CN114316661A - Synthesis method of corrosion-resistant high-throwing-power film type cathode electrophoretic paint - Google Patents
Synthesis method of corrosion-resistant high-throwing-power film type cathode electrophoretic paint Download PDFInfo
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- CN114316661A CN114316661A CN202210015398.0A CN202210015398A CN114316661A CN 114316661 A CN114316661 A CN 114316661A CN 202210015398 A CN202210015398 A CN 202210015398A CN 114316661 A CN114316661 A CN 114316661A
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- 238000005260 corrosion Methods 0.000 title claims abstract description 26
- 230000007797 corrosion Effects 0.000 title claims abstract description 24
- 238000001308 synthesis method Methods 0.000 title claims abstract description 12
- 239000003973 paint Substances 0.000 title claims description 20
- 238000000576 coating method Methods 0.000 claims abstract description 54
- 239000011248 coating agent Substances 0.000 claims abstract description 53
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001723 curing Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005751 Copper oxide Substances 0.000 claims abstract description 7
- 239000004917 carbon fiber Substances 0.000 claims abstract description 7
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 47
- 239000000839 emulsion Substances 0.000 claims description 40
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 32
- 239000007787 solid Substances 0.000 claims description 26
- 239000011347 resin Substances 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- 230000002209 hydrophobic effect Effects 0.000 claims description 17
- 239000012948 isocyanate Substances 0.000 claims description 17
- 150000002513 isocyanates Chemical class 0.000 claims description 17
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000000049 pigment Substances 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- 239000012752 auxiliary agent Substances 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 9
- 238000004040 coloring Methods 0.000 claims description 9
- 238000004945 emulsification Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 240000002853 Nelumbo nucifera Species 0.000 claims description 8
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 8
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- OQSZFKFFOJWHMV-UHFFFAOYSA-L calcium;n,n-diethylcarbamodithioate Chemical group [Ca+2].CCN(CC)C([S-])=S.CCN(CC)C([S-])=S OQSZFKFFOJWHMV-UHFFFAOYSA-L 0.000 claims description 8
- PUHAKHQMSBQAKT-UHFFFAOYSA-L copper;butanoate Chemical compound [Cu+2].CCCC([O-])=O.CCCC([O-])=O PUHAKHQMSBQAKT-UHFFFAOYSA-L 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 8
- 239000012895 dilution Substances 0.000 claims description 8
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- 239000003822 epoxy resin Substances 0.000 claims description 6
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- 238000000227 grinding Methods 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 150000004756 silanes Chemical class 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 claims description 5
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- WYNCHZVNFNFDNH-UHFFFAOYSA-N Oxazolidine Chemical compound C1COCN1 WYNCHZVNFNFDNH-UHFFFAOYSA-N 0.000 claims description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- 125000002091 cationic group Chemical group 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000000016 photochemical curing Methods 0.000 claims description 5
- -1 polyethylene Polymers 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
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- 239000002904 solvent Substances 0.000 claims description 5
- 238000010189 synthetic method Methods 0.000 claims description 5
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229930195725 Mannitol Natural products 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012753 anti-shrinkage agent Substances 0.000 claims description 4
- 239000000679 carrageenan Substances 0.000 claims description 4
- 229940113118 carrageenan Drugs 0.000 claims description 4
- 235000010418 carrageenan Nutrition 0.000 claims description 4
- 229920001525 carrageenan Polymers 0.000 claims description 4
- 235000015165 citric acid Nutrition 0.000 claims description 4
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims description 4
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011258 core-shell material Substances 0.000 claims description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 4
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000594 mannitol Substances 0.000 claims description 4
- 235000010355 mannitol Nutrition 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 claims description 4
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 claims description 4
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 4
- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 claims description 2
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Abstract
The invention discloses a synthesis method of a corrosion-resistant high-throwing-power film-type cathode electrophoretic coating, and particularly relates to the technical field of cathode electrophoretic coatings, wherein the cathode electrophoretic coating is prepared by a special preparation process, so that the prepared cathode electrophoretic coating not only has excellent normal-temperature storage stability, but also has strong integral surface hydrophobicity, has a contact angle with water larger than 130 degrees, can reduce the surface tension of the electrophoretic coating to a certain extent, can reduce irregular small pits formed on the surface of the coating after drying a wet film, increase the smoothness after film forming, reduce the problem of shrinkage cavity caused by the existence of foreign matters in the curing process of the coating, has good storage stability and curing speed, simultaneously, the coating has good scratch resistance due to the arrangement of a scratch resistance agent, and the cathode electrophoretic coating has a certain corrosion resistance due to the addition of carbon fibers and copper oxide, is beneficial to improving the corrosion resistance of the powder coating.
Description
Technical Field
The invention relates to the technical field of cathode electrophoretic paint, in particular to a synthesis method of corrosion-resistant high-throwing-power film type cathode electrophoretic paint.
Background
The cathode electrophoretic paint is a bi-component, one component is white uniform emulsion liquid, the other component is gray or black pigment slurry, the raw materials mainly comprise epoxy resin, ether alcohol compound, isocyanate and the like, the electrophoretic paint is from the 30 th century of 20 th century, the research on synthetic cationic resin is started from the middle of the 60 th century of 20 th century, the electrophoretic paint is used as a primer on household appliances with high requirements on corrosion resistance in the early 70 th of 20 th century, and then the cathode electrophoretic paint with higher corrosion resistance and decorative effect is gradually developed.
Because it has excellent anticorrosion, high swimming rate, high levelling property, high decorative and coating automation degree high, coating pollution characteristics such as being few, the wide application is in the automotive industry to popularize and apply to building materials, light industry, household electrical appliances and other industrial fields and hardware and handicraft surface anticorrosion and decoration, the technological process is: feeding → resin dissolution → epoxy amine addition → isocyanate blocking agent → resin neutralization → emulsification → component 1 emulsion; feeding → resin pigment → grinding and dispersing → adjusting → component 2 color paste, but the problem of shrinkage cavity is easily caused by the fact that some irregular small pits are formed on the surface of the dried cathode electrophoretic coating after the cathode electrophoretic coating prepared by the preparation method of the cathode electrophoretic coating in the prior art is used, so that the smoothness after film forming is lower, the hydrophobic effect, the wear-resisting effect and the corrosion-resisting effect are not ideal enough, the cathode electrophoretic coating is easily polluted, scratched or corroded by external impurities, and the storage stability is poor, therefore, the research on a new synthesis method of the corrosion-resisting high-throwing-power film type cathode electrophoretic coating has important significance for solving the problems.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for synthesizing a corrosion-resistant high-throwing-power film type cathode electrophoretic coating, and the technical problems to be solved by the invention are as follows: the cathode electrophoretic coating prepared by the preparation method of the cathode electrophoretic coating in the prior art is easy to have a problem of shrinkage cavity due to the fact that irregular small depressions are formed on the surface of the dried cathode electrophoretic coating when the cathode electrophoretic coating is used, so that smoothness after film forming is low, a hydrophobic effect, a wear-resisting effect and a corrosion-resisting effect are not ideal enough, the cathode electrophoretic coating is easy to be polluted, scratched or corroded by external impurities, and storage stability is poor.
In order to achieve the purpose, the invention provides the following technical scheme: a synthetic method of a corrosion-resistant high-throwing-power film type cathode electrophoretic coating comprises the following steps:
s1, adding measured dispersion resin, solvent, acetic acid and deionized water into a dispersion container in sequence, stirring, mixing uniformly, adding pigment, friction-resistant material and catalyst slurry, dispersing at 600 plus material rotation speed of 1000rpm, standing for more than 8h, dispersing at 500 plus material rotation speed of 700rpm for 30min until no carbon black dry powder is seen, grinding by a sand mill until the fineness is qualified, finally adjusting the solid content to the index range, controlling the color paste index to be 55% of soil 3% of the solid content and less than or equal to 15um, and discharging for later use to obtain the component A.
S2, uniformly mixing and stirring the oxazolidine modified cationic resin, the curing agent, the carbon fiber, the copper oxide, the formic acid and the auxiliary agent, adopting a special stepwise dilution emulsification process to obtain the oil-in-water core-shell emulsion which is a high-solid stable dispersion with the solid content of (40 +/-1)%, and discharging for later use to obtain the component B.
S3, adjusting the pH value of the emulsion to 7 +/-1 by using a small amount of 10% hydrochloric acid or 10% sodium hydroxide solution, then stirring the emulsion by using a high-shear machine at the rotating speed of 800-2000 rpm, simultaneously slowly adding an active substance, a lotus leaf hydrophobic agent, a filler and a surface hydrophobic anti-sticking auxiliary agent, continuously stirring the added mixture at high speed for 30min until a uniform milky concentrated emulsion is formed, and discharging for later use to obtain a component C.
S4, adding an isocyanate closure containing double bonds into the prepared acrylic resin in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, reacting at 80-90 ℃ for 3 hours under the action of a catalyst, heating to 100 ℃ for reaction for 0.5 hour, pouring the component A for uniform mixing, neutralizing with lactic acid until the pH is 5.0-5.5, adding an active diluent and a photoinitiator, uniformly mixing, pouring the component B for uniform mixing again, adding deionized water, mixing for 10 minutes, sequentially adding the component C, an anti-shrinkage agent, a coloring pigment, an anti-scratch agent and a binder, and uniformly mixing to obtain the photocuring cathode electrophoretic paint.
As a further scheme of the invention: the preparation method of the oxazolidine modified cationic resin comprises the following steps: the following components were added to a reactor equipped with a stirrer, reflux condenser, internal thermometer and nitrogen inlet, respectively, under nitrogen atmosphere: 70-100g of DER-331 epoxy resin, 20-40g of oxazolidine totally-enclosed curing agent and 0.5-1.0g of triphenylphosphine are uniformly stirred and mixed, heated to 140 ℃ with temperature rise of 120-.
As a further scheme of the invention: the active matter is hydrogen-containing siloxane polymer, the hydrogen content of the active matter is 0.1-1.7%, the lotus leaf hydrophobing agent is modified polyethylene wax, the emulsion is silicone-acrylate emulsion or silicone-containing styrene-acrylate emulsion, the average grain diameter is 50-200nm, the silicon content is not less than 2 percent, the solid content is 30-50 percent, the filler is a mixture of two or more of calcium carbonate, quartz powder and titanium dioxide, the granularity of the diatomite or the calcium carbonate is 500-800 meshes, the granularity of the quartz powder is 800-1200 meshes, the average granularity of the titanium dioxide is less than 0.25 mu m, the oil absorption is less than 45g/100g, the titanium dioxide is coated by silicon-aluminum, the surface hydrophobic anti-sticking auxiliary agent is dispersion liquid containing fluorine and silicon, the solid content of the dispersion liquid is 30-50%, and the effective content of fluorine silicon is not lower than 5%.
As a further scheme of the invention: the special stepwise dilution emulsification process comprises the following specific steps: firstly, dispersing and mixing the cationic resin and the curing agent, then adding one fourth of deionized water according to the formula amount, continuously mixing to obtain a W/O emulsion, adding one fourth of deionized water according to the formula amount again, and carrying out phase inversion to obtain the O/W emulsion.
As a further scheme of the invention: the antishrinking agent is a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate, the mass ratio of the calcium diethyldithiocarbamate to the calcium isooctanoate to the copper butyrate is 3:2:1, and the coloring pigment comprises carbon black, perylene black, titanium oxide, phthalocyanine blue, phthalocyanine green and ochre.
As a further scheme of the invention: the binder is MS modified silane.
As a further scheme of the invention: the scratch resistance agent is modified alumina, and the modified alumina comprises the following specific steps: uniformly mixing 6-10 parts of ethylene glycol and 45-55 parts of water, adding a mixture of 1-3 parts of Co (NO3) 2.6H 2O and B2O3, adding 2-5 parts of nano-alumina, heating to 40-50 ℃, preserving heat for 1-3H at 40-50 ℃, adding a mixture of 5-10 parts of citric acid, mannitol and carrageenan, heating to 53-57 ℃, preserving heat for 4-8H at 53-57 ℃, drying and crushing a product at 75-85 ℃ to obtain the modified alumina.
As a further scheme of the invention: the preparation method of the isocyanate closure containing double bonds comprises the following steps: in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, 1mol of isophorone diisocyanate and 0.8mol of 2-hydroxypropyl acrylate are mixed and reacted for 3h at 60 ℃ under the action of a dibutyltin laurate catalyst to prepare the isocyanate closure containing double bonds.
The invention has the beneficial effects that: the invention prepares the cathode electrophoretic coating through a special preparation process, so that the prepared cathode electrophoretic coating not only has excellent normal-temperature storage stability, but also silicon in the coating is easy to form a silicon-oxygen network structure on the surface layer, microscopic concave-convex fluctuation is easy to form on the surface of the coating after the coating is formed into a film, and silicon or fluorine can be uniformly distributed on the surface of the coating after size grading, so that the integral surface has strong hydrophobicity, the contact angle with water is more than 130 degrees, and the coating contains a shrinkage resistant agent component, so that the surface tension of the electrophoretic coating can be reduced to a certain degree, irregular small depressions formed on the surface of the coating after wet film drying can be reduced, the smoothness after film forming is increased, the problem of shrinkage cavity caused by the existence of foreign matters in the curing process of the coating is reduced, and simultaneously MS modified silane is adopted as a binder, so that the storage stability and the curing speed are good, the anti-scratch coating has high temperature resistance, high antifouling performance, high mechanical strength and high workpiece adhesion effect, and simultaneously has a good scratch resistance effect due to the arrangement of the scratch resistance agent, and the cathode electrophoretic coating has a certain corrosion resistance function due to the addition of the carbon fibers and the copper oxide, so that the anti-corrosion performance of the powder coating is improved.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a synthetic method of a corrosion-resistant high-throwing-power film type cathode electrophoretic coating comprises the following steps:
s1, adding measured dispersion resin, solvent, acetic acid and deionized water into a dispersion container in sequence, stirring, mixing uniformly, adding pigment, friction-resistant material and catalyst slurry, dispersing at 600 plus material rotation speed of 1000rpm, standing for more than 8h, dispersing at 500 plus material rotation speed of 700rpm for 30min until no carbon black dry powder is seen, grinding by a sand mill until the fineness is qualified, finally adjusting the solid content to the index range, controlling the color paste index to be 55% of soil 3% of the solid content and less than or equal to 15um, and discharging for later use to obtain the component A.
S2, uniformly mixing and stirring the oxazolidine modified cationic resin, the curing agent, the carbon fiber, the copper oxide, the formic acid and the auxiliary agent, adopting a special stepwise dilution emulsification process to obtain the oil-in-water core-shell emulsion which is a high-solid stable dispersion with the solid content of (40 +/-1)%, and discharging for later use to obtain the component B.
S3, adding an isocyanate closure containing double bonds into the prepared acrylic resin in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, reacting at 80-90 ℃ for 3 hours under the action of a catalyst, heating to 100 ℃ for reaction for 0.5 hour, pouring the component A for uniform mixing, neutralizing with lactic acid until the pH is 5.0-5.5, adding an active diluent and a photoinitiator, uniformly mixing, pouring the component B for uniform mixing again, adding deionized water, mixing for 10 minutes, sequentially adding the component C, a coloring pigment, an anti-scratch agent and a binder, and uniformly mixing to obtain the photocuring cathode electrophoretic paint.
The preparation method of the oxazolidine modified cationic resin comprises the following steps: the following components were added to a reactor equipped with a stirrer, reflux condenser, internal thermometer and nitrogen inlet, respectively, under nitrogen atmosphere: 70-100g of DER-331 epoxy resin, 20-40g of oxazolidine totally-enclosed curing agent and 0.5-1.0g of triphenylphosphine are uniformly stirred and mixed, heated to 140 ℃ with temperature rise of 120-.
The special stepwise dilution emulsification process comprises the following specific steps: firstly, dispersing and mixing the cationic resin and the curing agent, then adding one fourth of deionized water according to the formula amount, continuously mixing to obtain a W/O emulsion, adding one fourth of deionized water according to the formula amount again, and carrying out phase inversion to obtain the O/W emulsion.
The binder is MS modified silane.
The scratch resistance agent is modified alumina, and the specific steps of the modified alumina are as follows: uniformly mixing 6-10 parts of ethylene glycol and 45-55 parts of water, adding a mixture of 1-3 parts of Co (NO3) 2.6H 2O and B2O3, adding 2-5 parts of nano-alumina, heating to 40-50 ℃, preserving heat for 1-3H at 40-50 ℃, adding a mixture of 5-10 parts of citric acid, mannitol and carrageenan, heating to 53-57 ℃, preserving heat for 4-8H at 53-57 ℃, drying and crushing a product at 75-85 ℃ to obtain the modified alumina.
The preparation method of the isocyanate closure containing double bonds comprises the following steps: in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, 1mol of isophorone diisocyanate and 0.8mol of 2-hydroxypropyl acrylate are mixed and reacted for 3h at 60 ℃ under the action of a dibutyltin laurate catalyst to prepare the isocyanate closure containing double bonds.
Example 2:
a synthetic method of a corrosion-resistant high-throwing-power film type cathode electrophoretic coating comprises the following steps:
s1, adding measured dispersion resin, solvent, acetic acid and deionized water into a dispersion container in sequence, stirring, mixing uniformly, adding pigment, friction-resistant material and catalyst slurry, dispersing at 600 plus material rotation speed of 1000rpm, standing for more than 8h, dispersing at 500 plus material rotation speed of 700rpm for 30min until no carbon black dry powder is seen, grinding by a sand mill until the fineness is qualified, finally adjusting the solid content to the index range, controlling the color paste index to be 55% of soil 3% of the solid content and less than or equal to 15um, and discharging for later use to obtain the component A.
S2, mixing and stirring the oxazolidine modified cationic resin, the curing agent, formic acid and the auxiliary agent uniformly, and emulsifying to obtain the emulsifier, thereby obtaining the component B.
S3, adjusting the pH value of the emulsion to 7 +/-1 by using a small amount of 10% hydrochloric acid or 10% sodium hydroxide solution, then stirring the emulsion by using a high-shear machine at the rotating speed of 800-2000 rpm, simultaneously slowly adding an active substance, a lotus leaf hydrophobic agent, a filler and a surface hydrophobic anti-sticking auxiliary agent, continuously stirring the added mixture at high speed for 30min until a uniform milky concentrated emulsion is formed, and discharging for later use to obtain a component C.
S4, adding an isocyanate closure containing double bonds into the prepared acrylic resin in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, reacting at 80-90 ℃ for 3 hours under the action of a catalyst, heating to 100 ℃ for reaction for 0.5 hour, pouring the component A for uniform mixing, neutralizing with lactic acid until the pH is 5.0-5.5, adding an active diluent and a photoinitiator, uniformly mixing, pouring the component B for uniform mixing again, adding deionized water, mixing for 10 minutes, sequentially adding the component C, an anti-shrinkage agent, a coloring pigment and a binder, and uniformly mixing to obtain the photocuring cathode electrophoretic paint.
The preparation method of the oxazolidine modified cationic resin comprises the following steps: the following components were added to a reactor equipped with a stirrer, reflux condenser, internal thermometer and nitrogen inlet, respectively, under nitrogen atmosphere: 70-100g of DER-331 epoxy resin, 20-40g of oxazolidine totally-enclosed curing agent and 0.5-1.0g of triphenylphosphine are uniformly stirred and mixed, heated to 140 ℃ with temperature rise of 120-.
The active matter is hydrogen-containing siloxane polymer, the hydrogen content of the active matter is 0.1-1.7%, the lotus leaf hydrophobic agent is modified polyethylene wax, the emulsion is silicone-acrylic emulsion or silicon-containing styrene-acrylic emulsion, the average particle size of the emulsion is 50-200nm, the silicon content is not less than 2%, the solid content is 30-50%, the filler is a mixture of two or more of calcium carbonate, quartz powder and titanium dioxide, the particle size of the diatomite or the calcium carbonate is 500-800 meshes, the particle size of the quartz powder is 800-1200 meshes, the average particle size of the titanium dioxide is less than 0.25 mu m, the oil absorption is less than 45g/100g, the titanium dioxide is titanium dioxide coated by the silicon-aluminum, the surface hydrophobic anti-sticking auxiliary agent is fluorine-silicon-containing dispersion liquid, the solid content of the dispersion liquid is 30-50%, and the effective content of the fluorine silicon is not less than 5%.
The antishrinking agent is a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate, the mass ratio of the calcium diethyldithiocarbamate, the calcium isooctanoate and the copper butyrate is 3:2:1, and the coloring pigment comprises but is not limited to carbon black, perylene black, titanium oxide, phthalocyanine blue, phthalocyanine green and ochre.
The preparation method of the isocyanate closure containing double bonds comprises the following steps: in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, 1mol of isophorone diisocyanate and 0.8mol of 2-hydroxypropyl acrylate are mixed and reacted for 3h at 60 ℃ under the action of a dibutyltin laurate catalyst to prepare the isocyanate closure containing double bonds.
Example 3:
a synthetic method of a corrosion-resistant high-throwing-power film type cathode electrophoretic coating comprises the following steps:
s1, adding measured dispersion resin, solvent, acetic acid and deionized water into a dispersion container in sequence, stirring, mixing uniformly, adding pigment, friction-resistant material and catalyst slurry, dispersing at 600 plus material rotation speed of 1000rpm, standing for more than 8h, dispersing at 500 plus material rotation speed of 700rpm for 30min until no carbon black dry powder is seen, grinding by a sand mill until the fineness is qualified, finally adjusting the solid content to the index range, controlling the color paste index to be 55% of soil 3% of the solid content and less than or equal to 15um, and discharging for later use to obtain the component A.
S2, uniformly mixing and stirring the oxazolidine modified cationic resin, the curing agent, the carbon fiber, the copper oxide, the formic acid and the auxiliary agent, adopting a special stepwise dilution emulsification process to obtain the oil-in-water core-shell emulsion which is a high-solid stable dispersion with the solid content of (40 +/-1)%, and discharging for later use to obtain the component B.
S3, adjusting the pH value of the emulsion to 7 +/-1 by using a small amount of 10% hydrochloric acid or 10% sodium hydroxide solution, then stirring the emulsion by using a high-shear machine at the rotating speed of 800-2000 rpm, simultaneously slowly adding an active substance, a lotus leaf hydrophobic agent, a filler and a surface hydrophobic anti-sticking auxiliary agent, continuously stirring the added mixture at high speed for 30min until a uniform milky concentrated emulsion is formed, and discharging for later use to obtain a component C.
S4, adding an isocyanate closure containing double bonds into the prepared acrylic resin in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, reacting at 80-90 ℃ for 3 hours under the action of a catalyst, heating to 100 ℃ for reaction for 0.5 hour, pouring the component A for uniform mixing, neutralizing with lactic acid until the pH is 5.0-5.5, adding an active diluent and a photoinitiator, uniformly mixing, pouring the component B for uniform mixing again, adding deionized water, mixing for 10 minutes, sequentially adding the component C, an anti-shrinkage agent, a coloring pigment, an anti-scratch agent and a binder, and uniformly mixing to obtain the photocuring cathode electrophoretic paint.
The preparation method of the oxazolidine modified cationic resin comprises the following steps: the following components were added to a reactor equipped with a stirrer, reflux condenser, internal thermometer and nitrogen inlet, respectively, under nitrogen atmosphere: 70-100g of DER-331 epoxy resin, 20-40g of oxazolidine totally-enclosed curing agent and 0.5-1.0g of triphenylphosphine are uniformly stirred and mixed, heated to 140 ℃ with temperature rise of 120-.
The active matter is hydrogen-containing siloxane polymer, the hydrogen content of the active matter is 0.1-1.7%, the lotus leaf hydrophobic agent is modified polyethylene wax, the emulsion is silicone-acrylic emulsion or silicon-containing styrene-acrylic emulsion, the average particle size of the emulsion is 50-200nm, the silicon content is not less than 2%, the solid content is 30-50%, the filler is a mixture of two or more of calcium carbonate, quartz powder and titanium dioxide, the particle size of the diatomite or the calcium carbonate is 500-800 meshes, the particle size of the quartz powder is 800-1200 meshes, the average particle size of the titanium dioxide is less than 0.25 mu m, the oil absorption is less than 45g/100g, the titanium dioxide is titanium dioxide coated by the silicon-aluminum, the surface hydrophobic anti-sticking auxiliary agent is fluorine-silicon-containing dispersion liquid, the solid content of the dispersion liquid is 30-50%, and the effective content of the fluorine silicon is not less than 5%.
The special stepwise dilution emulsification process comprises the following specific steps: firstly, dispersing and mixing the cationic resin and the curing agent, then adding one fourth of deionized water according to the formula amount, continuously mixing to obtain a W/O emulsion, adding one fourth of deionized water according to the formula amount again, and carrying out phase inversion to obtain the O/W emulsion.
The antishrinking agent is a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate, the mass ratio of the calcium diethyldithiocarbamate, the calcium isooctanoate and the copper butyrate is 3:2:1, and the coloring pigment comprises but is not limited to carbon black, perylene black, titanium oxide, phthalocyanine blue, phthalocyanine green and ochre.
The binder is MS modified silane.
The scratch resistance agent is modified alumina, and the specific steps of the modified alumina are as follows: uniformly mixing 6-10 parts of ethylene glycol and 45-55 parts of water, adding a mixture of 1-3 parts of Co (NO3) 2.6H 2O and B2O3, adding 2-5 parts of nano-alumina, heating to 40-50 ℃, preserving heat for 1-3H at 40-50 ℃, adding a mixture of 5-10 parts of citric acid, mannitol and carrageenan, heating to 53-57 ℃, preserving heat for 4-8H at 53-57 ℃, drying and crushing a product at 75-85 ℃ to obtain the modified alumina.
The preparation method of the isocyanate closure containing double bonds comprises the following steps: in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, 1mol of isophorone diisocyanate and 0.8mol of 2-hydroxypropyl acrylate are mixed and reacted for 3h at 60 ℃ under the action of a dibutyltin laurate catalyst to prepare the isocyanate closure containing double bonds.
The following table is obtained according to examples 1 to 3:
| hydrophobicProperty of (2) | Resistance to shrinkage | Scratch resistance | Corrosion resistance | Stability of | |
| Example 1 | In general | Is poor | In general | It is preferable that | It is preferable that |
| Example 2 | It is preferable that | It is preferable that | In general | Is poor | In general |
| Example 3 | It is preferable that | It is preferable that | It is preferable that | It is preferable that | It is preferable that |
From the comparison in the table above, it can be seen that: the invention prepares the cathode electrophoretic coating through a special preparation process, so that the prepared cathode electrophoretic coating not only has excellent normal-temperature storage stability, but also silicon in the coating is easy to form a silicon-oxygen network structure on the surface layer, microscopic concave-convex fluctuation is easy to form on the surface of the coating after the coating is formed into a film, and silicon or fluorine can be uniformly distributed on the surface of the coating after size grading, so that the integral surface has strong hydrophobicity, the contact angle with water is more than 130 degrees, and the coating contains a shrinkage resistant agent component, so that the surface tension of the electrophoretic coating can be reduced to a certain degree, irregular small depressions formed on the surface of the coating after wet film drying can be reduced, the smoothness after film forming is increased, the problem of shrinkage cavity caused by the existence of foreign matters in the curing process of the coating is reduced, and simultaneously MS modified silane is adopted as a binder, so that the storage stability and the curing speed are good, the anti-scratch coating has high temperature resistance, high antifouling performance, high mechanical strength and high workpiece adhesion effect, and simultaneously has a good scratch resistance effect due to the arrangement of the scratch resistance agent, and the cathode electrophoretic coating has a certain corrosion resistance function due to the addition of the carbon fibers and the copper oxide, so that the anti-corrosion performance of the powder coating is improved.
The points to be finally explained are: although the present invention has been described in detail with reference to the general description and the specific embodiments, on the basis of the present invention, the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A synthetic method of a corrosion-resistant high-throwing-power film type cathode electrophoretic coating is characterized by comprising the following steps:
s1, adding measured dispersion resin, solvent, acetic acid and deionized water into a dispersion container in sequence, stirring, adding pigment, friction-resistant material and catalyst slurry after uniformly mixing, standing for more than 8h after dispersing at 600 plus 1000rpm, dispersing for 30min at 500 plus 700rpm until no carbon black dry powder is seen, grinding by a sand mill until the fineness is qualified, finally adjusting the solid content to the index range, controlling the color paste index to be 55% of soil 3% of the solid content and less than or equal to 15um, and discharging for later use to obtain a component A;
s2, uniformly mixing and stirring oxazolidine modified cationic resin, a curing agent, carbon fibers, copper oxide, formic acid and an auxiliary agent, adopting a special stepwise dilution emulsification process to obtain an oil-in-water core-shell emulsion which is a high-solid stable dispersion, wherein the solid content is (40 +/-1)%, and discharging for later use to obtain a component B;
s3, adjusting the pH value of the emulsion to 7 +/-1 by using a small amount of 10% hydrochloric acid or 10% sodium hydroxide solution, then stirring the emulsion by using a high-shear machine at the rotating speed of 800-2000 rpm, slowly adding an active substance, a lotus leaf hydrophobic agent, a filler and a surface hydrophobic anti-sticking auxiliary agent, continuously stirring the added mixture at high speed for 30min until a uniform milky concentrated emulsion is formed, and discharging for later use to obtain a component C;
s4, adding an isocyanate closure containing double bonds into the prepared acrylic resin in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, reacting at 80-90 ℃ for 3 hours under the action of a catalyst, heating to 100 ℃ for reaction for 0.5 hour, pouring the component A for uniform mixing, neutralizing with lactic acid until the pH is 5.0-5.5, adding an active diluent and a photoinitiator, uniformly mixing, pouring the component B for uniform mixing again, adding deionized water, mixing for 10 minutes, sequentially adding the component C, an anti-shrinkage agent, a coloring pigment, an anti-scratch agent and a binder, and uniformly mixing to obtain the photocuring cathode electrophoretic paint.
2. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the preparation method of the oxazolidine modified cationic resin comprises the following steps: the following components were added to a reactor equipped with a stirrer, reflux condenser, internal thermometer and nitrogen inlet, respectively, under nitrogen atmosphere: 70-100g of DER-331 epoxy resin, 20-40g of oxazolidine totally-enclosed curing agent and 0.5-1.0g of triphenylphosphine are uniformly stirred and mixed, heated to 140 ℃ with temperature rise of 120-.
3. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the active matter is hydrogen-containing siloxane polymer, the hydrogen content of the active matter is 0.1-1.7%, the lotus leaf hydrophobing agent is modified polyethylene wax, the emulsion is silicone-acrylate emulsion or silicone-containing styrene-acrylate emulsion, the average grain diameter is 50-200nm, the silicon content is not less than 2 percent, the solid content is 30-50 percent, the filler is a mixture of two or more of calcium carbonate, quartz powder and titanium dioxide, the granularity of the diatomite or the calcium carbonate is 500-800 meshes, the granularity of the quartz powder is 800-1200 meshes, the average granularity of the titanium dioxide is less than 0.25 mu m, the oil absorption is less than 45g/100g, the titanium dioxide is coated by silicon-aluminum, the surface hydrophobic anti-sticking auxiliary agent is dispersion liquid containing fluorine and silicon, the solid content of the dispersion liquid is 30-50%, and the effective content of fluorine silicon is not lower than 5%.
4. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the special stepwise dilution emulsification process comprises the following specific steps: firstly, dispersing and mixing the cationic resin and the curing agent, then adding one fourth of deionized water according to the formula amount, continuously mixing to obtain a W/O emulsion, adding one fourth of deionized water according to the formula amount again, and carrying out phase inversion to obtain the O/W emulsion.
5. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the antishrinking agent is a composition of calcium diethyldithiocarbamate, calcium isooctanoate and copper butyrate, the mass ratio of the calcium diethyldithiocarbamate to the calcium isooctanoate to the copper butyrate is 3:2:1, and the coloring pigment comprises carbon black, perylene black, titanium oxide, phthalocyanine blue, phthalocyanine green and ochre.
6. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the binder is MS modified silane.
7. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the scratch resistance agent is modified alumina, and the modified alumina comprises the following specific steps: uniformly mixing 6-10 parts of ethylene glycol and 45-55 parts of water, adding a mixture of 1-3 parts of Co (NO3) 2.6H 2O and B2O3, adding 2-5 parts of nano-alumina, heating to 40-50 ℃, preserving heat for 1-3H at 40-50 ℃, adding a mixture of 5-10 parts of citric acid, mannitol and carrageenan, heating to 53-57 ℃, preserving heat for 4-8H at 53-57 ℃, drying and crushing a product at 75-85 ℃ to obtain the modified alumina.
8. The synthesis method of the corrosion-resistant high-throwing-power film type cathode electrophoretic paint according to claim 1, characterized in that: the preparation method of the isocyanate closure containing double bonds comprises the following steps: in a three-neck flask provided with a reflux condenser, a stirrer and a thermometer, 1mol of isophorone diisocyanate and 0.8mol of 2-hydroxypropyl acrylate are mixed and reacted for 3h at 60 ℃ under the action of a dibutyltin laurate catalyst to prepare the isocyanate closure containing double bonds.
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