WATERBORNE CROSSLINKABLE DISPERSIONS

Abstract

The present invention further relates to a waterborne dispersion comprising (A) polymer P; (B) amphiphilic block copolymer obtained with a controlled radical polymerization process and comprising at least blocks [A] and [B], whereby block [A] comprises ethylenically unsaturated monomer(s) bearing water-soluble and/or water-dispersible functional groups (monomer(s) (i)), and block [B] comprises ethylenically unsaturated monomer(s) different from monomer(s) (i) (monomer(s) (ii)); and (C) crosslinker, characterized in that the polymer P is crosslinkable and comprises ethylenically unsaturated monomer(s) bearing crosslinkable functional groups different from monomer(s) (i) and monomer(s) (ii) (monomer(s) (iii)) in an amount of from 1 to 10 wt. %, based on the total weight of monomers used to prepare the polymer P, the amount of lock copolymer is higher than 1 wt. % and lower than 30 wt. %, based on the total weight of monomers used to prepare the block copolymer and polymer P; the acid value of the composition consisting of block copolymer and polymer P is higher than 1 and lower than 17 mg KOH per g of the block copolymer-polymer P composition.

Claims

1. A waterborne dispersion comprising (A) polymer P; (B) amphiphilic block copolymer obtained with a controlled radical polymerization process and comprising at least blocks [A] and [B], whereby block [A] comprises ethylenically unsaturated monomer(s) bearing water-soluble and/or water-dispersible functional groups (monomer(s) (i)), and block [B] comprises ethylenically unsaturated monomer(s) different from monomer(s) (i) (monomer(s) (ii)); and (C) crosslinker, wherein the polymer P is crosslinkable and comprises ethylenically unsaturated monomer(s) bearing crosslinkable functional groups different from monomer(s) (i) and monomer(s) (ii) (monomer(s) (iii)) in an amount of from 1 to 10 wt. %, based on the total weight of monomers used to prepare the polymer P, the amount of block copolymer is higher than 1 wt. % and lower than 30 wt. %, based on the total weight of monomers used to prepare the block copolymer and polymer P; the acid value of the composition consisting of block copolymer and polymer P is higher than 1 and lower than 17 mg KOH per g of the block copolymer-polymer P composition.

2. The waterborne dispersion according to claim 1, wherein the acid value of the block copolymer-polymer composition is higher than 1.5 and lower than 17, more preferably from 3 to 16, more preferably from 5 to 15 and most preferably from 9 to 15.

3. The waterborne dispersion according to claim 1, wherein the polymer P comprises ethylenically unsaturated monomer(s) (iii) bearing crosslinkable functional groups in an amount of from 2 to 7.5 wt. %, based on the total weight of monomers used to prepare the polymer P, more preferably from 2 to 5 wt. %.

4. The waterborne dispersion according to claim 1, wherein the amount of the block copolymer is from 2 to 20 wt. %, based on the total weight of monomers used to prepare the block copolymer and polymer P, preferably from 3 to 15 wt. %, more preferably from 4 to 12 wt. %.

5. The waterborne dispersion according to claim 1, wherein the ethylenically unsaturated monomer(s) (iii) bearing crosslinkable functional groups are carbonyl functional ethylenically unsaturated monomer(s), preferably ketone functional ethylenically unsaturated monomer(s).

6. The waterborne dispersion according to claim 5, wherein the ketone functional ethylenically unsaturated monomers are selected from the group consisting of (meth)acrolein, diacetone acrylamide, vinyl methyl ketone, and any mixture thereof.

7. The waterborne dispersion according to claim 5, wherein the ketone functional ethylenically unsaturated monomers is diacetone acrylamide.

8. The waterborne dispersion according to claim 1, wherein the crosslinker is a polyhydrazide, preferably a dihydrazide functional compound (containing two hydrazide groups (OCNHNH.sub.2)) with a molar mass below 1000 g/mole, preferably with a molar mass below 500 g/mole, more preferably with a molar mass below 250 g/mole, especially preferably adipic dihydrazide.

9. The waterborne dispersion according to claim 1, wherein block [A] has a Hansch parameter of less than 1.5 and block [B] has a Hansch parameter of at least 1.5.

10. The waterborne dispersion according to claim 1, wherein the amount of ethylenically unsaturated monomer(s) (ii) in block [B] is at least 75 wt. %, more preferably at least 90 wt. %, most preferably at least 95 wt % relative to the total weight amount of monomers used to prepare block [B].

11. The waterborne dispersion according to claim 1, wherein at least 90 wt. %, preferably at least 95 wt. % of the total amount of monomers (i) present in the block copolymer-polymer composition is present in block [A].

12. The waterborne dispersion according to claim 1, wherein the water-soluble and/or water-dispersible functional groups are carboxylate groups.

13. The waterborne dispersion according to claim 1, wherein the block copolymer is a diblock copolymer [A].sub.x[B].sub.y.

14. The waterborne dispersion according to claim 1, wherein block [A] has an average degree of polymerization x where x is an integer from 3 to 200, preferably lower than 150, more preferably lower than 100 and most preferably lower than 50.

15. The waterborne dispersion according to claim 1, wherein block [B] has an average degree of polymerization y where y is an integer >10, preferably >50, more preferably >100, and most preferably >150, where y>x.

16. The waterborne dispersion according to claim 1, wherein the polymer P is obtained by an emulsion polymerization effected in the presence of the block copolymer.

17. The waterborne dispersion according to claim 1, wherein the polymer P further contains ethylenically unsaturated monomer(s) (ii) different from (i) and (iii).

18. The waterborne dispersion according to claim 1, wherein the ethylenically unsaturated monomer(s) (ii) are selected from the group consisting of C.sub.1-12alkyl(meth)acrylate monomers, cyclohexyl (meth)acrylate, styrenic monomers and any mixture thereof, preferably the ethylenically unsaturated monomer(s) (ii) are selected from the group consisting of C.sub.1-12 alkyl(meth)acrylate monomers and any mixture thereof.

19. The waterborne dispersion according to claim 1, wherein the calculated glass transition temperature of the block copolymer is from 10 to 250 C., preferably from 30 to 200 C., more preferably from 50 to 150 C. and especially preferably from 60 to 120 C.

20. The waterborne dispersion according to claim 1, wherein the at least 20 wt. %, more preferably at least 30 wt. %, even more preferably of at least 50 wt. %, of the polymer composition of the polymer P has a polymer fraction with a calculated glass transition temperature >5 C., more preferably >10 C., even more preferably >15 C. and preferably <90 C., more preferably <70 C., even more preferably <50 C.

21. The waterborne dispersion according to claim 1, wherein the weight average molecular weight of the block copolymer is in the range of from 2,000 to 100,000 g/mol, more preferably from 5,000 to 50,000 g/mol and even more preferably from 7,000 to 35,000 g/mol.

22. The waterborne dispersion according to claim 1, wherein the weight average molecular weight of the block copolymer-polymer composition is higher than 100,000 g/mol, more preferably in the range of from 100,000 to 500,000 g/mol and even more preferably from 125,000 to 350,000 g/mol.

23. The waterborne dispersion according to claim 1, wherein the block copolymer is obtained via reversible addition-fragmentation chain transfer (RAFT) polymerization in the presence of a control agent and a source of free radicals, preferably the RAFT polymerization is effected in solution.

24. The waterborne dispersion according to claim 1, wherein the waterborne dispersion is a one-pack system.

25. A process for preparing a waterborne dispersion according to claim 1, whereby the process comprises at least the following steps: (a) Preparing an amphiphilic block copolymer comprising at least blocks [A] and [B] in at least the following steps: a. subjecting at least ethylenically unsaturated monomer(s) (i) bearing water-soluble and/or water-dispersible functional groups to a controlled radical polymerization to obtain block [A], b. subjecting at least ethylenically unsaturated monomer(s) (ii) that is different from (i) to a controlled radical polymerization to obtain block [B], wherein block [A] is prepared in the presence of block [B] or wherein block [B] is prepared in the presence of block [A], (b) optionally converting at least part of the potentially ionic groups to ionic groups present in block [A] before, during or after preparation of block [B]; (c) conducting an emulsion polymerization process in water of at least an ethylenically unsaturated monomer(s) bearing crosslinkable functional groups (iii) different from (i) and (ii) in the presence of the block copolymer obtained in step (a) or step (b) (when present) to obtain the block copolymer-polymer P; (d) adding a crosslinker to the block copolymer-polymer composition; wherein the amount of the block copolymer is higher than 1 wt. % and lower than 30 wt. %, based on the total weight of monomers used to prepare the block copolymer-polymer composition; the acid value of the block copolymer-polymer composition is higher than 1 and lower than 17 mg KOH per g of the block copolymer-polymer P composition.

26. A coating composition comprising the waterborne dispersion of claim 1.

27. A coating composition according to claim 26, wherein the coating composition further comprises titanium dioxide in an amount of 15 to 40 volume-%, more preferably from 18 to 30 volume-%, relative to the volume of non-volatile material in the coating composition.

28. A coating composition according to claim 26, wherein the coating composition is a one-pack system.

29. A method of coating a substrate comprising the steps of (1) applying the coating composition from claim 26 to a substrate and (2) drying the coating composition.

30. The method according to claim 29, wherein the substrate is aluminum or pre-treated aluminum.

31. The method according to claim 29, wherein the substrate is a profile for an architectural article, preferably the profile is a door frame, a window frame or door panel.

32. An article having a coating deposited thereon, wherein the coating is obtained by depositing a coating composition according to claim 26 to a substrate and drying the coating composition.

33. An article according to claim 32, wherein the article is a profile for an architectural article, preferably the profile is a door frame, a window frame or door panel.

34. The article according to claim 32, wherein the substrate comprises aluminium, preferably the substrate is aluminum or pre-treated aluminum.

35. The article according to claim 32, wherein the coating passes the detergent resistance test in AAMA 2604-17, section 8.7.4 and the detergent resistance test described in AAMA 2605-17, section 8.7.4.

Description

EXAMPLE 1

[0122] 434 gram of deionized water and 209 gram of the aqueous dispersion of oligomer 1 (14.1% in water) were added to a 2 L flask equipped with stirrer, condenser cooler and temperature measuring probe. The reaction mixture was heated while stirring to 85 C. under nitrogen atmosphere. Then a pre-emulsified monomer mixture consisting of in total 171 gram deionized water, 3.7 gram SLS (30 wt % in water), 430.8 gram BMA, 63.2 gram MMA, 48.7 gram BA and 16.8 gram DAAM was gradually added over a time period of 2 hours. In parallel to this feed, an initiator mixture of 1.6 gram APS and 63.6 gram deionized water set at a pH of about 8 with ammonia was added over a time period of 2 hours. At the end of both feeds the reaction mixture was mixed for 30 more minutes at 85 C. A post reaction with tert-butyl hydroperoxide and isoascorbic acid was then performed to react any residual monomer. The resultant emulsion was then cooled to room temperature and a sample was taken for SEC analysis. Following, a mixture of 6.9 gram ADH and 23.4 gram deionized water was added while mixing for 5 more minutes. The pH of the latex was set to about 8 by addition of ammonia.

[0123] Examples 2, 3, 4 and Comparative Examples 1 and 2 were prepared according a similar recipe and procedure as applied for Example 1, where only the type and amount of oligomer (on total polymer weight) was varied. An additional amount of deionized water was added during processing to reduce the viscosity as needed to ensure good mixing.

[0124] Comparative Examples 3 and 4 were prepared according a similar recipe and procedure as applied for Example 1, where only the amount of DAAM in the monomer mixture was varied from 3% (Example 1) to 0% (Comparative Example 3) or 0.5% (Comparative Example 4), and the amount of ADH relative to the total amount of DAAM in the oligomer polymer composition was kept constant, meaning that Comparative Example 3 did not contain any ADH.

[0125] Comparative Example 5 was synthesized according the same recipe and procedure as disclosed in WO2009090252 (Example 1).

[0126] Comparative Example 6 was synthesized according the same recipe and procedure as disclosed in WO2009121911 (Example 2).

[0127] Comparative Example 7 was prepared according a similar recipe and procedure as applied for Example 1, where the amount of oligomer 6 was initially varied from 5% to 15% and 30%, yet use of oligomer 6 at 5% and 15% resulted in significant fouling and grit formation during preparation of the emulsion polymer and synthesis of these binders could not be completed. At 30% oligomer 6 the fouling was still significant, but the synthesis could be completed. Over time however this binder showed settling (unstable), meaning that this binder was unsuited for further evaluation. Clearly, these surprising results show that a block copolymer is much more effective in emulsion particle stabilization than a statistical copolymer, and that use of a block copolymer at the same time results in an excellent detergent resistance performance following the test as described in section 8.7.4 of AAMA 2604-17 and AAMA 2605-17 specifications.

Comparative Example 8 (CE8)

[0128] CE8 is an emulsion polymer that does not contain an oligomer but is based on the same overall composition as Example 1, meaning it has the same low acid amount (0.9 wt %) and low surfactant amount (0.2%) as used in Example 1. The overall monomer composition of CE8 is similar to the combined monomer composition of the oligomer and polymer of Example 1. CE8 was synthesized as follows: 736 gram of deionized water was added to a 2 L flask equipped with stirrer, condenser cooler and temperature measuring probe, and heated to 70 C. while stirring under nitrogen atmosphere. Then 10 wt % of a pre-emulsified monomer mixture consisting of in total 205 gram deionized water, 4.5 gram SLS (30 wt % in water), 517.8 gram BMA, 104.1 gram MMA, 58.5 gram BA, 20.2 gram DAAM and 6.4 gram MAA was added to the reactor. The temperature of the reactor was kept for 5 minutes at 70 C. and then 10 wt % of an initiator mixture of 1.9 gram APS and 76.4 gram deionized water was added to start the seed formation. After 15 minutes the reaction mixture was further heated to 85 C. and then the remaining 90 wt % of monomer and initiator mixture feed was fed to the reactor over a time period of 2 hours. At the end of both feeds the reaction mixture was mixed for 30 minutes at 85 C. A post reaction with tert-butyl hydroperoxide and isoascorbic acid was then performed to react any residual monomer. The resultant emulsion was then cooled to room temperature and a sample was taken for SEC analysis. The pH of the latex was then set to about 8 by addition of ammonia and a mixture of 8.3 gram ADH and 28.2 gram deionized water was added while mixing for 5 more minutes.

Comparative Example 9 (CE9)

[0129] CE9 is an emulsion polymer that does not contain an oligomer but is based on a surfactant amount (1.4 wt %) and acid monomer amount (5 wt %) that is typically applied for conventional emulsion polymers. CE9 was synthesized as follows: 720 gram of deionized water and 28.8 gram SLS (30% in water) was added to a 2 L flask equipped with stirrer, condenser cooler and temperature measuring probe, and heated to 70 C. while stirring under nitrogen atmosphere. Then 10 wt % of a pre-emulsified monomer mixture consisting of in total 203 gram deionized water, 4.4 gram SLS (30 wt % in water), 512 gram BMA, 49.1 gram MMA, 82.9 gram BA, 19.9 gram DAAM and 34.9 gram MAA was added to the reactor. The temperature of the reactor was kept for 5 minutes at 70 C. and then 10 wt % of an initiator mixture of 1.9 gram APS and 75.5 gram deionized water was added to start the seed formation. After 15 minutes the reaction mixture was further heated to 85 C. and then the remaining 90 wt % of monomer and initiator mixture feed was fed to the reactor over a time period of 2 hours. At the end of both feeds the reaction mixture was mixed for 30 minutes at 85 C. A post reaction with tert-butyl hydroperoxide and isoascorbic acid was then performed to react any residual monomer. The resultant emulsion was then cooled to room temperature and a sample was taken for SEC analysis. The pH of the latex was then set to about 8 by addition of ammonia and a mixture of 8.2 gram ADH and 27.8 gram deionized water was added while mixing for 5 more minutes.

[0130] The specifications of the prepared emulsion polymers are given in Table 2. Solids level was gravimetrically determined. Viscosity of the binder was measured within 48 hours after synthesis, indicated as the initial viscosity, and after 6 months storage at room temperature, to determine shelf-stability. Final free monomer levels were all below 500 ppm.

TABLE-US-00002 TABLE 2 Viscosity Initial after 6 Particle viscosity months size Mn/Mw Exam- Solids pH (Brookfield) (Brookfield) (DLS) (SEC) ple [%] [] [mPa .Math. s] [mPa .Math. s] [nm] [kg/mol] EX1 33.4 8.1 93 84 65 60/170 EX2 29.3 8.1 900 906 59 40/116 EX3 34.2 8.2 81 90 70 not available EX4 39.4 8.2 76 76 92 63/187 CE1 39.6 8.2 20 23 109 90/314 CE2 26.5 8.1 1200 1442 51 35/97 CE3 34.6 8.1 182 180 63 58/164 CE4 34.3 8.1 176 173 65 60/167 CE5 34.9 8.3 66 67 69 49/333 CE6 36.1 8.5 118 168 77 23/194 CE7 33.5 8.0 49 47 76 not available CE8 39.3 8.2 5 5 337 118/543 CE9 39.0 8.0 32 27 104 125/354

[0131] White pigmented formulations of the examples (EX) and comparative examples (CE) were prepared using the ingredients and amounts (in grams) as listed in Table 3. All white pigmented formulations (denoted as PF) were prepared at a target total VOC content of around 150 g/L. The weighed amount of binder was adjusted relative to the solids content to ensure that each formulation contained the same level of binder on total formulation solids. The pigment volume concentration (PVC) was set at 20-21%. For preparation of the formulations, a let down was prepared by slowly adding the listed formulation ingredients (coalescing agents, wetting agent, deionized water, and neutralizing agent) as pre-mix to the binder under adequate agitation, followed by 15 minutes mixing. The mill base dispersion was separately prepared from mixing the deionized water, ZetaSperse 3600, Airase 5200 and Kronos 2160 under high shear for 15-20 minutes. This mill base dispersion was then added to the let down under adequate agitation, followed by some defoamer (Byk 024) and 15 minutes mixing. The viscosity of the formulation was then adjusted to about 400 mPa.Math.s with (part of) the indicated amounts of rheology modifiers (Acrysol RM-8W and RM-12W) to enable spray application.

TABLE-US-00003 TABLE 3 EX1- EX2- EX3- EX4- CE1- CE2- CE3- CE4- CE5- CE6- CE8- CE9- PF PF PF FP PF PF PF PF PF PF PF PF Let down EX1 672.6 EX2 766.7 EX3 656.8 EX4 570.1 CE1 567.3 CE2 847.7 CE3 649.2 CE4 654.9 CE5 643.7 CE6 622.2 CE8 571.6 CE9 575.9 Butyl Cellosolve .sup.1 30.5 30.5 30.5 30.5 30.5 30.5 30.5 30.5 30.5 30.5 30.5 30.5 Dowanol DPnB .sup.2 17.3 17.3 17.3 17.3 17.3 17.3 17.3 17.3 17.3 17.3 17.3 17.3 Troysol LAC .sup.3 6.8 6.8 6.8 6.8 6.8 6.8 6.8 6.8 6.8 6.8 6.8 6.8 Deionized water 47.8 47.8 47.8 69.8 72.7 47.8 47.8 47.8 59.0 80.4 68.5 64.0 Ammonia (28%) 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 1.2 Total let down 776.2 870.3 760.5 695.7 695.8 951.3 752.8 758.5 758.5 758.4 695.9 695.7 Mill base dispersion Deionized water 37.5 37.5 37.5 37.5 37.5 37.5 37.5 37.5 37.5 37.5 37.5 37.5 ZetaSperse 3600 .sup.4 23.7 23.7 23.7 23.7 23.7 23.7 23.7 23.7 23.7 23.7 23.7 23.7 Airase 5200 .sup.5 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 Kronos 2160 .sup.6 189.5 189.5 189.5 189.5 189.5 189.5 189.5 189.5 189.5 189.5 189.5 189.5 Total mill base 251.7 251.7 251.7 251.7 251.7 251.7 251.7 251.7 251.7 251.7 251.7 251.7 dispersion BYK 024 .sup.7 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Acrysol RM-8W .sup.8 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 Acrysol RM-12W .sup.8 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 26.0 Total formulation PF 1080.4 1174.5 1064.6 999.9 999.9 1255.5 1057.0 1062.7 1062.7 1062.6 1000.0 999.9 .sup.1 Ethylene Glycol Monobutyl Ether; coalescing agent (Dow Chemical Company) .sup.2 Dipropylene Glycol n-Butyl Ether; coalescing agent (Dow Chemical Company) .sup.3 Surfactant; wetting agent (Troy Chemical Corp.) .sup.4 Dispersant (Evonik) .sup.5 Defoamer (Evonik) .sup.6 Titanium dioxide pigment (Kronos) .sup.7 Defoame (Byk) .sup.8 Rheology modifier (Dow Chemical Company); prior to addition diluted with deionized water (1:1 weight ratio)

[0132] Each of the formulations were spray applied onto chromated aluminum panels (Q-panels AL-36, available from Q-lab) and allowed to dry for 10-15 min at ambient temperature (23 C.), followed by forced cure drying at 50 C. for 20 min. Subsequently, all panels were left to dry at ambient temperature (23 C.) and 50% relative humidity for 7 days prior to testing. The targeted dry film thickness of the coatings was about 1.2 to 1.6 mils (30 to 40 microns).

[0133] The detergent resistance of the dried coatings was determined following the test as described in section 8.7.4 of AAMA 2604-17 and of AAMA 2605-17. According to this test, a 3% (by weight) solution of detergent as prescribed in ASTM D2248, and distilled water was prepared. The solid detergent composition is as given in Table 4.

TABLE-US-00004 TABLE 4 % by Technical grade reagent weight Tetrasodium pyrophosphate (Na.sub.4P.sub.2O.sub.7), anhydrous 53 Sodium Sulfate (Na.sub.2SO.sub.4), anhydrous 19 Sodium metasilicate (Na.sub.2SiO.sub.3), anhydrous 7 Sodium carbonate (Na.sub.2CO.sub.3), anhydrous 1 Dodecylbenzenesulfonic acid, sodium salt, tech. 88% 20

[0134] The coated chromated aluminum panels were immersed in the detergent solution at 38 C. for 72 hours. The samples were then removed and wiped dry. Tape 25 mm wide was immediately applied by pressing down firmly against the coating to eliminate voids and air pockets. The tape specified per ASTM D3359 calls for Permacel 99, which is no longer available. Scotch Performance Flatback Tape 2525 available from 3M was used as alternative, which has a higher bond strength than Permacel 99 (adhesion to steel: 69 oz./inch width for Scotch 2525 versus 52 oz./inch width for Permacel 99). The tape was placed longitudinally along the entire length of the test specimens. If blisters are visible, the blistered area was taped and rated. The tape was sharply pulled off at a right angle to the plane of the surface being tested, per ASTM D3359. Passed means that there was no loss of adhesion of the coating to the metal, no blistering and no significant visual change in appearance when examined by the unaided eye. Results for the detergent resistance test are given in Table 5. The results clearly show that the working examples (EX) pass the challenging detergent resistance test on chromated aluminum panels whereas the comparative examples (CE) all fail this test.

TABLE-US-00005 TABLE 5 Detergent Example resistance EX1-PF Passed EX2-PF Passed EX3-PF Passed EX4-PF Passed CE1-PF Failed (a/b/c) CE2-PF Failed (a/b/c) CE3-PF Failed (a/c) CE4-PF Failed (c) CE5-PF Failed (a/b/c) CE6-PF Failed (a/b/c) CE8-PF Failed (a/b/c) CE9-PF Failed (a/b/c) a) failed on significant change in film appearance b) failed on blister formation c) failed on tape adhesion

[0135] Furthermore, significant differences in coating adhesion were found between the examples and the comparative examples. All examples (EX) showed good dry, wet and boiling water coating adhesion (min 3B-5B) when tested in the white pigmented formulation according the tests described in section 8.7.4 of the AAMA 2604-17 and AAMA 2605-17 specification. All comparative examples (CE) however showed poor dry, wet and boiling water adhesion (OB to max 3B) when tested in the white pigmented formulation according the tests described in section 8.7.4 of the AAMA 2604-17 and AAMA 2605-17 specification.

[0136] CE7 was not tested as this binder was not storage stable (settling within a few days) and could not be formulated.

[0137] FIGS. 1-5

[0138] Of Examples 1 and 2 and Comparative Examples 1-3, photos of coated chromated aluminum panels (Q-panels) after the detergent resistance test as described in section 8.7.4 of AAMA 2604/2605-17 have been taken, where the lower half of the coated panel was immersed for 72 hours in the 3 wt. % detergent solution at 38 C.:

[0139] FIG. 1: Example 1 (code 416).

[0140] FIG. 2: Example 2 (code 417),

[0141] FIG. 3: Comparative Example 1 (code 415),

[0142] FIG. 4: Comparative Example 2 (code 418), and

[0143] FIG. 5: Comparative Example 3 (code 419).

[0144] All photos were taken after performing the tape adhesion test, except for Comparative Example 1 (code 415) and Comparative Example 2 (code 418) as these samples already demonstrated clear adhesion failure before performing the tape adhesion test as visible from the strong coating delamination from the substrate.