CN108350385A - 基于脂肪酸和脂肪酸甘油酯的粉末润滑剂及其用途 - Google Patents

基于脂肪酸和脂肪酸甘油酯的粉末润滑剂及其用途 Download PDF

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CN108350385A
CN108350385A CN201680064122.4A CN201680064122A CN108350385A CN 108350385 A CN108350385 A CN 108350385A CN 201680064122 A CN201680064122 A CN 201680064122A CN 108350385 A CN108350385 A CN 108350385A
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weight
powder
component
aliphatic acid
triglycerides
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CN108350385B (zh
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G·J·奥丁克
A·钦舒乐
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Henkel AG and Co KGaA
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Abstract

本发明提供粉末形式的干燥润滑剂组合物，其特别适用于以深拉伸方法生产铝罐，其中所形成的铝罐立即被进一步加工以产生薄的无机和/或有机保护涂层。所述润滑粉末基于脂肪酸的碱金属盐和脂肪酸甘油酯的混合物。本发明还包括所述润滑粉末用于铝的冷成型的用途以及用于铝罐的深拉伸的方法。

Description

基于脂肪酸和脂肪酸甘油酯的粉末润滑剂及其用途
本发明提供粉末形式的干燥润滑剂组合物，其特别适用于以深拉伸方法生产铝罐，其中所形成的铝罐被立即进一步加工以产生薄的无机和/或有机保护涂层。所述润滑粉末基于脂肪酸的碱金属盐和脂肪酸甘油酯的混合物。本发明还包括所述润滑粉末用于铝的冷成形的用途以及铝罐的深拉伸方法。
在罐生产行业中，铝平板(aluminium flat)的深拉伸是成熟的方法。在这种深拉伸方法中，有必要补偿铝材料和成型工具(例如，由硬钢或碳化钨制成的冲头和模具)在接触区域处的摩擦。已知有大量的基于金属皂的组合物被用于支持金属的冷加工。润滑组分通常被分散或溶解在液体载体中，因此可形成低粘度液体或较粘稠的糊剂。对于所述成型工具和待成型的金属之间的摩擦的有效补偿至关重要的是，在冷成型方法期间可以形成具有高度均匀性和完整性的薄润滑膜。因此，润滑剂的均匀施加是实现成功润滑的首要前提条件。尽管具有润滑性质的物质本身是众所周知的，但是当被包含在液体载体中时，难以均匀地施加这些物质。此外，为了避免由于挥发性液体的闪蒸造成的金属内缺陷，在冷成型步骤之前基本上除去所有的挥发性物质是重要的。另一方面，在室温下大多为固体的润滑物质常常引起环境问题或本身是有害的。因此，不仅需要改进润滑性能，而且还需要改进可施加性(applicability)，以及降低进行冷成形所需的润滑材料的量，以满足工业规格要求。另一个问题在于除去成型的金属表面上润滑膜的残余。取决于润滑剂组合物的类型以及在冷成型步骤之后进一步的方法步骤，例如涂漆，去除方法可能本质上不同并可以从纯物理处理方法到几乎纯化学处理方法中选择。
例如，EP 0638116B公开了一种用于铝的金属加工的液体润滑剂组合物，其在惰性挥发性液体有机载体中包含饱和脂族一元醇。在将铝平板浸入到液体润滑剂组合物中之后，将湿膜干燥，从而获得薄的润滑膜，其在冷成型步骤之后可退火除去。
US 2012/0302472 A1公开了适用于等速万向节轴、滚动轴承和变速箱的基于木质素磺酸钙的防水润滑脂，其另外包含钙皂和作为液体载体的基础油。
基于该现有技术，本发明的目的在于提供适用于铝部件的深拉伸的润滑剂，其可容易地施加，同时需要较少量的润滑剂材料来支持所述深拉伸方法。进一步的必要性来自于这样的事实，即深拉伸的铝部件通常涂覆有保护层，因此在冷成型方法之后必须要清洁。因此，本发明的适用的润滑剂还应具有使用常规含水清洁剂可容易地从金属表面被去除的性质。
所述问题通过一种润滑粉末得到了解决，其包含
a)多于60重量％的至少一种脂肪酸的碱金属盐，
b)至少一种脂肪酸单酸甘油酯、甘油二酯或甘油三酯，
其中根据组分a)的化合物与组分b)的化合物的重量比不高于30。
这样的润滑粉末表现出了优异的润滑性，特别是在铝的深拉伸中，如由圆盘形铝板成型圆柱形罐。这种深拉伸可以用相对少量的润滑剂来完成。此外，由粘附于冷成型的制品表面的润滑粉末所产生的固体可以容易地通过用含水清洁剂漂洗而去除。
另一个优点在于本发明的粉末可通过常规手段，例如振动和翻滚，而施加于金属平板上。在施加足以支持后续深拉伸方法的粉末涂层的所述过程中，可以显著降低在摩擦和磨损作用于金属平板时所形成的金属粉尘。金属粉尘的减少对于减少材料损失以及确保呼吸空气中最低的金属粉尘颗粒含量是有利的。另一方面，金属粉尘的减少也降低了粘附在粉末涂层上的松散金属颗粒的量，其通常会在深拉伸时造成金属部件表面划痕，并从而导致冲压工具的寿命缩短。
根据本发明的粉末应理解为包含至少一种粉状固体的固体混合物，所述固体混合物适于倾倒。当基于所述固体混合物，软化点低于25℃的粉状固体的含量低于5重量％时，包含至少一种粉状固体的固体混合物通常适于倾倒。本发明的粉末可以容易地通过振动或翻滚包含所述粉末和金属部件的容器而粘附到金属部件上。在优选的实施方案中，由固体颗粒构成的润滑粉末的D50值小于100μm，优选小于60μm。然而，为了确保在冷成型方法中形成具有高度均匀性和完整性的润滑膜，所述润滑粉末的D50值为至少1μm，优选至少5μm，更优选至少10μm。D50值是指所述粉末的总固体颗粒的50体积％具有低于给定值的直径。D50值可以通过用静态光衍射法测量的累积粒度分布来得到和通过筛分分析来测量粒径大于60μm的固体部分。
根据组分a)的碱金属盐优选选自锂盐、钾盐和/或钠盐，更优选选自钠盐。
关于组分a)，通常优选本发明的润滑粉末包含C10-C22脂肪酸，更优选具有不多于一个不饱和碳-碳双键的C10-C22脂肪酸，甚至更优选饱和C10-C22脂肪酸，特别优选碱金属硬脂酸盐。
在本发明的上下文中，C10-C22或C14-C20脂肪酸在不包括构成羧基官能团的碳原子的最长烷基链中含有10-22或14-20个碳原子。
在本发明的润滑粉末中，根据组分a)的化合物的量优选为至少70重量％，更优选至少75重量％，甚至更优选至少80重量％，以便得到具有高效率的粉末。组分a)的量仅受限于根据组分b)的脂肪酸甘油酯的必须的量和有助于润滑粉末总体性能的任选添加剂，使得根据组分a)的化合物的量优选低于95重量％，更优选低于90重量％，基于粉末的总组成。
一定量的脂肪酸甘油酯是必须的，以确保一定量的粉末粘附到金属部件上，并在深拉伸方法期间足以形成润滑膜。此外，某些脂肪酸甘油酯的存在也有助于在深拉伸方法条件下形成强烈均化的润滑膜，特别是当含有组成润滑剂的常规添加剂时。由于本发明的粉末形成均匀的润滑涂层，因此该行为额外地支持了所述润滑粉末的性质并在深拉伸条件下表现出优异的润滑性能，防止待成型金属与成型工具的熔合。然而，随着脂肪酸甘油酯相对用量的增加，粉末变得过于易粘，因为粉末颗粒趋于团聚，使得粉末与金属部件的粘附性变差。因此，在优选的实施方案中，在本发明的粉末中的根据组分a)的化合物与根据组分b)的化合物的重量比为至少6，更优选至少8。
通常，根据所述润滑粉末的组分b)的至少一种脂肪酸单酸甘油酯、甘油二酯或甘油三酯也包括其衍生物，只要该衍生物由通过酯化与脂肪酸主链连接的甘油构成即可。因此，每当在本文中提及根据组分b)的脂肪酸甘油酯时，所述衍生物通过定义被包括在内。在润滑粉末的优选实施方案中，根据组分b)的化合物选自脂肪酸甘油二酯或甘油三酯，更优选脂肪酸甘油三酯。
更优选地，本发明的润滑粉末包含根据组分b)的化合物，所述化合物选自基于C10-C22脂肪酸，更优选基于C14-C20脂肪酸的单酸甘油酯、甘油二酯或甘油三酯，而所述甘油酯的碘值优选为50-130，更优选70-95。
本发明上下文中的碘值是通过每100克相应的甘油酯或甘油酯混合物的加成反应消耗的碘的量(克)而表征的脂肪酸甘油酯中碳-碳双键的量。根据DIN EN 14111：2003-10，所述碘值可以通过溶解在氯仿中的样品的碘量分析来测量，其通过添加过量的Wijs溶液(一氯化碘/乙酸)进行，其中过量的碘通过用硫代硫酸盐标准溶液进行氧化还原滴定来测定。
关于本发明的润滑粉末中脂肪酸甘油酯的绝对量，优选至少2重量％，更优选至少4重量％，甚至更优选至少6重量％的根据组分b)的化合物，优选地根据组分b)的化合物选自甘油三酯，更优选基于C10-C22脂肪酸的甘油三酯，甚至更优选基于C14-C20脂肪酸的甘油三酯，各自基于所述粉末的总组成，而对于每种选定的甘油三酯，碘值为50-130，优选70-95。然而，当组分b)的量过度增加时，可以观察到粉末在铝部件表面的粘附性变差。因此，组分b)的量优选不超过20重量％，更优选不超过15重量％，基于粉末的总组成。
特别优选地，本发明的润滑粉末的组分b)由基于烷氧基化的，优选乙氧基化和/或丙氧基化的脂肪酸的甘油三酯组成，其中烷氧基化度至少为20，更优选至少30，但是不超过50，这些甘油三酯优选基于C10-C22脂肪酸，更优选基于C14-C20脂肪酸，每种甘油三酯的碘值都优选为50-130，更优选70-95。在这方面，对于粉末对金属部件的粘附性和润滑性质更为有利的是，组分b)另外包含基于非烷氧基化脂肪酸的甘油三酯，其碘值为50-130，更优选70-95，这些甘油三酯同样优选基于C10-C22脂肪酸，更优选基于C14-C20脂肪酸。
为了充分利用基于烷氧基化脂肪酸的这些甘油三酯的存在，对通过常规施加方法(如翻滚)粘附到金属部件上的润滑粉末的量产生积极作用，优选基于根据组分b)的化合物的总量，烷氧基化甘油三酯的总比例为至少20重量％，优选至少40重量％，更优选至少60重量％。
本发明的润滑粉末本身也具有适用于作为基本配方的性质，可以向其添加其他组分以用于进一步提高润滑性能或赋予其他有益的性能，例如加工的金属部件的可清洁性或例如粉末自身形成粉尘的倾向降低。
为此，所述润滑粉末可另外包含至少一种碱金属木质素磺酸盐作为组分c)，其量优选为至少0.1重量％，至少0.2重量％，但优选小于5重量％，基于所述粉末的总组成。木质素磺酸盐来源于木质素的磺化，木质素是一种来源于木材的天然生物聚合物。因此，木质素磺酸盐是使用亚硫酸盐制浆(sulfite pulping)生产木浆的副产品。这些木质素磺酸盐进一步改善了粉末对金属部件的粘附性，从而提高了粉末施加的效率。
本发明的润滑粉末中的木质素磺酸盐的重均分子量优选为至少2,000g/mol，但优选不超过20,000g/mol，更优选不超过10,000g/mol。
组分c)的碱金属离子优选选自锂离子、钾离子和/或钠离子，优选选自钠离子。
此外，本发明的润滑粉末可另外包含作为组分d)的至少一种本领域技术人员已知为“极压添加剂(extreme pressure additive)”的化合物。这些添加剂在冷成型方法中在摩擦磨损(tribological wear)作用下会释放出选自硫和磷化合物的低分子量化合物，从而防止了待成型金属和成型工具的熔合。另外，发现了本发明上下文中的极压添加剂还有助于获得具有较小形成粉尘倾向的润滑粉末。在处理润滑粉末以施加到金属部件上时，减少粉尘的形成对于确保呼吸空气中的最低粉尘颗粒含量是有利的。作为组分d)的优选极压敏感物(extreme pressure sensitives)选自硫化物、多硫化物和/或二烷基二硫代磷酸酯，优选选自每个烷基链中具有不超过12个碳原子的二烷基二硫代磷酸酯，最优选选自每个烷基链都具有不超过12个碳原子的二烷基二硫代磷酸钠和/或二烷基二硫代磷酸锌。
在本发明的润滑粉末中，组分d)的量优选为至少1重量％，更优选至少2重量％，但优选不超过8重量％，更优选不超过5重量％，基于所述粉末的总组成。
本发明的粉末润滑剂还可以包含作为组分e)的少量通常作为溶剂使用的有机化合物。这些溶剂也可以有助于对金属部件的粘附性，但主要是有助于获得金属平板上所述粉末的均匀负载。大多数溶剂对通过湿法化学处理的深拉伸的金属部件的可清洁性也具有影响，因此只有少数溶剂是可以接受的。本发明上下文中的有机溶剂的分子量小于1,000g/mol。考虑到所有这些性质都受到溶剂存在的影响，优选润滑粉末另外包含作为组分e)的至少一种有机溶剂，其优选选自由选自氢、氧和碳的元素组成的有机化合物，并优选ET(30)值至少为158kJ/mol。令人惊讶地发现，当所述有机溶剂选自由选自氢、氧和碳的元素组成的有机化合物，且ET(30)至少为180kJ/mol，如具有不超过12个碳原子的单甘醇醚或二甘醇醚时，所述深拉伸的金属部件的可清洁性可得到改善。ET(30)值是溶剂极性的量度。所述值可以从溶解在相应溶剂中的Reichardt的吡啶鎓-N-苯酚甜菜碱染料(“甜菜碱30”)在25℃和1个大气压下的长波分子内电荷转移吸收带的光谱测量结果实验推导得到。
另外包含被脂肪酸酰化的亚烷基二胺的本发明的润滑粉末的一些具体实施方案对于减少特定深拉伸应用中的磨料磨损是有用的。因此可以优选向本发明的润滑粉末中添加作为组分f)的前述定义的根据组分a)的脂肪酸酰化的亚烷基二胺，最优选N，N′-亚乙基双(硬脂酰胺)。然而，基于本发明的润滑粉末的总组成，所述组分f)优选不超过20重量％，更优选不超过10重量％。
如已经指出的，只可以容许少量的有机溶剂，否则所述粉末会变得易粘且粘附性会变差。因此，根据组分e)的溶剂的量优选为至少1重量％，更优选至少2重量％，但优选小于10重量％，更优选小于8重量％，尤其优选小于5重量％，基于本发明粉末的总组成。
令人惊讶地发现，仅基于脂肪酸盐和脂肪酸甘油酯的粉末的润滑性足以用于深拉伸，并且不需要添加显著量的路易斯酸，如锌、铝或钙阳离子以增加润滑性。相反，含有大量多价阳离子如锌阳离子的这类粉末往往会导致难以从深拉伸铝部件上去除的润滑涂层，并因此与深拉伸的金属部件的工业客户的传统清洁方法相比，需要更强烈的清洁。为此，有利的是本发明的润滑粉末优选含小于5重量％，优选小于1重量％的锌阳离子，优选多价阳离子，基于所述粉末的总组成。
本发明的润滑粉末优选包含小于2重量％，优选小于1重量％，更优选小于0.1重量％的游离脂肪酸。
本发明的另一方面在于如本文所述的润滑粉末用于铝部件的冷成形，特别是用于铝的深拉伸的用途。
本发明的一个主要优点在于，与润滑液体或糊剂相比，所述润滑粉末材料具有高涂覆效率。该优点在下述方法中特别重要，在所述方法中，多种金属部件必须在短时间内用润滑组合物涂覆，例如在饮料罐生产工业中。
因此，本发明还包括一种生产铝罐的方法，其包括以下步骤：
a)将多个铝平板和本发明的润滑粉末置于一个容器中，优选筒中，其中所述润滑粉末的量优选每平方米的铝平板表面不超过20克，更优选不超过10克，但优选至少为1克；
b)振动或翻滚所述容器，优选筒体，以便用粉末润滑剂的润滑膜涂覆所述铝平板；
c)通过冲压，优选冲击挤出将所述铝平板深拉伸成罐；并任选地
d)对所述铝罐进行清洁和脱脂，优选使用基于水的清洁剂。
在该方法的优选实施方案中，所述罐呈圆柱形，且所述铝平板呈盘状。
实施例：
将本发明的不同粉末润滑剂(表1)施加于铝盘上，然后通过冲击挤出形成圆柱形薄壁铝罐。
通过翻滚特定量的润滑剂粉末，将润滑剂的薄层施加到直径为74mm且厚度为6mm的铝盘的表面上，使得每平方米铝盘的理论负载为7.8g。所述翻滚在15-22rpm下进行20分钟。
随后对经过润滑的圆盘进行冲击挤出以形成具有给定圆柱轴长度L和壁厚W的罐(L＝259mm；W＝0.74mm)的罐体。对于这种特定类型的冷成型，使用了水平冲击挤出机。冲头和模具由碳化钨制成。表1中的每种润滑剂粉末都得到了成功的冲压，从而得到了没有材料损坏的所需形状，且没有观察到壁厚的显著起伏。
表2显示了对于所有粉末润滑剂均实现了粉末与铝盘的合理的良好粘附。然而，很明显，基于锌的脂肪酸盐的润滑剂在翻滚后显示出最差的负载以及最差的冲压后铝罐的可清洁性(参见V1)。硬脂酸钠与脂肪酸甘油酯的组合使用总是能够产生高于80％的良好负载(参见E1-E4)。可清洁性仍取决于是否存在溶剂和所使用溶剂的类型，而含有ET(30)值高于180kJ/mol的二乙二醇单丁醚的润滑剂易于用弱碱性清洁剂清洁(参见E2vs E3)。相同的溶剂也有利于获得施加了粉末的圆盘的非常均匀的外观(参见E2vs E1)。
表2测试结果
1基于翻滚之前和之后的20Al盘的重量差测定
2在70℃下浸渍碱性清洁(8重量％Bonderite CAK 509；Fa.Henkel AG)2min：
⊙：差，有显著量的残留粉末
X：困难，一定量的残留粉末
+：容易，没有残留粉末
3在施加粉末的盘与其壳从10cm的高度坠落在黑色的金属板上之后目测评价
⊙：差，大多数粉末掉落
X：足够，有一些粉末掉落
+：良好，几乎没有粉末掉落
4在翻滚后评价
⊙：显著
X：可见
+：不可见
5翻滚后目视评价污点的直径
L：大(＞10mm)
M：中等(5-10mm)
SM：小至中等(2-5mm)
S：小(＜2mm)

Claims (15)

1.润滑粉末，其包含
a)多于60重量％的至少一种脂肪酸的碱金属盐，
b)至少一种脂肪酸的单酸甘油酯、甘油二酯或甘油三酯，
其中，根据组分a)的化合物与组分b)的化合物的重量比不高于30。
2.根据权利要求1所述的粉末，其中根据组分a)的化合物与根据组分b)的化合物的重量比至少为6，优选至少为8。
3.根据前述权利要求中一项或两项所述的粉末，其中至少一种脂肪酸的盐选自C10-C22脂肪酸，优选选自具有不超过一个不饱和碳-碳键的脂肪酸，更优选选自饱和的脂肪酸，特别优选选自硬脂酸盐。
4.根据前述权利要求中任一项所述的粉末，其中基于所述粉末的总组成，根据组分a)的化合物的量为至少70重量％，优选至少75重量％，但优选低于95重量％，更优选低于90重量％。
5.根据前述权利要求中任一项所述的粉末，其中组分b)选自甘油二酯或甘油三酯，更优选选自甘油三酯。
6.根据前述权利要求中任一项所述的粉末，其中组分b)选自基于C10-C22脂肪酸，优选基于C14-C20脂肪酸的单酸甘油酯、甘油二酯或甘油三酯，所述甘油酯的碘值优选为50-130，更优选为70-95。
7.根据前述权利要求中任一项所述的粉末，其中组分b)包含基于烷氧基化的、优选基于乙氧基化和/或丙氧基化的脂肪酸的甘油三酯，其中烷氧基化度至少为20，更优选至少30，但不超过50。
8.根据权利要求7所述的粉末，其中组分b)另外包含基于非烷氧基化的脂肪酸的甘油三酯，所述甘油三酯的碘值为80-100g I2/100g。
9.根据权利要求7或8中一项或两项所述的粉末，其中基于根据组分b)的化合物的总量，烷氧基化的甘油三酯的总比例为至少20重量％，优选至少40重量％，更优选至少60重量％。
10.根据前述权利要求中任一项所述的粉末，其中基于所述粉末的总组成，根据组分b)的化合物的量，优选根据选自甘油三酯的组分b)的化合物的量，更优选基于C10-C22脂肪酸的甘油三酯的量，甚至更优选基于碘值为50-130，优选碘值为70-95的C10-C22脂肪酸的甘油三酯的量为至少2重量％，优选至少4重量％，更优选至少6重量％，但优选不超过20重量％，更优选不超过15重量％。
11.根据前述权利要求中任一项所述的粉末，其中另外包含至少一种碱金属木质素磺酸盐作为组分c)，基于所述粉末的总组成，其量优选为至少0.1重量％，至少0.2重量％，但优选小于5重量％。
12.根据前述权利要求中任一项所述的粉末，其中另外包含至少一种极压添加剂作为组分d)，其优选选自二烷基二硫代磷酸酯，更优选选自二烷基二硫代磷酸钠和/或二烷基二硫代磷酸锌，其中在每个烷基链中具有不超过12个碳原子，基于所述粉末的总组成，所述极压添加剂的含量优选为1-8重量％，更优选2-5重量％。
13.根据前述权利要求中任一项所述的粉末，其中另外包含至少一种有机溶剂作为组分e)，所述有机溶剂优选选自由选自氢、氧和碳的元素组成的有机化合物，优选地ET(30)值至少为180kJ/mol，基于所述粉末的总组成，组分e)的含量优选为至少1重量％，更优选至少2重量％，但优选小于10重量％，更优选小于8重量％，特别优选小于5重量％。
14.根据前述权利要求中任一项所述的润滑粉末用于铝部件的冷成型的用途。
15.生产铝罐的方法，其包括以下步骤：
a)将多个铝平板和根据权利要求1-13中任一项所述的润滑粉末放置到一个容器中；
b)振动或翻滚所述容器，以便用粉末润滑剂的润滑膜涂覆所述铝平板；
c)通过冲压将所述铝平板深拉伸成罐；以及任选地
d)对所述铝罐进行清洁和脱脂，优选使用基于水的清洁剂。
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