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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- CN105295583A CN105295583A CN201510771637.5A CN201510771637A CN105295583A CN 105295583 A CN105295583 A CN 105295583A CN 201510771637 A CN201510771637 A CN 201510771637A CN 105295583 A CN105295583 A CN 105295583A
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- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000011248 coating agent Substances 0.000 title claims abstract description 40
- 238000000576 coating method Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000004048 modification Effects 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 19
- 239000013530 defoamer Substances 0.000 claims description 17
- 239000000080 wetting agent Substances 0.000 claims description 14
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 11
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 10
- 229940043232 butyl acetate Drugs 0.000 claims description 10
- 239000012467 final product Substances 0.000 claims description 10
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 9
- 238000009775 high-speed stirring Methods 0.000 claims description 9
- 238000010907 mechanical stirring Methods 0.000 claims description 9
- 229910000077 silane Inorganic materials 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 230000008878 coupling Effects 0.000 claims description 6
- 238000010168 coupling process Methods 0.000 claims description 6
- 238000005859 coupling reaction Methods 0.000 claims description 6
- 230000006837 decompression Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 125000005313 fatty acid group Chemical group 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 229920002050 silicone resin Polymers 0.000 abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000002310 reflectometry Methods 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000004886 process control Methods 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000005543 nano-size silicon particle Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- -1 alcohol ester Chemical class 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000003703 image analysis method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
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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