CN116445078A - 一种用于汽车紧固件的无铬防腐涂层及其制备方法 - Google Patents
一种用于汽车紧固件的无铬防腐涂层及其制备方法 Download PDFInfo
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- CN116445078A CN116445078A CN202310305331.5A CN202310305331A CN116445078A CN 116445078 A CN116445078 A CN 116445078A CN 202310305331 A CN202310305331 A CN 202310305331A CN 116445078 A CN116445078 A CN 116445078A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/103—Anti-corrosive paints containing metal dust containing Al
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F13/00—Inhibiting corrosion of metals by anodic or cathodic protection
- C23F13/02—Inhibiting corrosion of metals by anodic or cathodic protection cathodic; Selection of conditions, parameters or procedures for cathodic protection, e.g. of electrical conditions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/28—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen sulfur-containing groups
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
本申请提供了一种用于汽车紧固件的无铬防腐涂层及其制备方法;按总质量计,所述涂层的原料包括:金属粉12‑35%、氧化铝0.3‑1.2%、溶剂5‑15%、硅烷偶联剂10‑20%、钝化剂0.001‑0.005%、硼酸或植酸1‑3%、润湿流平剂0.5‑1%、消泡剂0.2‑0.5%、水补足余量为100%;通过优化配方组分体系和涂层的制备方法,本申请的涂层附着力强、耐磨性和耐腐蚀性高、涂层体系稳定,可用于汽车紧固件中。
Description
技术领域
本发明涉及防腐涂料技术领域,C09D183/00,尤其涉及一种用于汽车紧固件的无铬防腐涂层及其制备方法。
背景技术
达克罗涂层因其良好的防腐蚀能力被广泛用作金属工件的表面防护层,其制备原料包括片状锌粉、片状铝粉、铬酐及一系列助剂,其中锌和铝对金属具有阴极保护作用,热传导效率高,但铬离子因毒性强且被证明存在致癌作用已被严格限制使用,因此开发无铬防腐涂层成为了相关技术的发展方向;然而,目前的无铬涂层附着力、硬度和耐磨、耐蚀性较低,涂料体系稳定性也不佳,无铬涂层的广泛应用受到了限制,尤其是对于性能要求较严苛的汽车紧固件而言,因其所处的环境较为复杂,需要避免水或油污等的腐蚀,现有技术中无铬涂层在汽车底盘紧固件上的使用效果仍然表现不佳。
中国专利CN112280040A公开了一种新型绿色环保高防腐锌铝涂层,通过不同硅烷偶联剂的复配和金属氧化物溶胶的共同作用,形成涂层的成膜体系,所制备涂料具有优异的稳定性,但是该涂层达到最佳防腐效果的厚度较厚,为10μm,且涂层对金属基层的附着力仍然不足。中国专利CN107955539B公开了一种防腐涂料及其制备方法,采用锌铝合金粉、四氟化锆、γ-氨丙基三乙氧基硅烷、羧甲基纤维素钠、肌醇六磷酸酯等的共同作用,提高涂层的耐蚀性和生产环境的安全性,并降低图层固化温度,但是该涂层的抗冲击性能存在一定的提升空间。
因此,需开发一种附着力强、耐磨性和耐腐蚀性高、涂层体系稳定的汽车紧固件专用涂层。
发明内容
为了解决上述技术问题,本发明首先提供了一种用于汽车紧固件的无铬防腐涂层;按总质量计,所述涂层的原料包括:金属粉12-35%、氧化铝0.3-1.2%、溶剂5-15%、硅烷偶联剂10-20%、钝化剂0.001-0.005%、硼酸或植酸1-3%、润湿流平剂0.5-1%、消泡剂0.2-0.5%、水补足余量为100%。
进一步地,所述金属粉包括锌粉、铝粉、镁粉、锌铝合金粉、镍粉中的一种或多种的组合。
进一步地,所述金属粉为锌粉、铝粉或锌铝合金粉中的至少一种。
优选地,所述金属粉为锌粉和铝粉,质量比为(10-30):(2-5)。
进一步优选地,所述锌粉为片状结构,最大片层直径不大于20μm,片层厚度不大于0.8μm。
进一步地,所述锌粉的最大片层直径为5-20μm,片层厚度为0.2-0.8μm。
进一步地,所述铝粉为片状结构,最大片层直径为0.8-10μm,片层厚度为0.1-0.5μm。
进一步地,所述氧化铝粉为球形结构,粒径为0.3-10μm;优选为0.3-5μm;在涂层体系中,锌粉和铝粉的片层结构平行排列且构成交错和重叠结构,有效地抑制了水分子和腐蚀介质在涂层中的渗透速度,由于这种层叠结构并非是紧密堆积,而是存在一定的层间空隙,本申请加入球状的氧化铝,并进一步规定其粒径,进一步提高涂层的致密性并增强涂层的力学性能,但是当其添加量过多时,其空间阻碍作用表现的较为明显,反而会降低锌粉和铝粉的防腐效果,并且氧化铝的表面含有一定的醇羟基,可与硅酸酯键产生交联作用,当其粒径越小时,相同重量下数量越多,可结合的硅酸酯键也越多,与锌粉和铝粉与硅酸酯键的离子化反应产生竞争,导致锌粉和铝粉在涂层中的相容性降低,反而降低了涂层的长期耐腐蚀和附着性。
进一步地,所述硅烷偶联剂选自包括但不限于γ-烯丙基三甲氧基硅烷、γ-烯丙基三乙氧基硅烷、γ-丙烯基三丙氧基硅烷、γ-巯丙基三甲氧基硅烷、γ-硫氰基丙基三乙氧基硅烷、乙烯基三叔丁基过氧硅烷、双(三乙氧基硅基丙基)二硫化物、双(三乙氧基硅基丙基)四硫化物、3-氨丙基三乙氧基硅烷、N-正丁基-3-氨丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷中的至少一种。
进一步地,所述硅烷偶联剂选自γ-巯丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷中的至少一种或几种的组合。
在一种优选的实施方式中,所述硅烷偶联剂为γ-巯丙基三甲氧基硅烷和γ-缩水甘油醚氧丙基三甲氧基硅烷的组合,质量比为(1-2):1。
进一步地,所述钝化剂选自钼酸盐、磷钼酸盐、硝酸铈、硼酸盐、草酸氧钒、氟硅酸铵、氟钛酸铵、二硅化钼、苯丙三唑、膦酸中的任意一种或几种的组合。
优选地,所述钝化剂为钼酸盐、硝酸铈、氟硅酸铵、氟钛酸铵中的任意一种或几种的组合。
在一种优选的实施方式中,所述钝化剂为钼酸盐和硝酸铈,质量比为(1.5-4.5):1。
进一步地,所述润湿流平剂为非离子型表面活性剂,选自聚氧乙烯醚类或多元醇类中的任意一种或多种的组合。
进一步地,所述润湿流平剂为聚氧乙烯醚类,包括但不限于直链脂肪醇聚氧乙烯醚(AEO-7、AEO-9、AEO-10)、异构脂肪醇聚氧乙烯醚(E-1005、E-1007、E-1008、E-1009)、烷基酚聚氧乙烯醚(OP-10、OP-15、OP-20、NP-4、NP-10、NP-4P、NP-7P、BY-125、BY-140)中的至少一种。
进一步地,所述多元醇类选自甘油、季戊四醇、山梨醇、聚乙二醇中的至少一种。
在一种优选的实施方式中,所述润湿流平剂为AEO-9、OP-10、OP-15中的至少一种。
进一步地,所述消泡剂为有机硅类、矿物油类和聚醚类中的至少一种。
优选地,所述消泡剂为聚醚类消泡剂和/或有机硅类消泡剂,选自包括但不限于GPE-10、GPE-20、GPE-30、GPE-40、W-0505、W-0506、TEGO-901W、byk-094、byk-022中的任意一种或几种的组合。
在一种优选的实施方式中,所述消泡剂为byk-094。
进一步地,所述涂层的原料还包括具有可配位活性位点和杂原子的C5-C18酸酯类物质,用量占原料总量的5-10%。
进一步地,所述具有可配位活性位点和杂原子的C5-C18酸酯类物质为硼酸酯、铝酸酯、酞酸酯、锆酸酯类物质中的任意一种或几种的组合。
进一步地,所述具有可配位活性位点和杂原子的C5-C18酸酯类物质选自三乙醇胺硼酸酯、三乙醇胺铝酸酯、5-氟-2-(4,4,5,5-四甲基-1,3,2-二氧杂硼杂环戊烷-2-基)乙酸苄酯、丙基二油酸酰氧基(二辛基磷酸酰氧基)钛酸酯、异丙基三(二辛基磷酸酰氧基)钛酸酯、四(三乙醇胺)锆酸酯中的至少一种。本申请意外发现:通过添加一定量的具有可配位活性位点和杂原子的C5-C18酸酯类物质,可有效改善涂层的抗冲击性能和耐腐蚀性;本申请人分析原因为其结构中的配位活性位点可与涂层中的锌、铝及其离子形成配位作用,对锌、铝及其离子起到一定的包裹和固定作用,进一步增加锌、铝在有机涂层中的润湿分散性和稳定性,所形成的涂膜体系更加均匀并致密,涂层的抗冲击性能和防腐效果也更好,另外限定此酸酯物质含有杂原子是为了提高酸酯键的耐水解性,更好地保证涂层体系的稳定性。
在一种优选的实施方式中,所述具有可配位活性位点和杂原子的C5-C18酸酯类物质为三乙醇胺硼酸酯,用量占原料总量的5-8%;三乙醇胺硼酸酯由于其特殊笼状分子结构,其结构中心电子云密度高,与金属的配位作用更强,并且且笼状结构对锌、铝及其离子的包裹性更强,但是其表面张力较大,因此在体系中的用量不能太多。
进一步地,所述溶剂为高沸点溶剂,选自丙三醇、丙二醇、乙二醇、乙二醇单丁醚、乙酸辛酯一种或几种组合。
进一步地,所述涂层的涂料的制备方法为:
S1、将金属粉和氧化铝加入硅烷偶联剂和部分溶剂中,搅拌20-40min;
S2、将除具有可配位活性位点和杂原子的C5-C18酸酯类物质外的剩余原料加入,搅拌分散;
S3、将具有可配位活性位点和杂原子的C5-C18酸酯类物质加入其中,充分搅拌分散即可。
其次,本申请还提供了一种所述无铬防腐涂层的制备方法,包括以下步骤:
(1)对金属基底除油、除锈、喷砂;
(2)通过喷涂或浸涂将底层涂料涂覆于金属基底,烘干;
(3)通过喷涂或浸涂将无铬防腐涂层涂覆于底层涂料的表面;梯度烘干并烧结。
进一步地,所述步骤(1)中,喷砂粒径为20-40目。
进一步地,所述步骤(2)中,底层涂料的组分包括:按总质量计,硅烷类物质1-5%,水补足余量。
进一步地,所述硅烷类物质为巯丙基三甲氧基硅烷和3-氨丙基三乙氧基硅烷,质量比为(0.5-3):1。
进一步地,所述底层涂料的干膜厚度为0.05-0.2μm。
进一步地,所述步骤(3)中,无铬防腐涂层喷涂1-3次,每喷涂一次后均进行梯度烘干和烧结,每次喷涂的干膜厚度为2-3μm。
进一步地,所述梯度烘干为130-140℃烘干10-15min,再于160-180℃烘干5-7min;烧结温度为340-360℃,烧结时间为25-30min。
进一步的,所述无铬防腐涂层用于汽车紧固件的表面防护,所述紧固件为平面型或螺纹型的任一种。
有益效果
1、本申请中使用锌粉和铝粉作为阴极防护物质,使用球形氧化铝进一步优化两者形成的片层重叠结构,并对涂层进行增强,利用硅烷类物质的烷基化反应和偶联成膜性,稳定涂层体系中的固态物质,并增强涂层的结构强度,使用钝化剂在涂层表面形成钝化层阻止涂层的表面氧化反应,同时利用润湿流平剂、消泡剂、溶剂等原料组分的共同作用使涂层具有优异的性能;
2、本申请中具有可配位活性位点和杂原子的C5-C18酸酯类物质在体系中会与金属粉产生配位,对金属粉及其金属离子产生固定和包裹作用,增加了固态金属粉在有机体系中的分散性和相容性,并且该物质水解后的产物带有一定的羟基,可与金属表面或氧化铝表面的羟基或羧基产生缩合反应,进一步提高涂料的稳定性和涂层的致密性及耐腐蚀性能;
3、本申请优化了涂层的制备体系,通过涂覆底层增强防腐涂层对金属基底的附着力,可匹配螺纹等异形结构的紧固件的要求,另外优化涂层的烘干温度,使涂层具有更优异的致密性。
具体实施方式
实施例
实施例1
本实施例提供了一种用于汽车紧固件的无铬防腐涂层;按总质量计,所述涂层的原料包括:片状锌粉20%、片状铝粉3%、氧化铝0.7%、三乙醇胺硼酸酯6%、溶剂10%、硅烷偶联剂15%、钝化剂0.004%、硼酸2%、润湿流平剂0.6%、消泡剂0.4%、水补足余量为100%;
所述片状锌粉的最大片层直径为14μm,片层厚度为0.5μm,所述片状铝粉的最大片层直径为6μm,片层厚度为0.2μm;所述氧化铝粉为球形结构,粒径为1μm;所述硅烷偶联剂为γ-巯丙基三甲氧基硅烷和γ-缩水甘油醚氧丙基三甲氧基硅烷的组合,质量比为1.6:1;所述钝化剂为钼酸盐和硝酸铈,质量比为2:1;所述润湿流平剂为AEO-9和OP-10,质量比为1:1;消泡剂为byk-094;所述溶剂为乙二醇和乙酸辛酯,质量比为1:1。
涂层涂料的制备方法为:
S1、将片状锌粉、片状铝粉和氧化铝加入硅烷偶联剂和部分溶剂(占总溶剂体积的1/3)中,搅拌30min;
S2、将钝化剂、硼酸、润湿流平剂、消泡剂、剩余的溶剂和水加入S1中,搅拌分散;
S3、再将三乙醇胺硼酸酯加入其中,充分搅拌分散即可。
实施例2
本实施例提供了一种用于汽车紧固件的无铬防腐涂层;按总质量计,所述涂层的原料包括:片状锌粉12%、片状铝粉5%、氧化铝0.3%、三乙醇胺硼酸酯8%、溶剂15%、硅烷偶联剂10%、钝化剂0.005%、硼酸3%、润湿流平剂0.5%、消泡剂0.2%、水补足余量为100%;
所述片状锌粉的最大片层直径为20μm,片层厚度为0.8μm,所述片状铝粉的最大片层直径为10μm,片层厚度为0.5μm;所述氧化铝粉为球形结构,粒径为5μm;所述硅烷偶联剂为γ-巯丙基三甲氧基硅烷和γ-缩水甘油醚氧丙基三甲氧基硅烷的组合,质量比为1:1;所述钝化剂为钼酸盐和硝酸铈,质量比为4.5:1;所述润湿流平剂为AEO-9和OP-10,质量比为1.5:1;消泡剂为byk-094;所述溶剂为乙二醇和乙酸辛酯,质量比为2:1。
涂层涂料的制备方法同实施例1。
实施例3
本实施例提供了一种用于汽车紧固件的无铬防腐涂层;按总质量计,所述涂层的原料包括:片状锌粉30%、片状铝粉2%、氧化铝1.2%、三乙醇胺硼酸酯5%、溶剂5%、硅烷偶联剂20%、钝化剂0.002%、植酸1-3%、润湿流平剂0.8%、消泡剂0.5%、水补足余量为100%;
所述片状锌粉的最大片层直径为5μm,片层厚度为0.2μm,所述片状铝粉的最大片层直径为0.8μm,片层厚度为0.1μm;所述氧化铝粉为球形结构,粒径为0.3μm;所述硅烷偶联剂为γ-巯丙基三甲氧基硅烷和γ-缩水甘油醚氧丙基三甲氧基硅烷的组合,质量比为2:1;所述钝化剂为钼酸盐和硝酸铈,质量比为1.5:1;所述润湿流平剂为AEO-9和OP-10,质量比为1:1;消泡剂为byk-094;所述溶剂为乙二醇和乙酸辛酯,质量比为3:1。
涂层涂料的制备方法同实施例1。
实施例4
本实施例提供了一种所述无铬防腐涂层的制备方法,包括以下步骤:
(1)对金属基底除油、除锈、喷砂,喷砂粒径为40目;
(2)通过浸涂将底层涂料涂覆于金属基底,烘干;
所述底层涂料的组分包括:按总质量计,巯丙基三甲氧基硅烷1.5%、3-氨丙基三乙氧基硅烷3%,水余量;干膜厚度为0.1μm。
(3)通过喷涂将实施例1的无铬防腐涂层涂覆于底层涂料的表面;梯度烘干并烧结。
所述无铬防腐涂层喷涂2次,每次喷涂的干膜厚度为3μm;每喷涂一次后均进行梯度烘干和烧结,梯度烘干为130℃烘干15min,再于160℃烘干7min;烧结温度为350℃,烧结时间为30min。
实施例5
本实施例提供了一种所述无铬防腐涂层的制备方法,包括以下步骤:
(1)对金属基底除油、除锈、喷砂,喷砂粒径为20目;
(2)通过浸涂将底层涂料涂覆于金属基底,烘干;
所述底层涂料的组分包括:按总质量计,巯丙基三甲氧基硅烷2.5%、3-氨丙基三乙氧基硅烷2.5%、水余量,干膜厚度为0.2μm。
(3)通过喷涂将实施例1的无铬防腐涂层涂覆于底层涂料的表面;梯度烘干并烧结。
所述无铬防腐涂层喷涂3次,每次喷涂的干膜厚度为2μm;每喷涂一次后均进行梯度烘干和烧结,梯度烘干为140℃烘干10min,再于180℃烘干5min;烧结温度为350℃,烧结时间为30min。
对比例1
与实施例1基本一致,区别在于:所述片状锌粉的最大片层直径为25μm,片层厚度为1.1μm。
对比例2
与实施例1基本一致,区别在于:所述氧化铝粉粒径为0.08μm。
对比例3
与实施例1基本一致,区别在于:所述硅烷偶联剂为γ-巯丙基三甲氧基硅烷和γ-氨丙基三乙氧基硅烷,质量比为1.6:1。
对比例4
与实施例1基本一致,区别在于:所述硅烷偶联剂为γ-巯丙基三甲氧基硅烷和γ-缩水甘油醚氧丙基三甲氧基硅烷的组合,质量比为1:2。
对比例5
与实施例1基本一致,区别在于:所述润湿流平剂为OP-10。
对比例6
与实施例1基本一致,区别在于:所述三乙醇胺硼酸酯为12%。
对比例7
与实施例1基本一致,区别在于:所述三乙醇胺硼酸酯为0。
对比例8
与实施例4基本一致,区别在于:基底经步骤(1)处理后,直接根据步骤(3)喷涂无铬防腐涂层。
对比例9
与实施例4基本一致,区别在于:所述底层涂料的组分包括:按总质量计,3-氨丙基三乙氧基硅烷5%,水为95%;干膜厚度为0.15μm。
所述锌粉购自上海宏瑞化工有限公司,所述铝粉购自山东银箭金属颜料有限公司,所述氧化铝粉购自上海巷田纳米材料有限公司;所述三乙醇胺硼酸酯购自郑州冠达化工产品有限公司。
性能测试方法:
1、涂层附着力:按GB/T 9286-1998色漆和清漆漆膜的划格试验标准进行测试;
2、硬度:按GB/T 6739-2006色漆和清漆:铅笔法测定漆膜硬度标准进行测试;
3、冲击性试验:按照GB/T 1732-93漆膜耐冲击测定法标准进行测试,重锤设置为40cm;
4、中性盐雾试验:按照T1771-9标准进行测试;
5、耐强腐蚀性:按照各实施例的技术方案,将各涂层涂敷于螺栓(型号:M12)表面并固化,之后浸于质量分数为18%的硝酸溶液(80℃)中,记录出现锈点的时长。
性能测试结果:
测试结果见表1。
表1
Claims (10)
1.一种用于汽车紧固件的无铬防腐涂层,其特征在于,所述涂层的原料包括:金属粉12-35%、氧化铝0.3-1.2%、溶剂5-15%、硅烷偶联剂10-20%、钝化剂0.001-0.005%、硼酸或植酸1-3%、润湿流平剂0.5-1%、消泡剂0.2-0.5%、水补足余量为100%。
2.根据权利要求1所述的无铬防腐涂层,其特征在于,所述金属粉为锌粉、铝粉或锌铝合金粉中的至少一种。
3.根据权利要求2所述的无铬防腐涂层,其特征在于,所述锌粉为片状结构,最大片层直径不大于20μm,片层厚度不大于0.8μm;所述铝粉为片状结构,最大片层直径为0.8-10μm,片层厚度为0.1-0.5μm。
4.根据权利要求1所述的无铬防腐涂层,其特征在于,所述硅烷偶联剂选自γ-巯丙基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷中的至少一种或几种的组合。
5.根据权利要求1所述的无铬防腐涂层,其特征在于,所述钝化剂为钼酸盐和硝酸铈。
6.根据权利要求1所述的无铬防腐涂层,其特征在于,所述涂层的原料还包括具有可配位活性位点和杂原子的C5-C18酸酯类物质,用量占原料总量的5-10%。
7.根据权利要求6所述的无铬防腐涂层,其特征在于,所述具有可配位活性位点和杂原子的C5-C18酸酯类物质选自三乙醇胺硼酸酯、三乙醇胺铝酸酯、5-氟-2-(4,4,5,5-四甲基-1,3,2-二氧杂硼杂环戊烷-2-基)乙酸苄酯、丙基二油酸酰氧基(二辛基磷酸酰氧基)钛酸酯、异丙基三(二辛基磷酸酰氧基)钛酸酯、四(三乙醇胺)锆酸酯中的至少一种。
8.根据权利要求1-7任一项所述的无铬防腐涂层的制备方法,其特征在于,包括以下步骤:
(1)对金属基底除油、除锈、喷砂;
(2)通过喷涂或浸涂将底层涂料涂覆于金属基底,烘干;
(3)通过喷涂或浸涂将无铬防腐涂层涂覆于底层涂料的表面;梯度烘干并烧结;
所述底层涂料的组分包括:按总质量计,硅烷类物质1-5%,水补足余量。
9.根据权利要求8所述的无铬防腐涂层的制备方法,其特征在于,所述无铬防腐涂层喷涂1-3次,每次喷涂的干膜厚度为2-3μm。
10.根据权利要求9所述的无铬防腐涂层的制备方法,其特征在于,所述梯度烘干为130-140℃烘干10-15min,再于160-180℃烘干5-7min。
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