CN1053638A - 具有优良润滑性的金属表面处理组合物 - Google Patents
具有优良润滑性的金属表面处理组合物 Download PDFInfo
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- CN1053638A CN1053638A CN91100513A CN91100513A CN1053638A CN 1053638 A CN1053638 A CN 1053638A CN 91100513 A CN91100513 A CN 91100513A CN 91100513 A CN91100513 A CN 91100513A CN 1053638 A CN1053638 A CN 1053638A
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- acid
- monomer
- valency chromium
- lubricant
- methyl
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Abstract
一种润滑性优良的金属表面处理组合物,它含有
作为无机化合物的6价铬离子或6价铬离子和3价
铬离子,以及作为有机化合物的丙烯酸系聚合物乳
胶,作为润滑成分的用非离子系乳化剂分散的1种或
2种以上润滑剂分散物1重量%-50重量%(固体含
量比);pH为5以下,且在含铬酸盐水系树脂液中配
合润滑剂分散物。形成的保护膜具有优良的润滑性,
耐蚀性,涂覆性。
Description
本发明涉及对金属表面同时进行铬酸盐处理及有机树脂涂覆处理的金属表面处理组合物,更详细地说,涉及润滑性优良的金属表面处理组合物。
本发明之金属表面处理组合物的一般用途,是钢铁、铝、锌、锡、铜及这些金属的合金,以及这些金属的镀材等原材在环状、板状、线状、棒状等状态下在表面形成处理皮膜,从而得到在制造金属材料时能使表面处理过的金属材料具有良好的润滑性,成形加工性,耐蚀性,覆膜粘合性,涂覆后耐腐蚀性及耐指纹附着性。
以前,在金属加工及金属涂覆领域,为了提高耐腐蚀性和涂料的粘合性,一般在机械加工后或涂覆前的金属原材上施以铬酸盐处理、磷酸盐处理等表面处理。近年来,为了精简机械加工或涂覆工序中的表面处理和降低成本,试图预先对上述金属原材进行表面处理以致形成皮膜,然后用压力机油涂覆后进行机械加工,从而得到制品。即,试图省略制品加工或最终处理阶段中称之为铬酸盐处理、磷酸盐处理的表面处理,有一部分制品目前就是用这种方法制得的。
原材阶段预先实施的表面处理,尤其引人注意的是含铬酸盐水系树脂的涂覆方式。而且,提出施以反应型铬酸盐处理后水洗,并涂覆以有机树脂为主成分的药剂的涂覆方法,以及将配合有铬酸盐药剂的水系树脂(以下称含铬酸盐水系树脂)进行涂覆的方法中代表性的含铬酸树脂系涂覆方法。特开昭58-224175号等公开了前者方法,特开昭63-145785号等公开了后者方法。这些方法的优点是可省略制品的铬酸盐处理以致省力化和降低成本。后者之特开昭63-145785号方法是本申请人的共同申请所涉及的方法,按照这种方法制得的表面处理材料其耐蚀性、涂膜粘合性、涂漆后的耐蚀性,耐指纹附着性优良,而且碱脱脂后,溶剂脱脂后的性能也很优良,因此广泛用于家电制造。
将这些方法制得的表面处理原材进行机械加工时,树脂膜层夹在金属原材和工具之间,因此,比作为以前表面处理材料的磷酸盐处理钢材及铬酸盐处理钢材,其成形加工性优良,但是还不够好。因此,在反应型铬酸盐处理后进行涂覆的方法,以及含铬酸盐水系树脂的涂覆方法都需要预先在表面处理过的原材上涂覆压力机油然后再进行成形加工。因此,还需要在脱脂工序中除去涂覆的压力机油,然后再送往涂漆工序等复杂工序。
本发明目的是为了省略压力机油涂覆及其后去除的复杂工序而研究出一种组合物,即在含铬酸盐水系树脂形成的膜上的赋予润滑性,并可以在不需要涂覆压力机油的状态下进行成形加工,省去加工后的脱脂工序,即使在以加工状态表面处理过的原材上进行涂覆也能形成具有优良涂膜粘合性的保护膜的金属表面处理组合物。
本发明者们重复进行研究,结果完成在含铬酸盐水系树脂中使用1种或两种以上的非离子系乳化剂,并以固体含量为1重量-50重量%配合分散的润滑剂以致具有良好的贮存稳定性,而且能形成润滑性及加工成形性均优良之保护膜的金属表面处理组合物。还判明该金属表面处理组合物能形成耐腐蚀性,对金属及上涂层涂膜的粘合性优良的保护膜。
即本发明提供一种润滑性优良的金属表面处理组合物,其特征在于,它含有作为无机化合物的6价铬离子或6价铬离子和3价铬离子,以及作为有机化合物的下述丙烯酸类聚合物乳胶,作为润滑成分的非离子系乳化剂分散的1种或2种以上润滑剂分散物1重量%-50重量%(固体含量),其pH为5以下,并在含铬酸盐水系树脂液中配合润滑剂分散物。
丙烯酸系聚合物乳胶是将以下三种物质,用基本上不含阴离子性乳化剂及阳离子乳化剂的,但含有聚氧乙烯-聚氧丙烯嵌段聚合物系的非离子性乳化剂乳化聚合而得到的丙烯酸系聚合物乳胶;
1)乙烯系不饱和羧酸单体,
2)从(甲)以下通式表示的烷氧基亚甲基(甲基)丙烯酰胺及其衍生物:
但是,X为CnH2n+1(n=0或1)
Y为CmH2m+1(m=0-4)
(乙)酸性磷氧烷基(甲基)丙烯酸酯(アシッドホスホオキシアルキル(メタ)アクリレ-ト)
(丙)烷氧基烷基(甲基)丙烯酸酯
中选择出来的1或2种以上单体
3)从丙烯酸系单体(至少一部分由上述2)的(丙)构成)中选择出来的1或2种以上单体构成的,并根据要求含有这些共聚合性单体的骨架用单体。
以下详细说明本发明。
本发明中用作有机化合物的丙烯酸系聚合物乳胶,是将上述1)、2)、3)之各组单体乳化聚合而得到的。
以下说明各组单体。
1)之乙烯系不饱和羧酸单体是指不饱和单体或二羧酸。乙烯系不饱和羧酸单体,主要是对金属能赋予粘合性的羧基的供给源。乙烯系不饱和羧酸单体,包括丙烯酸、甲基丙烯酸、巴豆酸、衣康酸、马来酸或富马酸等以及它们的半酯。
2)之(甲)的通式
但是,X为CnH2n+1(n=0或1),
Y为CmH2m+1(m=0-4)
表示的烷氧基亚甲基(甲基)丙烯酰胺及其衍生物,n=0时是烷氧基亚甲基丙烯酰胺,n=1时是烷氧基亚甲基甲基丙烯酰胺,m=0时是甲氧基亚甲基(甲基)丙烯酰胺,m=1时是乙氧基亚甲基(甲基)丙烯酰胺,m=2时是丙氧基亚甲基(甲基)丙烯酰胺,m=3时是丁氧基亚甲基(甲基)丙烯酰胺,m=4时是戊氧基亚甲基(甲基)丙烯酰胺。
2)之(乙)的酸性磷氧烷基(甲基)丙烯酸酯,包括酸性磷氧基甲基丙烯酸酯、酸性磷氧基乙基丙烯酸酯,酸性磷氧基丙基丙烯酸酯、酸性磷氧基甲基丙烯酸甲酯、酸性磷氧基甲基丙烯酸乙酯、酸性磷氧基甲基丙烯酸丙酯。
2)之(丙)烷氧基烷基(甲基)丙烯酸酯包括:甲氧基甲基丙烯酸酯、甲氧基乙基丙烯酸酯、甲氧基甲基丙烯酸甲酯、甲氧基甲基丙烯酸乙酯、乙氧基甲基丙烯酸酯、乙氧基乙基丙烯酸酯、乙氧基甲基丙烯酸甲酯、乙氧基甲基丙烯酸乙酯。
上述(甲)、(乙)、(丙)之单体,由于各自具有的N-取代羟甲基(CH2=C-CONH)、磷酸基、烷氧基,以致能提高本发明之组合物形成的金属表面处理保护膜和在其上涂饰的涂膜之间的粘合性。因此,如果使用(甲)、(乙)、(丙)中至少一组以上即可得到上述效果。
3)之丙烯酸系单体是构成保护膜骨架的物质,包括甲基丙烯酸酯、甲基丙烯酸甲酯、乙基丙烯酸酯、甲基丙烯酸乙酯、异丙基丙烯酸酯、甲基丙烯酸异丙酯,正丁基丙烯酸酯、甲基丙烯酸正丁酯、2-乙基己基丙烯酸酯、甲基丙烯酸2-乙基己酯、辛基丙烯酸酯、甲基丙烯酸辛酯、丙烯腈、甲基丙烯腈、丙烯酰胺、甲基丙烯酰胺等,还包括2)之(丙)的烷氧基烷基(甲基)丙烯酸酯。
1)及2)的(甲)(乙)能赋予涂膜的粘合性,但并不是骨架。
根据需要在3)中含有的,它们的共聚性单体包括苯乙烯、甲基苯乙烯、乙酸乙烯、α位分支的饱和羧酸的乙烯酯、氯乙烯、乙烯甲苯、乙烯等。
因此,在3)中有以下组合。
①、丙烯酸类单体(是与2)之(丙)的烷氧基烷基(甲基)丙烯酸酯不共同的另一种丙烯酸系单体)、
②、①+烷氧基烷基(甲基)丙烯酸酯(即一部分与2)之(丙)的烷氧基烷基(甲基)丙烯酸酯共同,残部不共同的丙烯酸系单体)
③、烷氧基烷基(甲基)丙烯酸酯(即,2)之(丙)和3)同种)
④、①+共聚合性单体
⑤、②+共聚合性单体
⑥、③+共聚合性单体
3)之单体,构成本发明中使用的丙烯酸系聚合体乳胶的骨架,是支配树脂的硬软、可挠性、强伸度、弹性、粘附性、玻璃转移温度,最低造膜温度等物性及化学稳定性等的单体。
然而,烷氧基烷基(甲基)丙烯酸酯是一种作为2)的单体具有提高粘合性的作用,同时也具有骨架单体作用的特异单体,因此,本发明构成是,烷氧基烷基(甲基)丙烯酸酯还具有包括2)和3)两方面的特殊构成。
因此,例如,作为1)、2)、3)之单体的组合之一,还有丙烯酸-烷氧基烷基(甲基)丙烯酸酯-苯乙烯的组合,而所得之丙烯酸系聚合物乳胶作为本发明用的有机化合物是十分有效的。各有机化合物对其用量没有特别的限制。
用于本发明的丙烯酸系聚合乳胶聚合时所使用的乳化剂是非离子性乳化剂,这种非离子性乳化剂包括聚氧乙烯烷基醚、聚氧乙烯烷基苯酚醚、聚氧乙烯烷基酯、山梨糖醇烷基酯、聚氧乙烯山梨糖醇烷基酯、聚氧乙烯-聚氧丙烯嵌段聚合物等。非离子性乳化剂中有效量的离子性乳化剂共存时,即使用聚氧乙烯-聚氧丙烯嵌段聚合物(EO-PO嵌段聚合物),生成的乳胶的铬酸混合稳定性显著下降,因此不希望并用离子性乳化剂。
聚合时所用的非离子性乳化剂,采用的是聚氧乙烯-聚氧丙烯嵌段聚合物(EP-PO嵌段聚合物),因此可得到与铬酸的混合稳定性显著优良的乳胶。非离子性乳化剂中EP-PO嵌段聚合物所占的比例最好在5重量%-100重量%范围内。如果EP-PO嵌段物占的比例多,被认为有增加粗大乳胶粒子生成的倾向,但是由于将最终所得之乳胶的温度设定在较低值,因此,即使单独使用EP-PO嵌段聚合物进行聚合,也能避免粗大的乳胶生成。如果EO-PO嵌段聚合物在非离子性乳化剂中所占比例不足5重量%,则与铬酸的混合性不充分。
在本发明中作为无机化合物使用的6价铬离子,以铬酸或铬酸盐化合物的形式提供给组合物。铬酸通常以无水铬酸或无水铬酸的水溶液形式,铬酸盐以铬酸或重铬酸的铵、钾、锶、钡、钠、锌等盐的形式供给。
6价铬离子是强氧化剂,可使钢铁、锌、铝等金属表面不活泼化,具有保护金属不被腐蚀的作用。而且,6价铬离子的一部分,在保护膜形成时的干燥工序中加热情况下,被丙烯酸聚合物乳胶中的乳化剂和树脂中的官能团还原,成为3价铬离子,起到6价铬的水难溶性化和树脂的高分子化的作用。
本发明中根据情况使用的含有3价铬的无机化合物的3价铬离子是在含6价铬离子的水溶液中添加甲醇、乙醇、草酸、淀粉、过氧化氢、焦棓粉等还原剂,通过6价铬离子的部分还原而生成的。或者,将碳酸铬、氢氧化铬溶解在铬酸水溶液中也可生成3价铬离子。6价铬(铬酸)具有防锈作用,但却具有易溶于水的性质,在金属表面形成覆膜后,保护膜与水接触时6价铬容易溶解而从保护膜中脱离出来,结果导致保护膜的防锈效果显著减弱,而且还会有6价铬导致的环境污染问题。3价铬与6价铬(铬酸)结合从而形成难溶于水的铬酸铬,由于抑制了6价铬从保护膜中溶出,因而能维持防锈效果和防止环境污染。
因此,采用硝酸铬、硫酸铬、氯化铬、铬明矾等中的阴离子残存在保护膜形成组成液中的化合物,保护膜形成时3价铬离子的一部分或大半,和这些阴离子结合形成可溶性的3价铬化合物,因此,作为难溶于水的铬酸铬的生成量减少,这是不希望的。
3价铬还和树脂中的官能团结合并使丙烯酸聚合物树脂交联以致带来其高分子化,其结果是提高了在金属上形成的保护膜的耐碱脱脂性。
丙烯酸系聚合物乳胶树脂和6价铬离子及3价铬离子的比例最好是树脂/全铬=200~0.2。该比例若超过200则耐碱性不充分,形成之保护膜碱脱脂后的耐蚀性以及与上涂层涂料之间的涂膜粘合性降低。该比例若不足0.2,则在形成的保护膜上丙烯酸系重合物乳胶树脂的效果不充分,得不到足够的耐水性,耐碱性、与上涂层涂料的涂膜粘合性。
6价铬离子和3价铬离子的比例,在不含磷酸等其它酸的情况下,从药剂稳定性来看,以Cr3+/Cr6+是1以下为好,而在含磷酸等酸的情况下,为了充分获得6价铬的的耐蚀性,Cr3+/Cr6+是5以下为好。
用于本发明的丙烯酸系聚合乳胶、铬酸以及润滑剂作为必要成分的组合物使用应在pH5以下,而且润滑剂分散物添加前的含铬酸盐水系树脂pH也应在5以下,如果pH超过5,则上涂层粘合性不良,而且本发明表面处理膜和基底金属之间的粘合性降低,因此该保护膜在深冲加工时产生剥离,润滑特性也不良。如果将本发明所示单体组成聚合而成的乳胶在未中和状态使用,其组合物的pH在5以下,但超过5时则可用铬酸或磷酸进行调节。
本发明中使用的润滑剂,在成形加工时具有降低摩擦阻抗作用。而且,由于润滑材料在成形加工时产生热而一部分熔解,具有防止成形物和金属模之间的烧熔作用。作为这种润滑剂可使用其本身为公知的物质。以下例示润滑剂。
烃滑剂类:例如天然石蜡、合成石蜡、微晶石蜡、聚乙烯石蜡、氯化烃、氟代烃等。
脂肪酸系滑剂:月桂酸、硬脂酸、棕榈酸、羟基脂肪酸等。
脂肪酰胺系滑剂:例如,硬脂酰胺、棕榈酰胺、甲基双硬脂酰胺、乙烯双硬脂酰胺、油酰胺、芥酸酰胺、亚烷基双脂肪酰胺。
酯系滑剂:例如,硬脂酸丁酯之类的脂肪酸的低级醇酯、硬化蓖麻油等这类脂肪酸的多价醇酯、单硬脂酸乙二醇酯之类的乙二醇酯或聚乙二醇酯、酯石蜡等。
醇系滑剂:例如,十六(烷)醇、硬脂醇、棕榈醇等。
金属碱类:例如,硬脂酸钾、硬脂酸铅、月桂酸钾、棕榈酸钾等。
金属硫化物类:二硫化钼、二硫化钨等。
含氟聚合物:聚四氟乙烯、聚三氟乙烯、聚偏二氟乙烯、聚氟乙烯等。
其它:石墨、氟化石墨、氮化硼等。
为了分散这些润滑剂,可以仅使用非离子系乳化剂。使用阳离子、阴离子及两性乳化剂时,分散的润滑剂在含铬酸盐水系树脂中的混合性差。作为非离子系乳化剂,可使用聚氧乙烯烷基醚、聚氧乙烯烷基苯酚醚、聚氧乙烯烷基酯、山梨糖醇烷基酯、聚氧乙烯山梨糖醇烷基酯、聚氧乙烯-聚氧丙烯嵌段聚合物,以及全氟烷氧基乙烯加成物等。乳化剂的使用量,相对于分散的润滑剂最好为1-20重量%。乳化剂的量相对于润滑剂不足1重量%时,容易产生沉降和沉淀,即使不产生沉降和沉淀,也会在和含铬酸盐水系树脂混合时发生凝聚,其混合稳定性变差。另一方面,乳化剂的量超过20重量%时,形成之保护膜的耐水性、耐碱性等降低。这些润滑剂既可单独使用,也可2种以上并用,可进一步提高润滑性。润滑剂是在适量的水,最好是脱离子水中使用乳化剂使之分散。
润滑剂的配合量以固态形式在本发明组合物中为1-50重量%,特别是以5-40重量%为好。配合量在1重量%以下时,润滑性不充分,但在51重量%以上时,形成之保护膜的强度,以及对基底金属的粘合性降低,润滑性、耐蚀性、耐碱性、耐溶性、涂膜粘合性等降低。
在本发明的实施方案中,表面处理组合物中添加的磷酸离子是以正磷酸之类的酸、磷酸铵、磷酸钠、磷酸钾之类的碱性磷酸盐、磷酸钾、磷酸镁之类的碱土类磷酸盐、磷酸锌、磷酸锰、磷酸镍、磷酸钴、磷酸铝等金属磷酸盐的形式供给。这些磷酸离子在本发明之组合物保护膜形成时,容易产生6价铬离子的乳胶树脂成分还原,同时与3价铬化合形成难溶性盐,可以提高保护膜的耐碱性,耐蚀性。
在本发明的第二实施方案中,表面处理组合物中添加的二氧化硅可一次使用粒径为5μm-100μm大的微粒子状二氧化硅,其制法用气相法、液相法都行。二氧化硅在其表面上吸附6价铬使之稳定化从而抑制6价铬的溶出,因而能提高保护膜的耐蚀性。
本发明的第三实施方案中,表面处理组合物中添加的钴、镍、锰、锌等重金属,由于这些金属离子在保护膜形成时与铬酸结合而成难溶于水的铬酸重金属盐,在为去除压力机加工中的污物,将金属原材进行碱脱脂时减少6价铬的溶出,因而提高了耐蚀性。这些重金属离子希望以碳酸盐、氢氧化物,氧化物或磷酸盐的形式供给。硫酸盐、氯化物、硝酸盐等这些金属离子和形成可溶性盐之阴离子的化合物,由于会妨碍这些金属离子和铬酸的难溶性盐的形成,因此是不希望的。
本发明的第四实施方案中,表面处理组合物中添加的氟离子在保护膜形成时赋予金属表面活性化,改善了金属基底和保护膜的粘合性,继而改善了金属和涂膜之间的粘合性。氟离子可以氢氟酸、氢氟酸锆、氢氟酸硅、氢氟酸钛、氢氟酸硼及这些酸的胺盐、锂盐、钠盐、钾盐等的氟化物的形式添加。
以下是这四种添加物的添加量,而磷酸离子按PO4/全Cr重量比为0.05-5,二氧化硅微粒子按SiO2/全Cr重量比为0.1-10,氟化合物按F/全Cr重量比为0.01-0.5的范围是合适的、超出该范围以外,则添加效果不太好。钴、镍、锌、锰金属离子的情况下,如果这些金属离子和3价铬离子之合计克当量,与铬酸和磷酸之合计的克当量比(金属离子+Cr3+)/(CrO2- 4+PO3- 4)不是≤0.5,组合物中往往产生沉淀,因此希望上述比为0.5以下。
本发明之组合物所涂覆的原料,其对象是铁、铝、锌、锡、铜以及这些金属的合金类(作为合金元素,例如添加锌、铝、铬、硅、钴、锆、锡、钛、铁、铅、镍、镁、锰、钼、磷等一种或两种以上),这些金属原材料的镀材、以及这些金属原材及其镀材的铬酸盐处理材料、磷酸盐处理材料,阳极处理材料等也是其涂覆对象。处理对象的形状为板状、线圈状、棒状、线状等,在这些形状的金属原材上涂覆组合物的涂饰方法,例如可使用毛刷涂,喷涂、滚涂、淋涂、浸渍涂等。涂覆后的干燥、硬化方法,可采用热风炉、红外线炉、高频炉等。
以下,以本发明之金属处理组合物处理指标为例,说明表面处理钢板及铝板的制造。
将本发明之金属处理组合物涂覆在镀锌钢板、冷轧钢板、铝板等金属板上时的最佳铬附着量在1-500mg/m2,更佳为5-300mg/m2的范围内。铬附着量不足1mg/m2时则耐蚀性不足,但如果超过500mg/m2,则Cr的着色显著,商品价值差。
同样,最佳树脂附着量在10-2000mg/m2,更佳为50-1500mg/m2的范围内。不足10mg/m2时则润滑性,耐蚀性、耐指纹性、涂膜粘合性方面,其树脂的效果不够。即使树脂的附着量超过3000mg/m2,不仅没有提高耐蚀性、耐指纹性、涂膜粘合性,而且由于降低了焊接性而成为不适于熔接加工用途的保护膜。
本发明之组合物中的3价铬和丙烯酸聚合物树脂的交联时其到达板温必须在80℃以上,其干燥,固化条件在现存的表面处理钢板线中是充分对应的。
以上说明是就表面处理组合物的具体化合物进行的说明,但本发明并不限于这些化合物,而是基于权利要求范围记载所定义的内容。
含铬酸盐水系树脂含有强酸且作为强氧化剂的铬酸,因此润滑剂在有机化合物情况下接受凝聚作用和氧化作用,配合的涂覆剂容易产生沉淀、凝聚、增粘凝胶化等现象。而且,如果在含铬酸盐水系树脂中添加润滑剂,则会有涂覆后的涂膜粘合性降低的问题。本发明是对如何使润滑剂在含铬酸盐水系树脂中稳定地分散,实现在形成的保护膜上具有优良润滑性、耐食性、涂覆性的金属表面处理组合物方面进行的研究,发现使用非离子系乳化剂以致分散润滑剂,将由此获得的分散系和丙烯酸系聚合物乳胶混合是极有效的。
如上所述,涂覆、干燥而形成的本发明之组合物保护膜其润滑性优良,因此对一般加工度的成形品,可以不涂压力机油等将表面处理材料按原状态进行深冲加工等之压力成形加工而不会产生金属模的摩耗及板材切伤。而且,进行极严格的特殊压力加工时,本发明之表面处理保护膜仅成形性不足,因此,在这种情况下不能不使用压力机油,尽管如此,本发明之保护膜润滑性的效果仍能发挥。而且,本发明之表面处理保护膜,即使对碱脱脂,溶剂脱脂(三氯乙烷等)也显示出优良的耐脱脂性,前述性能在脱脂前后几乎没有差异。因此,将金属原材制造、处理、保管中产生的污染脱脂后进行加工时,能发挥优良的成形性。
同时,本发明之表面处理保护膜防金属腐蚀的耐蚀性,对金属的粘合性都很优良。由于这些性能优良,因此,即使是处理材料处于长期保管状态也不会引起金属腐蚀,而且还可避免由于基底原材的腐蚀和膜的剥离、润滑剂脱落而导致润滑性恶化。
以下说明本发明的实施例。
(实施例)
丙烯酸系聚合物乳胶的制造例1:
由以下方法制得丙烯酸系聚合物乳胶。
A)单体乳化液组成
离子交换水 150重量份
乳化剂840S1)16重量份
プロノン#2082)2重量份
甲基丙烯酸 4重量份
甲氧基亚甲基丙烯酰胺 2重量份
正丁基丙烯酸酯 82重量份
甲基丙烯酸甲酯 112重量份
B)装入4口烧瓶的组成
离子交换水 116重量份
乳胶840S 4重量份
プロノン#208 4重量份
C)聚合起始剂
5%过硫酸氨水溶液 10重量份
5%酸性亚硫酸钠水溶液 10重量份
1)聚氧乙烯辛基苯基醚的70%水溶液(花王石碱(株)制、非离子性乳化剂)
2)聚氧乙烯-聚氧丙烯嵌段聚合物(日本油脂(株)制、非离子性乳化剂)
(聚合法)
在容量为1L备有搅拌装置的4口烧瓶中,装入B)并加热溶解且保持在40℃,在另一个容量0.5L带塞的三角烧瓶里装入A)制成单体乳化液,将其10%加到5%过硫酸氨水溶液及5%酸性亚硫酸钠水溶液各25%之中,在40-50℃进行15-20分钟的聚合。然后,将剩余的90%的A)、和聚合起始剂各剩余的75%在40-50℃中花费3小时滴下。滴下终了后在40-50℃保持1小时结束聚合。所得乳胶其浓度43%,粘度300cp,pH2.2。
丙烯酸系聚合物乳胶的制造例2-4:(制造例:3、4是比较制造例)
制造例1中,按表1所示改变单体组成及乳化剂进行聚合,制得丙烯酸系聚合物乳胶。
润滑剂的分散例1:
按以下方法制得润滑剂的乳化物。
将石蜡蜡(日本精蜡株式会社制,品名155)40重量份加热至熔点,其中加入山梨糖醇单硬脂酸酯2重量份,聚氧乙烯硬脂酰醚3重量份并一起熔融。将熔融物保持在97℃,同时在搅拌下10分钟内添加95-99℃的脱离子水55重量份(转数=100rpm)。添加后,将石蜡-脱离子水系混合液在搅拌下(转数=20rpm)放冷,处于室温下。将石蜡浓度用脱离子水调整、得到浓度40重量%的石蜡蜡乳化物。润滑剂分散物的分散例2-12(乳化例8-12是比较乳化例):
在润滑剂的分散例1中,将润滑剂及乳化剂按表2变化,得到润滑剂分散物。
实施例1-12
将丙烯酸系聚合物乳胶的制造例1、2中所得之丙烯酸聚合物乳胶和6价铬(用CrO3),或其中加3价铬(用甲醇部分还原6价铬)等之无机化合物,和润滑剂之分散例1-7所得之润滑剂乳化物混合,得到表3所示内容的本发明金属表面处理组合物。将这些组合物以干燥膜量为1g/m2滚涂到干净的电镀锌钢板上(镀敷量=20g/m2),在使到达板温为100℃的热风中干燥,作为试验材料。本发明中金属表面处理组合物的稳定性及供试材料的性能试验结果示于表3中。
比较例1-11
制造例3、4中所得之丙烯酸系聚合物乳胶,以及润滑剂的分散例8-12,及6价铬,3价铬等无机化合物混合之,得到表3所示内容的金属表面处理组合物作为比较例。将这些组合物用上述同样方法涂覆干燥,作为比较组合物的处理材料。比较例组合物的稳定性、以及处理材料的性能试验结果示于表3。
试验方法及评价基准:
1.稳定性:
将金属表面处理组合物置于40℃的恒温条件下,观察直至凝胶化的天数。
○-30日以上
△-7日以上,不足30日
×-不足7日
2.未涂覆板耐蚀性
本发明实施例及比较的供试材料不进一步用涂料涂覆,实施144小时的盐水喷雾试验(JIS-Z-2371),测定生锈面积。
○-生锈面积:不足5%
△-生锈面积:5-30%
×-生锈面积:31%以上
3.涂覆板耐蚀性
在供试材料,比较材料上涂覆烤漆型蜜胺醇酸涂料(涂膜厚20±2μm),在该涂膜上刻出直达基底金属的伤痕,进行200小时的盐水喷雾试验。实施完后剥离胶带,测定伤痕两侧平均剥离宽度,评价涂覆板的耐蚀性。
○-剥离宽度:0.1-3.0m/m
×-3.1m/m以上
4.涂膜粘合性
在上述涂板上刻出1mm见方的100个方块、用杯突试验机推压5mm后,剥离胶带测定涂覆残存的刻度数。
○-残存的刻度数:90-100
×-残存的刻度数:89以下
5.深冲性
坯料径:96mmφ,冲头:40mmφ,防皱压:1.0ton的条件下进行圆筒深冲试验。
○-深冲脱模,保护膜的结构等观察不出异常现象
×-不能深冲脱模
而且,上述试验中1-4是按本发明实施例之供试材料及比较材料的碱脱脂前后来回2次进行实施。碱脱脂是使用中碱脱脂剂(日本パ-ヵラィジング制パルクリ-ンN-364S)、浓度:0.2%、以液温=60-65℃,喷射压0.8kg/cm2进行2分钟清洗。
表1
制造丙烯酸系聚合物乳胶的单体、乳化剂
3)月桂基硫酸钠(花王石碱(株)制的阴离子性乳化剂)
Claims (3)
1、润滑性优良的金属表面处理组合物,其特征在于,它含有作为无机化合物的6价铬离子或6价铬离子和3价铬离子,以及作为有机化合物的下述丙烯酸系聚合物乳胶,作为润滑成分的用非离子系乳化剂分散的1种或2种以上润滑剂分散物1重量%-50重量%(固体含量比),pH为5以下,且在含铬酸盐水系树脂液中配合润滑剂分散物;
1)乙烯系不饱和羧酸单体,
2)(甲)用以下通式表示的烷氧基亚甲基(甲基)丙烯酰胺及其衍生物
但,X为CnH2n+1(n=0或1)
Y为CmH2m+1(m=0-4)
(乙)酸性磷氧烷基(甲基)丙烯酸酯,
(丙)烷氧基烷基(甲基)丙烯酸酯
中选择出来的1种或2种以上的单体,
3)从丙烯酸系单体(至少一部分往往是由上述2)的(丙)构成)中选择出来1种或2种以上构成,根据要求含有这些共聚性单体的骨架用单体,
将上述1)、2)、3),用基本上不含阴离子性乳化剂及阳离子性乳化剂,但含有聚乙烯-聚氧丙烯嵌段聚合物系乳化剂的非离子性乳化剂进行乳化聚合而得到的丙烯酸系聚合物乳胶。
2、根据权利要求1所述之金属表面处理组合物,其中,作为无机化合物,还含有(1)磷酸离子、(2)二氧化硅以及(3)钴、镍、锰、锌之1种以上金属离子构成的(1)、(2)、(3)组中的1种以上。
3、根据权利要求1或2所述之金属表面处理组合物,其中,作为无机化合物,还含有氟离子。
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US20060019839A1 (en) * | 2003-12-12 | 2006-01-26 | Murray John A | Engine part coating created from polysiloxane and coating method |
US20060052253A1 (en) * | 2004-09-03 | 2006-03-09 | Murray John A | Lubricant including polyether-or polyester modified polydialkylsiloxane |
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ATE551441T1 (de) * | 2006-02-14 | 2012-04-15 | Henkel Ag & Co Kgaa | Zusammensetzung und verfahren einer trivalenten dry-in-place korrosionsfesten chromiumbeschichtung zur verwendung auf metall- oberflächen |
EP2044239B1 (en) * | 2006-05-10 | 2014-09-03 | Henkel AG & Co. KGaA | Method for making a corrosion resistant coating on metal surfaces using an improved trivalent chromium-containing composition |
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JP6574973B1 (ja) * | 2018-10-09 | 2019-09-18 | サイデン化学株式会社 | 金属表面処理用樹脂エマルション、金属表面処理剤、表面処理金属材及びその製造方法、並びに樹脂エマルションの製造方法 |
CN116670236A (zh) * | 2021-01-06 | 2023-08-29 | 汉高股份有限及两合公司 | 用于涂锌铝钢的基于Cr(III)的改善钝化 |
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-
1990
- 1990-01-23 JP JP2011747A patent/JPH03219086A/ja active Pending
-
1991
- 1991-01-23 KR KR1019910001103A patent/KR930007152B1/ko not_active IP Right Cessation
- 1991-01-23 CN CN91100513A patent/CN1043242C/zh not_active Expired - Fee Related
-
1993
- 1993-05-17 US US08/061,341 patent/US5378291A/en not_active Expired - Fee Related
Cited By (8)
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CN1061367C (zh) * | 1996-06-21 | 2001-01-31 | 日本帕卡濑精株式会社 | 金属材料的冷塑性加工用水系润滑剂 |
CN100540642C (zh) * | 2003-02-03 | 2009-09-16 | 本田技研工业株式会社 | 水溶性金属加工用润滑剂 |
CN105368560A (zh) * | 2015-11-25 | 2016-03-02 | 苏州捷德瑞精密机械有限公司 | 一种环保型切削液及其制备方法 |
CN106784418A (zh) * | 2016-12-16 | 2017-05-31 | 苏州福斯特光伏材料有限公司 | 一种防腐蚀处理层及其在锂电池软包装材料中的应用 |
CN106784418B (zh) * | 2016-12-16 | 2020-01-10 | 苏州福斯特光伏材料有限公司 | 一种防腐蚀处理层及其在锂电池软包装材料中的应用 |
CN109233985A (zh) * | 2018-10-31 | 2019-01-18 | 首钢集团有限公司 | 一种镀锌板用无机润滑溶液及处理方法 |
CN113831956A (zh) * | 2020-06-24 | 2021-12-24 | 上海梅山钢铁股份有限公司 | 一种冷轧乳化液粒径尺寸的控制方法 |
CN113831956B (zh) * | 2020-06-24 | 2022-10-14 | 上海梅山钢铁股份有限公司 | 一种冷轧乳化液粒径尺寸的控制方法 |
Also Published As
Publication number | Publication date |
---|---|
CN1043242C (zh) | 1999-05-05 |
JPH03219086A (ja) | 1991-09-26 |
KR910014536A (ko) | 1991-08-31 |
US5378291A (en) | 1995-01-03 |
KR930007152B1 (ko) | 1993-07-30 |
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