CN111393683B - 一种改性阳离子微凝胶及其制备方法和应用 - Google Patents
一种改性阳离子微凝胶及其制备方法和应用 Download PDFInfo
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- CN111393683B CN111393683B CN202010312985.7A CN202010312985A CN111393683B CN 111393683 B CN111393683 B CN 111393683B CN 202010312985 A CN202010312985 A CN 202010312985A CN 111393683 B CN111393683 B CN 111393683B
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- diisocyanate
- modified cationic
- acid
- epoxy resin
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Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- 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
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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
- C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
- C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
本发明属于电泳涂料制备技术领域,公开了一种改性阳离子微凝胶,主要由环氧树脂、双酚A、有机溶剂、碱性催化剂、聚氨酯硫化物、酸、水和可水解环氧树脂等组分制成,其中,由于环氧主链中的硫盐和可水解环氧树脂中的叔胺的存在,使制得的微凝胶带有阳离子特性,从而微凝胶的水分散性得以提高;同时,改性阳离子微凝胶的主链引入了具有硫结构的聚氨酯硫化物,其在与配方中各组分进行交联固化时提高了改性阳离子微凝胶对基材的结合力和电泳涂料的锐边防腐性能。本发明还提供了一种电泳涂料,采用本发明的改性阳离子微凝胶经复配所得的电泳涂料具有良好的锐边防腐性能的同时也兼具优异的综合防腐性和外观流平性,应用前景广泛。
Description
技术领域
本发明属于电泳涂料制备技术领域,具体涉及一种改性阳离子微凝胶及其制备方法和应用。
背景技术
电泳涂料被广泛应用在以汽车车体和汽车部件为主要用途的领域中。特别以阴极电泳涂料为主的电泳涂装方式,自上世纪六十年代投人工业生产以来由于其涂膜性能优异、涂料利用率高及低VOC含量等优点,发展非常迅速。现今阴极电泳涂料以广泛运用于汽车车身、汽摩配件、家电、家具配件、五金机电、军工等行业与领域。
阴极电泳涂料在规定温度下进行烘烤使涂装在基材上的树脂进行交联固化。在这情况下,树脂由于随着温度的提高,玻璃化温度降低引起涂层粘度降低,流动性提高而使在工件的边缘部位的涂层变薄或者剥落。特别是带有锐边工件的边缘部位变薄或者剥落时,该边缘由于长期暴露于外界环境中而得不到涂层有效保护容易导致严重的被腐蚀。随着汽车销量逐年萎缩,顾客在购车时对品质提出高要求,汽车生产商也对汽车品质提出更高要求,尤其是对汽车车身及其边缘部位的耐防腐性要求越来越高。
近些年在电泳涂料中添加微凝胶树脂来提高工件锐边防腐性为电泳行业最常规、最有效的手段之一。现有技术中制备改性阳离子微凝胶的方法有环氧-胺类、丙烯酸类、硅氧烷类等,但存在如下缺陷:设计环氧扩链因需要足够大的分子量才能起到微凝胶效果,因此,生产过程中控制难度大、凝胶化风险大;电泳涂料因需达到锐边防腐要求,需添加大量的微凝胶,但同时锐边防腐性仍不够好;微凝胶水分散体的分散颗粒尺寸较大,水溶性差,导致电泳涂料的涂层粗糙度高,外观流平变差;电泳涂料添加微凝胶后普遍导致层间附着力以及与基材结合力变差,无法做到同时兼顾锐边防腐和综合防腐性能等弊病。
发明内容
本发明旨在至少解决现有技术中存在的技术问题之一。为此,本发明的目的在于提供一种改性阳离子微凝胶及其制备方法和应用,通过将聚氨酯硫化物交联至阳离子微凝胶的主链上,并将所得到的改性阳离子微凝胶应用在电泳涂料中,能够有效提高电泳涂料的锐边防腐性能及综合防腐性能。
为了克服上述技术问题,本发明采用的技术方案如下:
一种改性阳离子微凝胶,所述改性阳离子微凝胶按重量份计,主要由以下原料组分制得:环氧树脂10-50份、双酚A5-25份、有机溶剂15-35份、碱性催化剂0.01-0.1份、聚氨酯硫化物5-25份、酸6-20份、水11-55份、可水解环氧树脂10-30份。
作为上述方案的进一步改进,所述碱性催化剂选自胺类、咪唑类、咪唑啉类和磷类中的至少一种,具体包括三乙胺、N、N-二甲基苄胺、三乙醇胺、四甲基氯化铵、三苯基膦、三乙胺酸盐、二甲基咪唑、四甲基咪唑、溴化四乙基铵、N、N-二甲基乙醇胺等。优选为N、N-二甲基苄胺、二甲基咪唑和三苯基膦中的至少一种。
作为上述方案的进一步改进,所述酸选自二羟甲基丙酸、氨基磺酸和乙酸中的至少一种。具体选自甲酸、乙酸、乳酸、丙酸、丁酸、辛酸、戊酸、己酸、苯甲酸、二羟甲基丙酸、N-乙酰基甘氨酸、N-乙酰基-β-丙氨酸、硼酸、磷酸、盐酸、硫酸、丙烯酸、甲基丙烯酸、氨基磺酸、马来酸酐、丙二酸二异丙酯、2-磺基苯甲酸酐、甲烷磺酸、羟乙基磺酸等中的至少一种。优选为二羟甲基丙酸、氨基磺酸、乙酸中的至少一种。
作为上述方案的进一步改进,所述聚氨酯硫化物的结构式为:
其中,R1选自羟甲基、羟乙基、羟丙基或羟丁基中的其中一种,R2选自羟甲基、羟乙基、羟丙基、羟丁基、甲基、乙基或丙基中的其中一种,且R1和R2为不同的基团,R3为含多异氰酸酯组分,选自芳香族多异氰酸酯或脂肪族多异氰酸酯中的一种或两种,或为多异氰酸酯聚合物;R4为封闭剂,选自醇醚类、苯酚类、内酰胺类、活性亚甲基化合物、硫醇类、酸酰胺类、胺类、咪唑类、脲类、氨基甲酸酯类、亚胺类、肟类、亚硫酸盐类、羟肟酸酯类等中的一种。
作为上述方案的进一步改进,所述聚氨酯硫化物按重量份计,主要由以下原料组分制得:含多异氰酸酯组分174-250份、有机溶剂100-200份、封闭剂118-190份、羟基硫化合物106-138份、聚氨酯合成用碱性催化剂0.9-1.3份。
进一步,所述含多异氰酸酯组分为芳香族多异氰酸酯或脂肪族多异氰酸酯中的一种或两种,或为多异氰酸酯聚合物。具体包括甲苯二异氰酸酯(TDI)、TDI二聚物、二苯基甲烷二异氰酸酯(MDI)、苯二亚甲基二异氰酸酯(XDI)、萘二异氰酸酯(NDI)、甲基环已基二异氰酸酯(HTDI)、二环已基甲烷二异氰酸酯(HMDI)、聚二苯基甲烷二异氰酸酯(PMDI)、二苯基甲烷二异氰酸酯(CMDI)、异佛尔酮二异氰酸酯(IPDI)、IPDI三聚体、己二异氰酸酯(HDI)、HDI三聚体、HDI缩二脲、2,2,4-三甲基己烷二异氰酸酯(TMHDI)、对苯二异氰酸酯(PPDI)、二甲基联苯二异氰酸酯(TODI)、1,4-环己烷二异氰酸酯(CHDI)、四甲基间苯二亚甲基二异氰酸酯(TMXDI)、三甲基-1,6-六亚甲基二异氰酸酯(TMHDI)、环己烷二亚甲基二异氰酸酯(HXDI)、降冰片烷二异氰酸酯(NBDI)等中的至少一种。其中,优选为甲苯二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯(MDI)、异佛尔酮二异氰酸酯(IPDI)中的至少一种。
进一步,所述封闭剂选自醇醚类、苯酚类、内酰胺类、活性亚甲基化合物、硫醇类、酸酰胺类、胺类、咪唑类、脲类、氨基甲酸酯类、亚胺类、肟类、亚硫酸盐类、羟肟酸酯类等中的至少一种。具体包括如甲醇、乙醇、丙醇、异丙醇、丁醇、戊醇、己醇、异辛醇、庚醇、辛醇、壬醇、异壬醇、葵醇、月桂醇、硬脂醇、乙二醇甲醚、二乙二醇甲醚、乙二醇乙醚、二乙醇乙醚、丙二醇甲醚、乙二醇丁醚、二乙二醇丁醚、乙二醇己醚、二乙二醇己醚、乙二醇异辛醚、丙二醇甲醚、丙二醇苯醚、苄醇、环己醇、苯酚、甲酚、二甲酚、氯代苯酚、乙基酚、正丁胺、二丁胺、苯胺、丙酮肟、乙酮肟、甲乙酮肟、二乙基己醇、二甲基咪唑、己内酰胺、戊内酰胺、丁内酰胺、三羟甲基丙烷、丙二醇等中的至少一种。优选为异辛醇、二乙二醇丁醚、二乙二醇己醚中的至少一种。
作为上述方案的进一步改进,所述羟基硫化合物的结构式为:
R1-S-R2
其中,R1选自羟甲基、羟乙基、羟丙基或羟丁基中的其中一种,R2选自羟甲基、羟乙基、羟丙基、羟丁基、甲基、乙基或丙基中的其中一种,且R1和R2为不同的基团。
具体地,所述羟基硫化合物选自羟基乙硫醚、2-羟基乙基苯甲基硫醚、2-羟基乙基正丙基硫醚、2-羟基乙基异丙基硫醚、2-羟基乙基异丁基硫醚、2-羟基乙基正戊基硫醚、2-羟基乙基-4-硝基苯基硫醚、对乙烯基苄基2-羟基乙基硫醚、2-苄硫基乙醇、2(4-氯苄基硫代)乙烷、2-苯硫基乙醇、2-羟基乙基戊基硫化物、2-羟基乙基己基硫化物、硫代羟甲基乙醇、硫代羟乙基丙醇、硫代羟乙基丁醇、硫代羟乙基丁氧基丙醇等中的至少一种。优选为硫代羟甲基乙醇、硫代羟乙基丙醇、羟基乙硫醚中的至少一种。
进一步,所述聚氨酯合成用碱性催化剂选自辛酸亚铋/锡、二月桂酸二丁基铋/锡、三乙胺、三乙醇胺、四甲基氯化铵、N,N二甲基咪唑、三苯基磷中至少一种。
进一步,所述有机溶剂选自烃类、醇类、醇醚类、酮类或酯类中的至少一种。其中,烃类包括甲苯、二甲苯、三甲苯等;醇类包括:甲醇、乙醇、正丁醇、异丙醇、异辛醇、乙二醇、丙二醇等;醇醚类包括:乙二醇乙醚、二乙二醇乙醚、乙二醇丁醚、二乙二醇丁醚、乙二醇己醚、二乙二醇己醚、丙二醇甲醚、丙二醇苯醚、二乙二醇二丁醚等;酮类包括:丙酮、丁酮、甲基异丁基酮、环己酮、异氟尔酮、乙酰丙酮等;酯类包括:乙二醇乙基醚醋酸酯、乙二醇丁基醚醋酸酯等。优选为甲基异丁基酮、乙二醇丁醚或二甲苯中的至少一种;
进一步,所述聚氨酯硫化物的制备方法为:
(1)称取原料,将174-250份含多异氰酸酯组分和50-100份有机溶剂混合,在惰性气体保护下,升温至40℃-100℃,加入封闭剂,保温反应1-2h,得到混合物1,冷却至室温;
(2)取羟基硫化合物、碱性催化剂与有机溶剂混合均匀,得到混合物2;
(3)将混合物2加入混合物1中,在40-80℃下保温反应1-2h,得所述聚氨酯硫化物。
进一步,所述可水解环氧树脂按重量份计由以下组分制得:缩水甘油酯环氧树脂100-300份、有机溶剂50-200份、胺类化合物300-500份。
其中,可水解环氧树脂原料配方中的所述缩水甘油酯环氧树脂化合物选自正丁基缩水甘油醚(BGE)、烯丙基缩水甘油醚(AGE)、5-乙基己基缩水甘油醚(EHAGE)、苯乙烯氧化物(SO)、苯基缩水甘油醚(PGE)、(邻)甲酚缩水甘油醚(CGE)、壬基酚缩水甘油醚、对叔丁基苯酚缩水甘油醚、对异丁基苯基缩水甘油醚(BPGE)、甲基丙烯酸缩水甘油酯(GMA)、三级羧酸缩水甘油酯、C8-C10-缩水甘油醚、C12-C14-缩水甘油醚中的至少一种。优选为甲基丙烯酸缩水甘油酯(GMA)和/或对叔丁基苯酚缩水甘油醚。
可水解环氧树脂原料配方中的所述有机溶剂选自烃类、醇类、醇醚类、酮类或酯类中的至少一种。其中,烃类包括甲苯、二甲苯、三甲苯等;醇类包括:甲醇、乙醇、正丁醇、异丙醇、异辛醇、乙二醇、丙二醇等;醇醚类包括:乙二醇乙醚、二乙二醇乙醚、乙二醇丁醚、二乙二醇丁醚、乙二醇己醚、二乙二醇己醚、丙二醇甲醚、丙二醇苯醚、二乙二醇二丁醚等;酮类包括:丙酮、丁酮、甲基异丁基酮、环己酮、异氟尔酮、乙酰丙酮等;酯类包括:乙二醇乙基醚醋酸酯、乙二醇丁基醚醋酸酯等。优选为甲基异丁基酮、乙二醇丁醚或二甲苯中的至少一种。
可水解环氧树脂原料配方中的所述胺类化合物选自丁胺、辛胺、二乙胺、二丁胺、甲基丁胺、乙醇胺、乙二醇胺、二乙醇胺、二丁醇胺、N甲基乙醇胺、三乙胺酸盐、氨基乙基乙醇胺的酮亚胺、二乙烯三胺丙酮亚胺、二乙烯三胺丁酮亚胺、二乙烯三胺甲基异丙基酮亚胺、二乙烯三胺甲基异丁基酮亚胺中的至少一种。优选为至少含有氨基乙基乙醇胺的酮亚胺和/或二乙烯三胺甲基异丁基酮亚胺。
进一步,所述可水解环氧树脂的制备方法为:将缩水甘油酯环氧树脂、有机溶剂混合均匀,得到混合物;在惰性气体保护下,将混合物升温至50-100℃,加入胺类化合物,升温至100-150℃,保温2h后,每隔1h取样测试物料的粘度,直至粘度不发生变化时即到终点,即得所述可水解环氧树脂。
一种如上任一项所述的改性阳离子微凝胶的制备方法,包括如下步骤:
(1)称取原料组分,将10-50份环氧树脂、5-25份双酚A和10-25份有机溶剂进行混合;
(2)在惰性气氛中,升温至90-110℃,搅拌;
(3)加入0.01-0.1份碱性催化剂,升温至120-170℃保温,进行环氧扩链反应,直至环氧当量为900-1200g/mol;
(4)在80-100℃条件下加入5-25份聚氨酯硫化物和5-10份有机溶剂,搅拌,加入1-5份水和5-15份酸,保温2h后,每隔1h取样测试物料的粘度,直至粘度不再发生变化;
(5)加10-50份水,搅拌,加入10-30份可水解环氧树脂,在80-100℃下保温反应4-10h,再加入1-5份酸进行中和,出料,得所述改性阳离子微凝胶。
一种由如上任一项所述的改性阳离子微凝胶制备的电泳涂料,所述电泳涂料按重量份计,主要由以下原料组分制得:色浆50-100份、乳液300-600份、改性阳离子微凝胶1.5-120份、水300-700份。其中,所述色浆为KD-663色浆,所述乳液为D-663乳液,均来源于广东科德环保科技股份有限公司。
作为上述方案的进一步改进,所述电泳涂料的固体含量为10-25%,灰分为10-25%,pH为5.0-6.5。
作为上述方案的进一步改进,所述电泳涂料的电导率为800-2000μs/cm,MEQA值为25-40(MEQA是指在电泳涂装中,对含100g固体份的涂料进行滴定所需的酸的毫摩尔数,单位为mmol)。
所述的电泳涂料的制备方法为:按电泳涂料的原料配方,向水中边搅拌边加入乳液,再搅拌条件下加入色浆,最后再加入改性阳离子微凝胶,在30±2℃下,敞口搅拌熟化24h以上,制得的电泳涂料的外观均匀平整光滑,厚度在10-40μm内可调。电泳电压80-300V,电泳温度为25-35℃,电泳时间为3min(30秒软启动);在150-180℃下进行烘烤,烘烤时间为20-40分钟。
本发明的有益效果是:
(1)本发明提出了一种改性阳离子微凝胶及其制备方法,该改性阳离子微凝胶主要由环氧树脂、双酚A、有机溶剂、碱性催化剂、聚氨酯硫化物、酸、水和可水解环氧树脂等组分制成,其中,由于环氧主链中的硫盐和可水解环氧树脂中的叔胺的存在,使制得的微凝胶带有阳离子特性,从而微凝胶的水分散性得以提高;同时,改性阳离子微凝胶的主链引入了具有硫结构的聚氨酯硫化物,其在与配方中各组分进行交联固化时提高了改性阳离子微凝胶对基材的结合力和电泳涂料的锐边防腐性能。
(2)本发明还提供了一种电泳涂料,通过合成聚氨酯硫化物并将其交联至阳离子微凝胶的主链上,再将所得改性阳离子微凝胶应用在电泳涂料中,能够有效提高电泳涂料的锐边防腐性能、综合防腐性能和外观流平性,同时,与传统的硫盐分散树脂相比较,改性阳离子微凝胶对基材的结合力、所得的电泳涂料的锐边防腐性能及综合防腐性能均得到明显的提高,含有软性结构的聚氨酯使得电泳涂料涂膜的外观与光泽度得以有效提高,因而,使得电泳涂料具有良好的锐边防腐性能的同时也兼具优异的综合防腐性和外观流平性。
具体实施方式
下面结合实施例对本发明进行具体描述,以便于所属技术领域的人员对本发明的理解。有必要在此特别指出的是,实施例只是用于对本发明做进一步说明,不能理解为对本发明保护范围的限制,所属领域技术熟练人员,根据上述发明内容对本发明所作出的非本质性的改进和调整,应仍属于本发明的保护范围。同时,下述所提及的原料未详细说明的,均为市售产品;未详细提及的工艺步骤或提取方法为均为本领域技术人员所知晓的工艺步骤或提取方法。
实施例1
称取原料组分,将10份环氧树脂、5份双酚A和10份甲基异丁基酮进行混合;在惰性气氛中,升温至90℃,搅拌;加入0.01份N、N-二甲基苄胺,升温至120℃保温,进行环氧扩链反应,直至环氧当量为900-1200g/mol;降温至80℃,加入5份聚氨酯硫化物和5份甲基异丁基酮,搅拌,加入1份去离子水和5份二羟甲基丙酸,保温2h后,每隔1h取样测试物料的粘度,直至粘度不再发生变化;加10份去离子水,搅拌,加入10份可水解环氧树脂,在80℃下保温反应4-10h,再加入1-5份乙酸进行中和,出料,得改性阳离子微凝胶1。
实施例2
称取原料组分,将50份环氧树脂、25份双酚A和25份甲基异丁基酮进行混合;在惰性气氛中,升温至110℃,搅拌;加入0.1份N、N-二甲基苄胺,升温至170℃保温,进行环氧扩链反应,直至环氧当量为900-1200g/mol;降温至100℃,加入25份聚氨酯硫化物和10份甲基异丁基酮,搅拌,加入5份去离子水和15份二羟甲基丙酸,保温2h后,每隔1h取样测试物料的粘度,直至粘度不再发生变化;加50份去离子水,搅拌,加入30份可水解环氧树脂,升温至100℃,保温反应10h,再加入5份乙酸进行中和,出料,得改性阳离子微凝胶2。
实施例3
称取原料组分,将30份环氧树脂、15份双酚A和18份甲基异丁基酮进行混合;在惰性气氛中,升温至100℃,搅拌;加入0.05份N、N-二甲基苄胺,升温至140℃保温,进行环氧扩链反应,直至环氧当量为900-1200g/mol;降温至90℃,加入10份聚氨酯硫化物和8份甲基异丁基酮,搅拌,加入3份水和10份二羟甲基丙酸,保温2h后,每隔1h取样测试物料的粘度,直至粘度不再发生变化;加30份水,搅拌,加入20份可水解环氧树脂,在90℃下保温反应7h,再加入3份乙酸进行中和,出料,得改性阳离子微凝胶3。
实施例4
称取原料组分,将电泳涂料的原料配方,向300份去水中边搅拌边加入300份乳液,再搅拌条件下加入50份色浆,最后再加入2份改性阳离子微凝胶,在28℃下,敞口搅拌熟化24h以上,得电泳涂料工作液1。其中,色浆为KD-663色浆,乳液为D-663乳液,均购于广东科德环保科技股份有限公司。
实施例5
称取原料组分,将电泳涂料的原料配方,向500份去水中边搅拌边加入450份乳液,再搅拌条件下加入75份色浆,最后再加入50份改性阳离子微凝胶,在32℃下,敞口搅拌熟化24h以上,得电泳涂料工作液2。其中,色浆为KD-663色浆,乳液为D-663乳液,均购于广东科德环保科技股份有限公司。
实施例6
称取原料组分,将电泳涂料的原料配方,向700份去水中边搅拌边加入600份乳液,再搅拌条件下加入100份色浆,最后再加入100份改性阳离子微凝胶,在30℃下,敞口搅拌熟化24h以上,得电泳涂料工作液3。其中,色浆为KD-663色浆,乳液为D-663乳液,均购于广东科德环保科技股份有限公司。
对比例1
与实施例6的区别在于,对比例1未添加本发明的改性阳离子微凝胶,得到电泳涂料工作液,记为对比例成品1。
实施例7
经检测,上述实施例4-6所得电泳涂料工作液1-3和对比例工作液1,从外观、膜厚、光泽、附着力性、柔韧性、耐水性(40℃,h)、耐冲、耐盐雾性(h,单侧腐蚀≤2mm)、刀片锐边防腐锈点数(300h)耐碱性、耐酸性等进行涂膜性能评价,得到如下表1。其中,涂膜性能评价过程中的电泳涂装按照以下标准进行打板测试:槽温30±2℃,按常规方法在250±50V下通电电泳至膜厚20±2μm。电泳结束后洗净,再在160℃下烘烤20min,然后进行涂膜性能测试。
表1 电泳涂料工作液1-3和对比例成品1的涂膜性能评价
从表1可以看出,实施例4-6所得电泳涂料工作液1-3随着改性阳离子微凝胶的添加量增大,锐边防腐效果得到明显的改善,同时电泳涂层的整体防腐性影响较少;随着改性阳离子微凝胶的增加,涂膜外观流平没发生橘皮等影响流平外观的问题。此外,未添加改性阳离子微凝胶的对比例成品1的刀片锐边防腐锈点数为55,明显高于实施例4-6所得电泳涂料工作液1-3的刀片锐边防腐锈点数。
对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下还可以做出若干简单推演或替换,而不必经过创造性的劳动。因此,本领域技术人员根据本发明的揭示,对本发明做出的简单改进都应该在本发明的保护范围之内。上述实施例为本发明的优选为实施例,凡与本发明类似的工艺及所作的等效变化,均应属于本发明的保护范畴。
Claims (7)
1.一种改性阳离子微凝胶,其特征在于,所述改性阳离子微凝胶按重量份计,由以下原料组分制得:环氧树脂10-50份、双酚A 5-25份、有机溶剂15-35份、碱性催化剂0.01-0.1份、聚氨酯硫化物5-25份、酸6-20份、水11-55份、可水解环氧树脂10-30份;所述可水解环氧树脂按重量份计由以下组分制得:缩水甘油酯环氧树脂100-300份、有机溶剂50-200份、胺类化合物300-500份;
所述聚氨酯硫化物的结构式为:
其中,R1’选自甲基、乙基、丙基或丁基中的其中一种,R3为含多异氰酸酯组分反应后的残基;R4为封闭剂反应后的残基;
所述聚氨酯硫化物按重量份计,由以下原料组分制得:含多异氰酸酯组分174-250份、有机溶剂100-200份、封闭剂118-190份、羟基硫化合物106-138份、聚氨酯合成用碱性催化剂0.9-1.3份;
所述聚氨酯硫化物的制备方法为:
(1)称取原料,将174-250份含多异氰酸酯组分和50-100份有机溶剂混合,在惰性气体保护下,升温至40℃-100℃,加入封闭剂,保温反应1-2h,得到混合物1,冷却至室温;
(2)取羟基硫化合物、碱性催化剂与有机溶剂混合均匀,得到混合物2;
(3)将混合物2加入混合物1中,在40-80℃下保温反应1-2h,得所述聚氨酯硫化物;
所述羟基硫化合物的结构式为:R1-S-R2;其中,R1选自羟甲基、羟乙基、羟丙基或羟丁基中的其中一种,R2选自羟甲基、羟乙基、羟丙基、羟丁基、甲基、乙基或丙基中的其中一种,且R1和R2为不同的基团;
所述含多异氰酸酯组分包括甲苯二异氰酸酯、TDI二聚物、二苯基甲烷二异氰酸酯、苯二亚甲基二异氰酸酯、萘二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯、聚二苯基甲烷二异氰酸酯、二苯基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、IPDI三聚体、己二异氰酸酯、HDI三聚体、HDI缩二脲、2,2,4-三甲基己烷二异氰酸酯、对苯二异氰酸酯、二甲基联苯二异氰酸酯、1,4-环己烷二异氰酸酯、四甲基间苯二亚甲基二异氰酸酯、三甲基-1,6-六亚甲基二异氰酸酯、环己烷二亚甲基二异氰酸酯、降冰片烷二异氰酸酯中的至少一种;
所述封闭剂包括如甲醇、乙醇、丙醇、异丙醇、丁醇、戊醇、己醇、异辛醇、庚醇、辛醇、壬醇、异壬醇、葵醇、月桂醇、硬脂醇、乙二醇甲醚、二乙二醇甲醚、乙二醇乙醚、二乙醇乙醚、丙二醇甲醚、乙二醇丁醚、二乙二醇丁醚、乙二醇己醚、二乙二醇己醚、乙二醇异辛醚、丙二醇甲醚、丙二醇苯醚、苄醇、环己醇、苯酚、甲酚、二甲酚、氯代苯酚、乙基酚、正丁胺、二丁胺、苯胺、丙酮肟、乙酮肟、甲乙酮肟、二乙基己醇、二甲基咪唑、己内酰胺、戊内酰胺、丁内酰胺、三羟甲基丙烷、丙二醇中的至少一种;
所述改性阳离子微凝胶的制备方法,其特征在于,包括如下步骤:
(1)称取原料组分,将10-50份环氧树脂、5-25份双酚A和10-25份有机溶剂进行混合;
(2)在惰性气氛中,升温至90-110℃,搅拌;
(3)加入0.01-0.1份碱性催化剂,升温至120-170℃保温,进行环氧扩链反应,直至环氧当量为900-1200g/mol;
(4)在80-100℃条件下加入5-25份聚氨酯硫化物和5-10份有机溶剂,搅拌,加入1-5份水和5-15份酸,保温2h后,每隔1h取样测试物料的粘度,直至粘度不再发生变化;
(5)加10-50份水,搅拌,加入10-30份可水解环氧树脂,在80-100℃下保温反应4-10h,再加入1-5份酸进行中和,出料,得所述改性阳离子微凝胶。
2.根据权利要求1所述的改性阳离子微凝胶,其特征在于,所述碱性催化剂选自胺类、咪唑类、咪唑啉类和磷类中的至少一种。
3.根据权利要求1所述的改性阳离子微凝胶,其特征在于,所述酸选自二羟甲基丙酸、氨基磺酸和乙酸中的至少一种。
4.一种如权利要求1-3任一项所述的改性阳离子微凝胶的制备方法,其特征在于,包括如下步骤:
(1)称取原料组分,将10-50份环氧树脂、5-25份双酚A和10-25份有机溶剂进行混合;
(2)在惰性气氛中,升温至90-110℃,搅拌;
(3)加入0.01-0.1份碱性催化剂,升温至120-170℃保温,进行环氧扩链反应,直至环氧当量为900-1200g/mol;
(4)在80-100℃条件下加入5-25份聚氨酯硫化物和5-10份有机溶剂,搅拌,加入1-5份水和5-15份酸,保温2h后,每隔1h取样测试物料的粘度,直至粘度不再发生变化;
(5)加10-50份水,搅拌,加入10-30份可水解环氧树脂,在80-100℃下保温反应4-10h,再加入1-5份酸进行中和,出料,得所述改性阳离子微凝胶。
5.一种电泳涂料,其特征在于,按重量份计由以下原料组分制得:色浆50-100份、乳液300-600份、权利要求1-3任一项所述的改性阳离子微凝胶1.5-120份、水300-700份。
6.根据权利要求5所述的电泳涂料,其特征在于,所述电泳涂料的固体含量为10-25%,灰分为10-25%,pH为5.0-6.5。
7.根据权利要求5所述的电泳涂料,其特征在于,所述电泳涂料的电导率为800-2000μs/cm,MEQA值为25-40。
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Denomination of invention: A modified cationic micro gel and its preparation method and application Granted publication date: 20230523 Pledgee: Industrial and Commercial Bank of China Limited Foshan Ronggui Sub branch Pledgor: GUANGDONG KODEST ECO-TECHNOLOGY INC. CO.,LTD. Registration number: Y2024980001773 |