechanical stirring, there-necked flask is placed in ultrasonic disperse instrument ultrasonic disperse 30min.
Step 4, then there-necked flask is connect Vacuum filtration device and carry out vacuum decompression suction filtration, gets filter residue and puts into baking oven, dry 8h at 120 DEG C, after pulverize, to obtain final product.
4., according to the preparation method of the arbitrary described hydrophobic heat reflection fluorocarbon coating of claim 1-3, it is characterized in that, described nano-TiO
2and Nano-meter SiO_2
2average particle size particle size be 20-100nm.
5., according to the preparation method of the arbitrary described hydrophobic heat reflection fluorocarbon coating of claim 1-3, it is characterized in that, described defoamer is silicone antifoam agent;
Described wetting agent is BYK163;
Described dispersion agent is fatty acid dispersion agent.
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| CN105925073A (en) * | 2016-06-27 | 2016-09-07 | 山东科技大学 | Anti-corrosion super-hydrophobic heat reflecting paint and preparation method thereof |
| CN106634267A (en) * | 2016-12-22 | 2017-05-10 | 辽宁师范大学 | Super-hydrophobic and anti-icing transparent coating and preparation method thereof |
| CN107418316A (en) * | 2017-05-24 | 2017-12-01 | 南通高盟新材料有限公司 | A kind of solar reflection coating and preparation method thereof |
| CN109147999A (en) * | 2018-08-27 | 2019-01-04 | 江苏新长峰线缆有限公司 | A kind of ageing-resistant cable |
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| CN105925073B (en) * | 2016-06-27 | 2018-03-20 | 山东科技大学 | A kind of corrosion-resistant super-hydrophobic heat reflection coatings and preparation method thereof |
| CN106634267A (en) * | 2016-12-22 | 2017-05-10 | 辽宁师范大学 | Super-hydrophobic and anti-icing transparent coating and preparation method thereof |
| CN107418316A (en) * | 2017-05-24 | 2017-12-01 | 南通高盟新材料有限公司 | A kind of solar reflection coating and preparation method thereof |
| CN109147999A (en) * | 2018-08-27 | 2019-01-04 | 江苏新长峰线缆有限公司 | A kind of ageing-resistant cable |
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| CN115612360A (en) * | 2022-10-26 | 2023-01-17 | 上海立邦长润发涂料有限公司 | Preparation and application methods of water-based groove paint |
| CN117025076A (en) * | 2023-09-11 | 2023-11-10 | 天津大学 | Self-cleaning anti-reflection nano film and preparation method thereof |
| CN117025076B (en) * | 2023-09-11 | 2024-01-30 | 天津大学 | Self-cleaning anti-reflection nano film and preparation method thereof |
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