CN1148437C - 金属材料的塑性加工用润滑剂 - Google Patents

金属材料的塑性加工用润滑剂 Download PDF

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CN1148437C
CN1148437C CNB991097157A CN99109715A CN1148437C CN 1148437 C CN1148437 C CN 1148437C CN B991097157 A CNB991097157 A CN B991097157A CN 99109715 A CN99109715 A CN 99109715A CN 1148437 C CN1148437 C CN 1148437C
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lubricant
weight
plastic working
water
composition
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CN1243150A (zh
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今井康夫
永田秀二
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NIPPON BACALAIJINGU CO Ltd
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NIPPON BACALAIJINGU CO Ltd
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Abstract

本发明提供一种塑性加工时作为润滑剂，可以不必通过由磷酸盐形成底膜，而通过水系浸渍或喷涂使其附着后，使其干燥的简便步骤得到极优异润滑性的金属材料塑性加工用润滑剂组合物者。该金属材料的塑性加工用润滑剂组合物含有(A)合成树脂、(B)水溶性无机盐和水、(B)/(A)(固体成份重量比)为0.25/1～9/1，合成树脂溶解或分散于其中。该组合物还可包含润滑材料、固体润滑剂、极压添加剂。

Description

金属材料的塑性加工用润滑剂
技术领域
本发明涉及润滑性优良的供钢铁、钛、铝等金属材料进行塑性加工用的润滑剂。更详细而言，本发明涉及在进行塑性加工时，通过喷雾或浸渍对被加工物进行涂布后立即干燥的简单工艺，以形成具优异润滑性被膜的塑性加工金属材料用的润滑剂。
背景技术
一般在对金属材料塑性进行加工时为减少被加工材料与工具之间因金属接触而产生的摩擦，防止热胶着或金属磨损的目的，都会使用液状或固体状的润滑剂。所用润滑剂因使用方法的不同可大体上可分为二种。其一为物理性附着于金属表面的润滑剂，另一为通过化学反应使在金属表面形成载体被膜后附着润滑材料的润滑剂。前一种润滑剂为以矿物油、植物油或合成油为基油，并添加极压添加剂的润滑剂，有附着于金属表面后直接进行塑性加工的类型，或使金属皂、石墨或二硫化钼等固体润滑剂与粘合剂成份一起分散于水中，附着于金属表面后使其干燥，然后进行塑性加工的类型等。这些润滑剂可以采用涂布或浸渍的使用方法，所以使用方法极为简便，还有几乎不需液体管理等优点，因此多用于比较轻的塑性加工。另外，后一种润滑剂的处理即所谓的化学被膜处理，是通过化学反应在金属表面生成有载体作用的磷酸盐被膜后，用硬脂酸钠或硬脂酸钙等反应皂或非反应皂作为润滑材料进行处理。此种类型具有作为载体的化学被膜与作为润滑材料的金属皂的二层结构，具有极佳的耐高热胶着性。所以在拔丝、拉管、锻造等塑性加工领域被广为使用。
但是，磷酸盐处理是一种化学反应，所以必须有复杂的液体管理，而且为了在所形成的化学被膜上涂布润滑材料，必须进行包括水洗或酸洗在内的多项处理工艺。此外，由于处理时使用水洗水或由化学被膜产生大量废液，以及为控制化学反应必须加热，因此，必须花费大笔设备投资或高额操作费用。
为解决此类问题，代替花费较多的磷酸盐处理，曾有人努力改善上述物理方法润滑膜的性能，以期将它提高至等同于化学处理的程度。作为这种努力的结果是提出使用油系润滑剂或水系润滑剂的方法。作为油系润滑剂，特公平4-1798号公报公开了“在氯化石蜡、磷酸酯等极压添加剂与异丁烯-正丁烯的共聚物与动植物油等配合的润滑油中，配合金属皂或固体润滑剂的冷加工用润滑剂”。但即使是这些高性能润滑剂，与化学被膜处理后进行反应皂润滑处理的润滑法比较，在加工性上仍有问题，而且，由于使用极压添加剂，加工时会有产生臭气的缺点。
另外，水系润滑剂的场合，有直接以湿式使用的润滑剂，以及作为干式被膜使用的润滑剂，直接以湿式使用的水系润滑剂与上述油系润滑剂一样，是直接浇注于工具或加工材料上使用，作为干式被膜使用的水系润滑剂则与上述化学被膜一样，是在处理槽浸渍处理后，在干燥工序中使水分蒸发，得到固体被膜。作为前者，特公昭58-30358号公报中公开了“以碳酸氢盐(固体)为主成份，且在其中已加入少量分散剂、表面活性剂和固体润滑剂的供金属管的冷或热加工用的润滑剂”，但仍无法达到取代化学被膜处理而广泛使用的地步。另外，作为后者，特开昭52-20967号公报公开了“以水溶性高分子或其水性乳胶为基材，配合固体润滑剂与化学被膜形成剂所成的润滑剂组合物”等，但仍无法得到可与化学被膜处理相匹敌的润滑剂。
发明内容
本发明为解决上述现有技术所存在问题，提供一种金属材料塑性加工用润滑剂组合物，作为塑性加工用润滑剂，不需要由磷酸盐形成的底膜，在水系中，通过浸渍或喷雾使其附着后干燥的简便工艺，即可具有与磷酸盐处理法相匹敌的润滑性。
本发明人等为解决上述课题，经再三深入研讨的结果，发现若将金属板浸渍于含合成树脂与水溶性无机盐的水溶液或水分散液中，并进行干燥的话，即可得到密合性极佳的强韧被膜。另外又发现通过使此水溶液或水分散液中含有润滑材料或固体润滑剂等，可使所得被膜具有极优异的润滑性能，从而完成了本发明。
也就是说，本发明是一种金属材料的塑性加工用润滑剂组合物，其特征在于，含有(A)合成树脂、(B)水溶性无机盐和水，且(B)/(A)(固体成份重量比)为0.25/1～9/1，合成树脂呈溶解或分散状态。
本发明的金属材料塑性加工用润滑剂组合物中优选还含有1～20重量％至少一种选自金属皂、蜡、聚四氟乙烯和油的物质作为润滑材料成份。上述水溶性无机盐以至少一种选自硫酸盐、硼酸盐、钼酸盐、钒酸盐和钨酸盐为宜。上述合成树脂优选至少一种选自聚乙烯醇、聚乙烯吡咯烷酮、丙烯酸树脂、乙酸乙烯树脂、环氧树脂、聚氨酯树脂及酚系树脂的树脂。本发明组合物中成份(A)与成份(B)的较佳组合是成份(A)为聚氨酯树脂、成份(B)为硼酸盐的组合。换言之，本发明组合物的较佳实施形态以固体成份计，是含有0.3～10.0重量％的成份(A)聚氨酯，以及含有1.0～10.0重量％的成份(B)硼酸盐，进而含有润滑材料的上述金属材料塑性加工用润滑剂组合物。本发明组合物中更优选以含1～20重量％的至少一种选自二硫化钼、石墨、聚四氟乙烯、氮化硼、云母和氟化石墨的物质作为固体润滑剂。另外，本发明组合物优选还含有0.5～5重量％的至少一种选自硫系极压添加剂，有机钼系极压添加剂、磷系极压添加剂和氯系极压添加剂的物质作为极压添加剂。
具体实施方式
以下更详细说明本发明。本发明的金属材料塑性加工用润滑剂组合物中所用的(A)合成树脂，只要是能够形成耐塑性加工且具有密合性和被膜强度的被膜，即不必特别限定，例如可用聚乙烯醇、聚乙烯吡咯烷酮、丙烯酸系树脂、乙酸乙烯树脂、环氧树脂、聚氨酯树脂及酚系树脂。使用的树脂无论是水溶性或水分散性皆可，可按使用目的选择。例如塑性加工后必须脱膜时可选水溶性合成树脂，需要耐水性时可选择水分散性合成树脂。
本发明中使用的合成树脂溶解或分散于本发明组合物中。为使其分散，可根据需要采用公知的表面活性剂。
聚乙烯醇是水解聚乙酸乙烯而制成，但除了完全水解物以外水解度为50％或以上的水解物亦可使用。本发明中的聚乙烯醇还包括由50摩尔％或以上的乙烯醇单元与乙烯单元构成的共聚物。聚乙烯醇的分子量以凝胶渗透色谱法测定时最好为300～2000。
聚乙烯吡咯烷酮是聚合N-乙烯基-2-吡咯烷酮而制得的。用凝胶渗透色谱法测定，聚乙烯吡咯烷酮的分子量优选为500～1000。
丙烯酸系树脂可举出聚合至少一种丙烯酸系单体而得到的树脂。丙烯酸系单体可以举出丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、甲基丙烯酸异丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、甲基丙烯酸2-乙基己酯、丙烯酸辛酯等(甲基)丙烯酸C1～C8烷基酯；丙烯酸甲氧基甲酯、丙烯酸甲氧基乙酯、丙烯酸乙氧基甲酯、丙烯酸乙氧基乙酯、甲基丙烯酸甲氧基甲酯、甲基丙烯酸甲氧基乙酯、甲基丙烯酸乙氧基甲酯、甲基丙烯酸乙氧基乙酯、丙烯酸甲氧丁酯等(甲基)丙烯酸低级烷氧基低级烷基酯；(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸3-羟丙酯等(甲基)丙烯酸羟基低级烷基酯；丙烯酰胺、甲基丙烯酰胺；N-羟甲基丙烯酰胺、N-羟甲基甲基丙烯酰胺、N-丁氧基甲基丙烯酰胺、N-丁氧甲基甲基丙烯酰胺等N-未取代或具有取代(尤其是低级烷氧基取代)羟甲基的(甲基)丙烯酰胺；丙烯酸膦酰氧基甲酯、丙烯酸膦酰氧基乙酯、丙烯酸膦酰氧基丙酯、甲基丙烯酸膦酰氧基甲酯、甲基丙烯酸膦酰氧基乙酯、甲基丙烯酸膦酰氧基丙酯等(甲基)丙烯酸膦酰氧基低级烷基酯；丙烯腈；丙烯酸、甲基丙烯酸等。本发明中的丙烯酸系树脂亦包含至少一种上述的丙烯酸系单体与苯乙烯、甲基苯乙烯、乙酸乙烯、氯化乙烯、乙烯基甲苯、乙烯等其他乙烯性单体中至少一种单体的共聚物，且含有30摩尔％或以上丙烯酸系单体单元。丙烯酸系树脂的分子量以凝胶渗透色谱法测定时为1000～1,000,000，尤其以100,000～600,000为宜。
乙酸乙烯树脂是由乙酸乙烯聚合而得到的树脂。本发明中乙酸乙烯树脂亦包括聚乙酸乙烯树脂中的乙酸乙烯单元水解未达50％的那些。另外，本发明中的乙酸乙烯树脂还包含乙酸乙烯与乙烯的共聚物(乙酸乙烯单元50摩尔％或以上)。乙酸乙烯树脂的分子量以凝胶渗透色谱法测定时以200～2000为宜。
环氧树脂，可例举，使双酚类尤其是双酚A(2，2-双(4′-羟苯基)丙烷)与环氧氯丙烷反应所得的双酚型环氧树脂，尤其可为以下式所示双酚A型环氧树脂。除此之外还有例如使酚-酚醛清漆树脂的酚性羟基缩水甘油醚化所得的酚醛清漆型环氧树脂，芳香族羧酸的环氧丙基酯，以过酸使乙烯性不饱和化合物的双键环氧化的过酸环氧型等。另外还可举出如上所述在环氧树脂的树脂骨架上加成环氧乙烷或环氧丙烷得到的物质多元醇的环氧丙基醚型等。其中以使用双酚A型环氧树脂为最佳。环氧树脂的分子量以凝胶渗透色谱法测定时以350～5000为宜。
聚氨酯树脂是具有氨酯键(NHCOO)的合成树脂，聚氨酯树脂一般可用具有二个或以上异氰酸酯基的多异氰酸酯化合物与具有二个或以上活性氢基的多元醇进行加聚反应所得的树脂。该多元醇可为聚酯多元醇和聚醚多元醇。聚酯多元醇有例如由乙二醇、二甘醇、三甘醇、1，2-丙二醇、1，3-丙二醇、新戊二醇、1，2-丁二醇、1，3-丁二醇、1，4-丁二醇、3-甲基戊二醇、己二醇、氢化双酚A、三羟甲基丙烷、丙三醇等低分子量多元醇，与琥珀酸、戊二酸、己二酸、癸二酸、邻苯二酸、间苯二酸、对苯二酸、苯三甲酸、四氢邻苯二甲酸、桥亚甲基四氢邻苯二甲酸、六氢邻苯二甲酸等元酸反应所得的末端具有羟基的聚酯化合物。
另外，聚醚多元醇可为例如乙二醇、二甘醇、三甘醇、1，2-丙二醇、1，3-丙二醇、新戊二醇、1，2-丁二醇、1，3-丁二醇、1，4-丁二醇、3-甲基戊二醇、己二醇、双酚A、氢化双酚A、三羟甲基丙烷、丙三醇等低分子量多元醇或它们的环氧乙烷和/或环氧丙烷高加成物、聚乙二醇、聚丙二醇、聚乙二醇/丙二醇等聚醚多元醇、聚己内酯多元醇、聚烯烃多元醇、聚丁二烯多元醇等。
另外，多异氰酸酯可例举脂肪族、脂环式和芳香族多异氰酸酯，具体而言有四亚甲基二异氰酸酯、六亚甲基二异氰酸酯、赖氨酸二异氰酸酯、氢化苯二甲基二异氰酸酯、1，4-环己基二异氰酸酯、4，4′-二环己基甲烷二异氰酸酯、2，4′-二环己基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、3，3′-二甲氧基-4，4′-亚联苯基二异氰酸酯、1，5-萘二异氰酸酯、1，5-四氢化萘二异氰酸酯、2，4-甲苯二异氰酸酯、2，6-甲苯二异氰酸酯、4，4′-二苯甲烷二异氰酸酯、2，4′-二苯基甲烷二异氰酸酯、亚苯基二异氰酸酯、苯二甲基二异氰酸酯、四甲基苯二甲基二异氰酸酯等。
聚氨酯树脂的分子量在以凝胶渗透色谱法测定时以500～500,000为宜。
酚树脂可举出由酚、甲酚、二甲苯酚等至少一种酚类与甲醛反应所得的树脂，可为酚醛清漆型树脂，可溶酚醛型树脂中的任一树脂。使用酚醛清漆型树脂时，必须使六亚甲基四胺等作为硬化剂共存。酚树脂被膜于后述的干燥步骤中进行硬化。对于酚树脂的分子量并无特别限制。
上述各种合成树脂当然亦可使用市售品，此种情况下，一般在合成树脂为水溶性时可以作为水溶液取得，合成树脂为水不溶性时，可使用后述的、与为使润滑材料分散所用的表面活性剂同样的表面活性剂使之分散于水的分散液取得。
其次，水溶性无机盐(B)是在通过干燥与合成树脂一起形成均匀的被膜时，为使被膜具有硬度和强度而添加的物质。所以所选出的水溶性无机盐具有可均均地溶解于溶液中，干燥时可与合成树脂均匀析出，借此提高被膜强度的性质。作为这种性质的水溶性无机盐以使用至少一种选自硫酸盐、硼酸盐、钼酸盐、钒酸盐和钨酸盐为宜。可为例如硫酸钠、硫酸钾、硼酸钠(四硼酸钠等)、硼酸钾(四硼酸钾等)、硼酸铵(四硼酸铵等)、钼酸铵、钼酸钠、钨酸钠、钒酸钠等的物质。它们可单独使用，亦可组合二种或以上使用。
本发明中的合成树脂(A)与水溶性无机盐(B)的重量比(固体成份重量比)(B)/(A)必须为0.25/1～9/1。该重量比小于0.25/1时被膜的硬度不足，金属材料会产生金属磨损或热胶着。另外，该重量比大于9/1时，则会降低被膜的密合性和随动性，加工时被膜变得易脱落、润滑性降低。上述(B)/(A)重量优选为0.3/1～8/1，更佳为0.5/1～7/1。
所形成被膜的性质可用水溶性或水分散性合成树脂与水溶性无机盐的重量比加以调整。根据加工或滑动部位所受负担大小决定最适当的重量比。即水溶性无机盐的比例多时被膜硬度便增大，耐负荷性能提高，但被膜的密合性会降低。
例如，如塑性加工封闭锻造那种，加工条件严苛的情况时，添加较多量水溶性无机盐为宜，具体而言，合成树脂(A)与水溶性无机盐(B)的重量比(固体成分重量比)(B)/(A)以1.5/1～9/1为宜，2/1～8/1较好，2/1～7/1最好。又如薄板的压制加工时，由于被膜的随动性以大为佳，所以水溶性无机盐的比例以少为好，其重量比以0.25/1～2/1为宜，0.3/1～2/1更好。
关于合成树脂和水溶性无机盐的配合量，使二者的总量(固体成份合计)为本组合物的1～20重量％为好，1～15重量％较好，3～10重量％更好。
将本发明的金属材料塑性加工用润滑剂组合物用于金属表面上时，若塑性加工为一段塑性加工时，由上述成份(A)、(B)和水组成的组合物中还可以根据需要进一步含有润滑材料成份、固体润滑剂和/或极压添加剂，这种润滑剂组合物很适宜用于金属材料，但若塑性加工为多段的塑性加工(例如拉丝或锻造时的多段加工)时，优选将上述成份(A)、(B)和水的组合物涂布于金属材料，将干燥后生成的被膜作为载体，然后在其上面在每一加工阶段再根据需要涂布润滑材料成份、固体润滑剂和/或极压添加剂(例如撒下去)然后进行塑性加工。
所以本发明的金属材料塑性加工用润滑剂组合物，特别是供金属材料进行一段塑性加工时，或多阶段加工时，可根据需要进一步含有润滑材料成份、固体润滑剂和/或极压添加剂为宜。
上述成份中润滑材料成份通常优选含于该组合物中。该润滑材料成份以优选在水溶液中稳定，且不会降低被膜强度，此种物质可为金属皂、蜡、聚四氟乙烯和油。具体而言，金属皂可为硬脂酸钙、硬脂酸铝、硬脂酸钡、硬脂酸锂、硬脂酸锌等，蜡可为聚乙烯蜡、聚丙烯蜡、巴西棕榈蜡、蜜蜡、石蜡等、聚四氟乙烯可为例如聚合度100万～1000万左右的聚四氟乙烯。另外，油可用植物油、矿物油、合成油等，例如植物油有棕榈油、蓖麻籽油、菜籽油等，矿物油有机油、涡轮机油、锭子油等，合成油有酯油、硅油等。
这些成分可以水分散液或水乳胶的形态与其他成份混合，使其含于本组合物中。
润滑材料通常被分散或乳化于本发明组合物中。
润滑材料的配合量以1～20重量％为好，1～10重量％较宜，2～7重量％更好。配合量小于1重量％时被膜受到的摩擦增加，容易发生热胶着，超过20重量％时，会降低被膜的密合性。
上述含成份(A)、成份(B)、润滑材料和水的本发明组合物的较佳实施形态是含有以固体成份计为0.3～10.0重量％的(A)聚氨酯树脂、1.0～10.0重量％的(B)硼酸盐、润滑材料和水、(B)/(A)(固体成份重量比)为0.25/1～9/1的金属材料塑性加工用润滑剂组合物。聚氨酯树脂为0.3重量％或以上是为防止降低被膜的密合性而考虑的较佳数值、10.0重量％或以下是因考虑到防止降低被膜硬度，发生热胶着而言的较佳数值。又，硼酸为1.0重量％或以上是从防止被膜的硬度变弱导致金属材料发生热胶着的观点而言的较佳数值、10.0重量％或以下是从可防止被膜因密合性或被膜的延展性降低，加工时被膜易于脱落，导致降低其润滑性的观点而言为较佳数值。
此实施形态中，润滑材料的种类及其配合量均可与上述一样。
加工条件较严苛的塑性加工时，本发明组合物优选还含有固体润滑剂。这时所用固体润滑剂优选可稳定地存在于被膜中，在较重的负荷重量下亦有助于润滑。这种固体润滑剂可举出石墨、二硫化钼、氮化硼、氟化石墨、云母等。
该固体润滑剂的配合量以1～20重量％为宜。1～10重量％较宜，1～5重量％更好。配合量小于1重量％时耐热胶着性有不足之虞，大于20重量％时则有密合性降低之虑。
加工条件更严苛的塑性加工时，最好在上述组合物中进一步含有极压添加剂。这时作为极压添加剂优选在被膜中稳定，通过加工可在工具与金属的接触面发挥极压效果者为宜。此种极压添加剂可为硫化烯烃、硫化酯、亚硫酸酯、硫代碳酸酯、氯化脂肪酸、磷酸酯、亚磷酸酯、二硫代胺基甲酸钼(MoDTC)、二硫代磷酸钼(MoDTP)、二硫代磷酸锌(ZnDTP)等硫系极压添加剂，有机钼系极压添加剂、磷系极压添加剂和氯系极压添加剂。
该极压添加剂的配合量以0.5～5重量％为宜，1～3重量％更好。配合量未达0.5重量％时会有极压效果不足之虑，超过5重量％时则有被膜密合性降低之虑。
为使合成树脂、润滑材料、固体润滑剂和/或极压添加剂分散或乳化而需要表面活性剂时，表面活性剂可用非离子性表面活性剂、阴离子性表面活性剂、两性表面活性剂和阳离子性表面活性剂中的任何一种。对非离子性表面活性剂虽无特别限制，但可例举聚氧化乙烯烷基醚、聚氧化烯(乙烯和/或丙烯)烷苯基醚、聚乙二醇(或环氧乙烷)与高级脂肪酸(例如碳数12～18)所构成的聚氧乙烯烷基酯、脱水山梨醇和聚乙二醇与高级脂肪酸(例C12～C18)所构成的聚氧化乙烯脱水山梨醇烷基酯等。对阴离子性表面活性剂并不特别限制，但可例举用脂肪酸盐、硫酸酯盐、磺酸盐、磷酸酯盐、二硫代磷酸酯盐等。两性表面活性剂亦不特别限制，但可用例如氨基酸型及甜菜碱型羧酸盐、硫酸酯盐、磺酸盐、磷酸酯盐等。阳离子性表面活性剂亦不特别限制，可用例如脂肪族胺盐、季铵盐等。这些表面活性剂可分别单独或组合二种或以上使用。
关于本发明润滑剂组合物的制造方法，只要所制造的润滑剂组合物能满足上述条件即不必特别加以限制。例如，可在水溶性无机盐的水溶液中加入水溶性或水分散性合成树脂，充分搅拌后，添加作为任意成份的润滑材料、固体润滑剂和/或极压添加剂，根据需要使用表面活性剂和水，使其为分散液或乳化液后，经添加上述任意成分、搅拌，可制造本发明组合物。
本发明的润滑剂组合物可在进行铁或钢、铜或铜合金、铝或铝合金、钛或钛合金等金属材料的冷塑性加工(拉丝、拉管、锻造等)时作为润滑剂使用。关于金属材料的形状，不限于棒状材料或块状材料等材料，经热锻造后的造形物(齿轮、轴)等进行加工时也可考虑使用，所以不特别限制。
涂布本发明润滑剂组合物之前，为得到更佳的结果可优选对加工的金属材料依序进行脱脂(一般可用碱脱脂剂)、水洗、酸洗(为了除去金属材料的氧化垢，提高被膜的密合性可使用盐酸等进行)、水洗等前处理，清洁其表面。若未附着有氧化垢时亦可省去酸洗→水洗步骤。这些预处理可依常规方法实施。
本发明的润滑剂组合物可依浸渍、喷雾、浇涂等常规方法涂布于金属材料上。涂布只要润滑剂组合物可充分地覆盖在金属表面上即可，至于涂布时间并无特别限制。涂布后润滑剂组合物必须进行干燥。干燥虽可置于常温进行，但通常于60～150℃进行10～60分钟较为适宜。
用本发明组合物涂布且干燥后的被膜重量，从防止热胶着的观点而言，以1g/m2或以上为宜，又，就成本而言以30g/m2或以下为宜，5～20g/m2更佳，最佳为8～15g/m2。
本发明的润滑系统可考虑由水溶性或水分散性合成树脂与水溶性无机盐的复合被膜而形成者。即可以认为将水溶性或水分散性树脂与水溶性无机盐混合的水溶液附着于金属表面，然后还有使其干燥的步骤，因此首先由于水的蒸发，水溶液的浓度上升，水溶性无机盐的结晶即开始析出。然后由于水再蒸发，合成树脂的浓度升高，并逐渐析出而附着于于金属表面。这时因已有无机盐结晶析出，所以水溶性或水分散性合成树脂便成为一种均匀地分散有水溶性无机盐结晶的被膜。因此，可以认为由于合成树脂与无机盐一起均匀地析出，结果可形成兼具有合成树脂的柔软性与密合性，无机盐的硬度与强度的被膜。
在此与比较例一起举出本发明的实施例，具体说明本发明及其效果。
实施例1～3，比较例1～2
以表1所示比例调制润滑剂组合物。将水溶性无机盐溶解于水后，溶解酚树脂，充份搅拌，以此进行调制。在此润滑剂组合物中浸渍包登(Bowden)摩擦试验片(材质：SPC钢板、150mm×75mm×1.0mm)30秒钟后，于100℃干燥30分钟。然后，向干燥后的整个被膜均匀撒上硬脂酸钙粉末(日本油脂公司制)后，供包登摩擦试验用。
又，涂布包登摩擦试验润滑剂组合物之前，对试验片进行下述(1)～(2)的预处理步骤、进行热风干燥。
(1)碱脱脂(日本Parkerlizing公司制，精细洗剂4360，浓度20g/l，温度60℃，浸渍10分钟)。
(2)水洗以常温的自来水喷洗。
被膜重量(g/m2)是由润滑剂组合物涂布前后的重量差计算出。包登摩擦试验是以试验负荷5kg，试验温度为室温，试验钢球5mmφ，测定摩擦系数与热胶着次数(摩擦系数达到0.25时的滑动次数)。平均摩擦系数是测定热胶着次数×1/2次的前后10次的平均数。
实施例4～17，比较例3～6
依表2所示比例调制润滑剂组合物。将水溶性无机盐溶解于水后，溶解聚氨酯树脂、聚乙烯醇、酚树脂或丙烯酸酯树脂，进行充分搅拌。再添加表2所示的添加剂1(润滑材料)(聚乙烯蜡分散液、硬脂酸钙分散液、聚四氟乙烯或棕榈油乳剂)，进行搅拌，调制成润滑剂组合物。在此润滑剂组合物中浸渍30秒包登摩擦试片(材料：SPC钢板、150mm×75mm×1.0mm)后，于100℃干燥30分钟，供包登摩擦试验用。包登摩擦试验和包登试验片的预处理按实施例1～3同样进行。
将后方冲孔试验片浸渍于润滑剂组合物30秒后，于100℃烘箱放置30分钟，进行彻底干燥后供试验用。
另外，后方冲孔试验片在涂布润滑剂组合物之前，对试验片进行以下的预处理步骤(1)～(4)，然后进行热风干燥。
(1)碱脱脂：(用日本Parkelizing公司制精细洗剂4360，浓度20g/l，温度60℃，浸渍10分钟)。
(2)水洗：用常温的自来水喷洗30秒。
(3)酸洗：盐酸，浓度17.5重量％，温度室温，浸渍时间10分钟。
(4)水洗：用常温的自来水喷洗30秒。
供后方冲孔试验的材料是市售的S45C球状退火材料，试验片的形状为直径30mmΦ，以2mm为单位，将高度由16mm变化至40mm(13水准)。
后方冲孔试验采用200吨曲柄压机，装配模具，在外周部被固定的圆柱状试验片上，用断面收缩率可达50％的直径的冲压机，由上方冲压穿孔，制得杯状成形物。这时冲压的下死点(lower deadpoint)是进行调节使试验片底部所残留的部份为10mm。后方冲孔试验是对试验片由高度较低的试验片开始依序进行加工，试验至加工面发生伤痕为止。评价是以内面无伤痕的试验片的杯内高度作为良好冲孔深度表示。
模型：SKD11
压机：HAP40，螺头直径21.21mmφ
试验片：S45C，球状化的退火材料
孔深度：16、20、24、28、32、36、40、44、48、52、56、60mm。
加工速度：30冲程/分钟
将后方冲孔试验示于图1。
比较例7
与实施例4～10同样的试验片，依表2所示条件对后方冲孔试验片进行化学处理和反应型皂润滑剂处理，所得试验片与实施例4～10一样供包登摩擦试验和后方冲孔试验用。
实施例18～34
以表3所示比例调制润滑剂组合物。即，依实施例4～10进行同样操作后，将添加剂B(二硫化钼、石墨、氮化硼、氟化石墨、硫化植物油、MoDTC、MoDTP、ZnDTP或亚磷酸酯)与2重量％的表面活性剂(非离子系)与水预先混合以后才添加入。
被膜处理，包登摩擦试验和后方冲孔试验均与实施例4～10同样地进行。
将以上试验结果示于表1～表3。由表1～表3可知，使用本发明的金属材料塑性加工用润滑剂组合物的实施例1～34以简便的作业即可发挥极优的润滑性。另一方面，在本发明的范围以外的，无法满足本发明构成条件的比较例1～6则没能同时满足优异的润滑性和简便的作业性。又，比较例7的磷酸盐被膜虽显示与本发明同等的润滑性，但工艺太多，不能采用简便的设备。
另外，对表1～表3中使用的各成份作如下的说明。
酚树脂：使酚-酚醛清漆进行氨基化并使其成水溶化物(分子量500～6000)
聚氨酯树脂：将分子量1000的聚乙二醇与六亚甲基二异氰酸酯进行加聚得到的物质(分子量50000或以上)
丙烯酸树脂：丙烯酸、甲基丙烯酸甲酯和丙烯酸正丁酯的共聚物。分子量15万或以上。使用表面活性剂：聚氧化乙烯烷苯基醚
PVA：聚乙烯醇(分子量1000)
PE蜡(聚乙烯乳胶蜡)：由乙烯的乳化聚合制造(分子量16000～20000)
PTFE(聚四氟乙烯蜡)：住友3-M制
StCa分散液(硬脂酸钙分散液)：中京油脂制
棕榈油乳胶：用聚氧化烯烷苯基醚分散棕榈油
硫化植物油：日本油脂制
亚磷酸酯：界化学制
添加剂2(固体润滑剂或极压添加剂)，均以聚氧化烯烷苯基醚分散。
另外，各成份的重量％表示成份本身的重量％。因此例如，水分散液的情况时，不包含水或用于分散的表面活性剂在内。
表1  实施例1～3，比较例1、2
                   内  容  成  份     涂布 水溶性无机盐/合成树脂                   试验结果
水溶性无机盐 合成树脂 添加剂 被膜量(g/m2) 包登   后方冲孔
  成分   重量％   成份 重量％ 成份 重量％     成份   平均摩擦系数  热胶着次数  良好冲孔深度(mm)
  实施例   1   钨酸钠     2   酚树脂   4  -   硬脂酸钙粉末   0.50     8.2   0.15   625    -
  2   钼酸钠     4   酚树脂   6  -   硬脂酸钙粉末   0.67     7.1   0.13   482    -
  3   四硼酸钾     4   酚树脂   6  -   硬脂酸钙粉末   0.67     7.0   0.13   523    -
  比较例   1   钨酸钠   9.5   酚树脂   1  -   硬脂酸钙粉末   9.5     8.1   0.18   212    -
  2   钨酸钠   0.5   酚树脂   4  -   硬脂酸钙粉末   0.13     8.7   0.15   128    -
酚树脂：对酚-酚醛清漆氨基化并使其水溶化(分子量500～6000)
聚氨酯树脂：将分子量1000之聚乙二醇与六亚甲基二异氰酸酯予以加成聚合者(分子量50000或以上)
丙烯酸树脂：丙烯酸、甲基丙烯酸甲酯、丙烯酸正丁酯的共聚物，分子量15万式以上使用表面活性剂：聚氧化乙烯烷基苯基醚
PVA：聚乙烯醇(分子量1000)
PE蜡(聚乙烯乳胶蜡)：由乙烯进行乳化聚合制造(分子量16000～20000)
PTFE(聚四氟化乙烯蜡)：住友3-M制
StCa分散液(硬脂酸钙分散液)：中京油脂制
棕榈油乳胶：以聚氧化烯烷基苯基醚分散棕榈油
硫化植物油：日本油脂制
亚磷酸酯：界化学制
Mo-DTC：二硫代胺基甲酸钼
Mo-DTP：二硫代磷酸钼
Zn-DTP：二硫代磷酸锌
添加剂2是均以聚氧化烯烷基苯基醚分散。
表2  实施例4～17、比较例3～7
                                  内  容  成  分 水溶性无机盐/合成树脂                    试验结果
  水溶性无机盐        合成树脂      添加剂1(润滑材料)       添加剂2 被膜量(g/m2)          包登 后方冲孔良好冲孔深度(mm)
成份  重量％ 成份 重量％ 成份 重量％ 成份 重量％   平均摩擦系数  热胶着次数
  实施例     4     钨酸钠   3     酚树脂     1     PE蜡     5  -     3     8.7     0.08     635     44
    5     钨酸钠   3     PVA     1     PE蜡     3  -     3     9.1     0.09     425     44
    6     钨酸钠   6     聚氨酯树脂     2     PE蜡     5  -     3     11.8     0.07     823     44
    7     钼酸钠   3     酚树脂     1     PE蜡     3  -     3     9.2     0.09     740     44
    8     四硼酸钠聚氨   3     酚树脂     1     StCa分散液     3  -     3     10.2     0.08     735     44
9 钒酸钾   3     酚树脂     1     StCa分散液     5  -     3     10.1     0.07     631     44
    10     硫酸钾   3     丙烯酸树脂     1     StCa分散液     3  -     3     9.7     0.08     688     44
    11     四硼酸钠   3     聚氨酯树脂     1     PE蜡     5  -     3     9.0     0.09     688     44
    12     四硼酸钠   3     聚氨酯树脂     3     PE蜡     5  -     1     12.2     0.08     823     44
    13     四硼酸钠   3     聚氨酯树脂     8     PE蜡     5  -     0.38     11.1     0.07     888     44
    14     四硼酸钠   2     聚氨酯树脂     1     StCa分散液     3  -     2     8.8     0.09     510     44
    15     四硼酸钾   3     聚氨酯树脂     5     StCa分散液     3  -    0.60     8.5     0.09     635     44
    16     四硼酸钾   3     聚氨酯树脂     1     PTFE     5  -     3     12.3     0.07     912     44
    17     四硼酸钾   8     聚氨酯树脂     1     棕榈油乳胶     3  -     8     9.5     0.08     823     44
  比较例     3     钨酸钠  9.5     酚树脂     1     PE蜡     3  -     9.50     9.1     0.18     158     40
    4     钨酸钠  0.5     PVA     4     PE蜡     3  -     0.13     10.4     0.12     210     36
    5     钨酸钠   3      -     PE蜡     5  -     -     8.2     0.21     112     28
    6        -     聚氨酯树脂     3     PE蜡     5  -     -     9.7     0.11     69     20
7   磷酸锌薄膜处理日本Parkelizing公司制Parbond：181X(浓度90g/l)处理条件：浸渍80℃，10分钟 反应皂润滑处理日本Parkelizing公司制Poloob2 35(浓度70g/L)处理条件：浸渍80℃，5分钟 化学被膜重量5.8金属皂量2.3热溶皂量2.5     0.10     409     44
表3  实施例18～34
                             内  容  成  分 水溶性无机盐/合成树脂                    试验结果
      水溶性无机盐     合成树脂 添加剂1(润滑材料)          添加剂2 薄膜量(g/m2)         包登 后方冲孔良好冲孔深度(mm)
  成份 重量％     成份   重量％   成份 重量％   成份   重量％   平均摩擦系数   热胶着次数
  实施例   18   钨酸钠     3     酚树脂     1   PE蜡   3 二硫化钼     2     3.00     11.2     0.15     822     48
  19   钨酸钠     6     酚树脂     1   PE蜡   3 石墨     2     6.00     10.6     0.12     862     48
  20   钨酸钠     3     PVA     1   PE蜡   3 BN     2     3.00     11.2     0.17     685     44
  21   钨酸钠     7     PVA     1   PE蜡   3 氟化石墨     2     7.00     11.1     0.16     624     44
  22   钨酸钠     3     PVA     1   PE蜡   3 硫化油脂     1     3.00     9.8     0.11     612     44
  23   钨酸钠     3     PVA     1   PE蜡   3 MoDTC     1     3.00     9.2     0.14     741     44
  24   钨酸钠     3     PVA     1   PE蜡   3 MoDTP     1     3.00     9.1     0.15     618     44
  25   钼酸钠     2     丙烯酸树脂     1   PE蜡   3 ZnDTP     1     2.00     8.2     0.11     589     44
  26   四硼酸钾     6     丙烯酸树脂     1   PE蜡   3 二硫化钼     2     6.00     11.5     0.16     854     48
  27   钒酸钾     6     丙烯酸树脂     1   PE蜡   3 二硫化钼     2     6.00     11.7     0.17     727     48
  28   硫酸钾     6     丙烯酸树脂     1   PE蜡   3 二硫化钼     2     6.00     10.7     0.16     818     48
  29   四硼酸钠     3     聚氨酯树脂   3   PE蜡   3 石     2     1     10.3     0.12     623     48
30 四硼酸钠 3 聚氨酯树脂 3 PE蜡 3 二硫化钼 2 1 9.2 0.11 624 48
  31   四硼酸钠     3     聚氨酯树脂   3   PE蜡   3 氮化硼     2     1     10.3     0.12     521     48
  32   四硼酸钠     3     聚氨酯树脂   3   PE蜡   3 亚磷酸酯     2     1     9.3     0.08     812     44
  33   四硼酸钠     3     聚氨酯树脂   3   PE蜡   3 MoDTC     1     1     10.8     0.10     441     44
  34   四硼酸钠     3     聚氨酯树脂   3   PE蜡   3 ZnDTP     1     1     9.3     0.08     452     44
[发明之效果]
由以上说明可知，使用本发明的金属材料塑性加工用润滑剂组合物时可用简便的处理即可形成具有极优润滑性的被膜。又，无废弃物，所以作业环境极佳。
[附图的简单说明]
附图表示使用本发明的塑性加工用润滑剂组合物进行后方冲孔试验的概要。

Claims (8)

1.一种金属材料的塑性加工用润滑剂，其特征为，它含有(A)合成树脂、(B)水溶性无机盐和水，(B)与(A)的固体成份重量比为0.25/1～9/1，且合成树脂为溶解或分散于其中者。
2.如权利要求1所述的金属材料的塑性加工用润滑剂，其中含有1～20重量％的一种或二种或以上选自金属皂、蜡、聚四氟乙烯和油的物质作为润滑材料。
3.如权利要求1或2所述的金属材料的塑性加工用润滑剂，其中水溶性无机盐为一种或二种或以上选自硫酸盐、硼酸盐、钼酸盐、钒酸盐及钨酸盐。
4.如权利要求1-3中任一项所述的金属材料的塑性加工用润滑剂，其中合成树脂为一种或二种或以上选自聚乙烯醇、聚乙烯吡咯烷酮、丙烯酸树脂、乙酸乙烯树脂、环氧树脂、聚氨酯树脂和酚系树脂。
5.如权利要求1所述的金属材料的塑性加工用润滑剂，其中含有0.3～10.0重量％固体成份的成份(A)聚氨酯树脂，和1.0～10.0重量％成份(B)的硼酸盐，还含有润滑材料。
6.如权利要求5所述的金属材料的塑性加工用润滑剂，其中含有1～20重量％一种或二种或以上选自金属皂、蜡、四氟乙烯和油的物质作为润滑材料。
7.如权利要求1-6中任一项所述的金属材料的塑性加工用润滑剂，其中含有1～20重量％一种或二种或以上选自二硫化钼、石墨、氮化硼、云母和氟化石墨的物质作为固体润滑剂。
8.如权利要求1-7中任一项的金属材料的塑性加工用润滑剂，其中含有0.5～5重量％一种或二种或以上选自硫系极压添功剂、有机钼系极压添加剂、磷系极压添加剂和氯系极压添加剂的物质作为极压添加剂。
CNB991097157A 1998-06-09 1999-06-09 金属材料的塑性加工用润滑剂 Expired - Fee Related CN1148437C (zh)

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