CN1088968A - 用于已成型金属表面的改进表面调理剂 - Google Patents

用于已成型金属表面的改进表面调理剂 Download PDF

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Publication number
CN1088968A
CN1088968A CN93118616A CN93118616A CN1088968A CN 1088968 A CN1088968 A CN 1088968A CN 93118616 A CN93118616 A CN 93118616A CN 93118616 A CN93118616 A CN 93118616A CN 1088968 A CN1088968 A CN 1088968A
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Prior art keywords
composition
fatty acid
ethoxylated
lubricant
ethoxylation
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CN93118616A
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English (en)
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沙米·B·阿瓦德
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Henkel Corp
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Henkel Corp
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Priority claimed from US07/492,695 external-priority patent/US5030323A/en
Application filed by Henkel Corp filed Critical Henkel Corp
Publication of CN1088968A publication Critical patent/CN1088968A/zh
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Abstract

将经酸或碱清洁的铝表面与一种水基组合物接 触干燥后，铝表面的摩擦力降低，但不降低其可印性 和漆涂层粘合力，并去除在清洁过程或清洁浸渍之后 可能在铝表面上产生的棕色污点。所述组合物包括 (i)乙氧基化的磷酸酯，(ii)铝、锆、铁、锡和/或铈的 离子，(iii)一种金属侵蚀成分等的混合物。

Description

本申请是1990年3月13日提出的共同待批的申请序号492，695的部分继续申请，后者是1989年8月18日提出的共同待批的申请序号395，620（现在的美国专利4，944，889）的部分继续申请，而申请号395，620是1987年6月1日提出的申请号57，129（现在的美国专利4，859，351）的部分继续申请。因此美国专利4，859，351说明书的全部内容被参考结合入本文。为了简便起见，这份专利通常简称“'351专利”。因此，在美国专利4，859，351中没有重复记载的申请号395，620（1989年8月18日申请）说明书的全部内容也被参考结合入本文。
除了在'351专利中指定的一般范围外，本发明的一个具体方案是特指组合物及其使用方法，这就可得到一种已处理过的成形金属表面，该金属表面在润湿时大体上或完全没有“水膜残迹”，换句话说，在此表面上的全部水都可自发地铺展于该表面上。本发明的另一个具体方案是特指适用于与已成形金属表面接触的含水组合物，这种组合物在干燥后在其上沉积一种运动性提高的润湿剂膜，所述组合物在贮存期间防止由微生物作用引起的变质和/或在使用时防止起泡。
除了在'351专利中已记载的现有技术外，1979年4月10日授予Kelly的美国专利4，148，670给出了一种用于铝的转变涂覆液，它含有锆和/或钛的化合物、氟化物和磷酸盐，及任选的以可溶解状态的多羟基化合物。所述的磷酸盐是通常的无机磷酸盐，并且指出，通过处理不能提高运动性。
1976年6月22日授予Das的美国专利3，964，936给出了一种用于铝的转变涂覆液，它含能产生一种即使经沸水处理时仍保持其光亮外观和抗变色的表面。这种涂覆液含有锆和氟的化合物，也可含有硼酸。既没有指出使用含磷组分，也没有指出经处理后提高运动性。
在本说明书中，除了在权利要求书和实施例中或在其他地方明确指出的外，在确定本发明的最宽范围时，所有描述成分量的或反应条件的数字都应理解为由词“大约”来修饰。在特别说明确切数量范围内的操作通常是优选的。同样，除了另有指明外，无论何时一种以上物质被理解为适合于某种组合物的某种特定组分，它被理解为包括所列举物质的任何两种或两种以上的混合物也同样是适宜的。
现在业已发现，一种已成形的铝表面通过与一种水基酸或碱性清洗剂充分接触通常已完全清洁和去油，可有效和有利地进行表面调理，以便赋予该表面提高的运动性，即较低的静态表面摩擦系数，当经过随后的干燥时，对已处理过的表面不会损伤漆的反射性或可印性或附着性，具体方法是将该表面与一种组合物接触，这种组合物包含，或最好基本上由水和下列组分构成：
（A）一种水溶性组分，它选自符合化学通式Ⅰ的物质，
其中，R1、R3和R6分别选自氢或含有1-4个碳原子的烷基，较使是选自氢和甲基，最佳是选自氢;X、Y和Z各是一个整数并分别选自0-25;及R2、R4和R5分别选自氢、一价阳离子、多价阳离子的一价部分、含有1-20个碳原子的烷基和含有1-20个碳原子的芳基和芳烷基;只是在该式中至少R2、R4和R5中的一个，（ⅰ）不是氢和（ⅱ）至少有一个烷氧基键合在它和磷原子之间;
（B）一种选自水溶性盐类的组分，这种盐含有包括选自Fe、Zr、Sn、Al和Ce原子的离子;
（C）一种金属浸蚀组分，它较佳是选自硝酸，硫酸，磷酸，氢氟酸，氢氯酸，氢溴酸，氢碘酸，硫酸和磷酸的酸式盐，硝酸、硫酸、磷酸、氢氟酸、氢氯酸、氢溴酸和氢碘酸与碱生成的盐，这种碱的离子化产物常数低于与其作用生成盐的酸的离子化产物常数，以及任何这些物质的混合物;并且任选，
（D）一种选自符合通式Ⅱ的组分，
Figure 931186161_IMG2
其中，R7是一个直链的、环状的或支链的饱和一价脂族烃部分，它含有1-25个，较佳是4-20个碳原子;X是选自氢、卤素或苯基和R1;S是一个1-50的整数，较佳是1-20;并且R1的含义与通式Ⅰ相同;
（E）一种选自符合通式Ⅲ的组分，
Figure 931186161_IMG3
其中，R8是一个直链的、环状的或支链的饱和一价脂族烃部分，它含有4-25个，较佳是8-12个，最佳是9个碳原子;（C6H4）是一个邻位、间位或对位亚苯基环;并且R1和S的含义与通式Ⅱ相同;
（F）一种选自用于含有组分（B）离子的金属的螯合剂组分，它较佳是选自分子，包括聚合物分子，每个分子至少有两部分是选自含氨基、取代氨基、羧基、膦酸盐、磺酸盐和羰基部分;
（G）一种选自符合通式Ⅳ的组分，
Figure 931186161_IMG4
其中，R10是一个直链或支链的饱和或不饱和一价脂族烃部分，它含有1-25个，较佳是4-20个碳原子;并且R1和X的含义与通式Ⅰ相同。
应当指出的是，并不是所有指定的组分必须是独立的物质。例如氟锆酸（即H2ZrF6）既可用作组分（B），又可用作组分（C）。
对于组分（A）的较佳选择是选择符合通式Ⅰ的分子，此时X和Z各是O，并且R2和R5各是氢或一种阳离子或阳离子部分，而且这类物质可用作全部组分（A）、（B）和（C），例如如果R2是氢及R6是（1/3）Fe+3。
依据本发明的这种具体方案，在用于处理溶液中的组分（A）的量较佳是浓度达到每升有0.00001-0.0032克原子磷，或最佳是每升有0.0005-0.0015克原子磷。依据本发明的这种具体方案，用于处理溶液中的组分（B）的量也可独立地优选这样的浓度，即每升有0.00001-0.01克原子的在组分（B）中列举的全部金属原子，或最佳是0.0001-0.003克原子。
组分（A）可独立地优选自按照通式Ⅰ的分子，此时（ⅰ）X或是O或是不低于R2中碳原子数的0.5倍;（ⅱ）Y或是O或是不低于R4中碳原子数的0.5倍;（ⅲ）Z或是O或是不低于R5中碳原子数的0.5倍。
不考虑其具体组成，在根据本发明的具体方案的方法中与一种已成形铝表面接触的组合物较佳是含有0.001-10%（重量）的上述全部组分（A）、（B）和（C），最好是0.005-0.05%（重量），并用任选组分和水达到平衡。所用的水不一定必须是去离子的或其他特殊纯化的;普通自来水通常也可得到令人满意的结果。在与一种已成形铝表面接触期间，组合物的pH值的较佳范围是1-8，最佳范围是2-5。pH值可依需要调节，使用中最好用硝酸和/或硫酸，以保持pH值在所希望的范围内。在与已成形铝表面接触期间，组合物的温度较佳是10-85℃，最佳是21-54℃。接触方式可以是喷淋、浸渍或任何其他常规方法，或这些方法的混合。较佳的接触时间是5-60秒，最佳是20-30秒。在根据本发明处理后以及在进一步加工前，例如干燥、印刷、喷漆，或类似处理，通常较佳是先用自来水清洗处理过的表面，然后再用去离子水清洗。
与所有其他的选择无关，如果按照本发明的这种具体方案的一种组合物含有一定量的如上述定义的任选组分（D）和（E），而其量足以防止或至少基本上降低粗大的肉眼可发现的相分离趋势。则这种组合物是较佳的，相反，就会出现上述相分离趋势。业已发现，如在组合物中仅含有组分（A）至（C）和任选的如上述定义的组分（F）和（G），在该组合物配制成并使用某些时间后，则富集金属的相趋于从该组合物的残余物分离出来。较佳的是组分（D）和（E）的重量比范围是从3∶1至1∶3，或最佳范围是从1.7∶1至1∶1.4。单独来看，如果结合组分（D）和（E）与组分（A）的重量比范围在3.3∶1至1∶2是较佳的，或者在1.8∶1至1∶1.5是最佳的。
除了处理方法和直接用于处理的组合物外，本发明的另一个具体方案就是一种浓缩物，要用于处理的这种组合物可通过用水稀释浓缩物而制备。上述浓缩物最多含有上述组分（A）、（B）、（C）和上述任选的（D）、（E）、（F）和/或（G），其用量是上述直接用于处理金属表面组合物的百分重量的30-200倍。
本发明的这些具体方案的组合物和方法具有超过在'351专利中描述的几个优点：
-依据本发明处理后，一种表面可多次用自来水或去离子水清洗，与根据'351专利实施例处理的罐表面相比，不损失改进的表面运动性和其他优点;
-如果在已处理的表面和一种洗涤组合物之间长时间的接触或者在清洁后但在用本发明组合物处理之前进行一次漂洗（例如，由于高速生产线的非计划性停止），由浅至深的棕色斑点（认为是水合铝氧化物）常常在此处理过的表面形成;任何上述斑点可通过根据本发明的处理除去，然而采用'351专利实施例中教导的方法处理后，这些斑点通常仍存在;
-根据本发明的方法，在pH值低至足以抑制细菌生长时比按照'351专利实施例的方法更易操作;
-几乎任何易得的工业或自来水源都可用于配制或稀释本发明的组合物，而'351专利教导，为了达到最佳效果通常需要去离子水;
-根据本发明方法制备的表面很容易被水润湿并因而没有“水膜残迹”存在，而它是大多数铝罐制造者所不希望的;根据'351专利实施例处理的罐更可能有水膜残迹存在。
本发明的另一个具体方案包括上述详细描述的组合物及其使用和上述参考专利申请395，620和美国专利4，859，351中描述的组合物及其使用，这些组合物在贮存和/或使用期间防止微生物的破坏作用，和/或在制备和/或使用中防止起泡沫。
除了那些对提高组合物的运动性或稳定性有某些不利影响的外，任何抗微生物剂或杀生物剂都可如本文上面所述那样有益地以足以有效抑制生物生长的量加到该组合物中。过氧化氢通常是用于此目的最佳选择。如上所述，在含水浓缩组合物中，适合用大约99倍自身重量的水稀释，以配制随时可以直接用于金属的组合物，干燥后以提高运动性，过氧化氢的浓度范围从0.375至3.75%（重量）是较佳的。而浓缩范围在1.4-2.2%（重量）是最佳的。在更浓缩的组合物中，优选的杀生物剂浓度应当是由所希望的浓缩物的稀释度来确定。然而，一般说来，由于浓缩过氧化氢具有相对低的稳定性，如果要使用的话，较佳的是将该组分仅加入到一种足够稀的浓缩物中，使过氧化氢的浓度在配制该组合物时不超过3%（重量）。
除了对组合物的已描述的运动性提高或稳定性有某些不利影响的那些外，任何消泡剂都可按照本文的上述教导有益地以有效降低在制备和/或使用该组合物时所观察到的泡沫的量加到该组合物中。优选的消泡剂是蜡、低挥发性液体链烷烃和高分子量脂肪酸衍生物的结合。通常，硅氧烷类消泡剂不希望供本发明使用，因为它们会引起形成水膜残迹。通常相当于0.05-2%（重量）的消泡剂量是较佳的，而0.5-1%（重量）通常是最佳的。
对于按照本发明方法处理来说，保留了'351专利中描述的所有优点，即提高的运动性、低摩擦系数、高质量可印性和良好的漆附着力等等。
通过研究下列非限定性实施例可进一步理解本发明的实施。
实施例
实施例1-7的总条件和比较
在所有这些实施例中，处理过的表面是通用的已有最终形状和尺寸的铝饮料罐。这些饮料罐在pH为2的硫酸水溶液中、在温度54℃下进行30秒的酸预洗，然后用一种常规的碱性的含表面活性剂的洗涤剂，在pH为12.3和54℃下洗涤60秒，接着用自来水冲洗30秒，这些预处理都是在用本发明的组合物，如在下面具体实施例中给出的组合物处理之前。（在这些具体实施例中给出的组合物是本发明的浓缩物;为了处理，使用的是表1中指定的百分重量浓缩物的自来水溶液。）经过这种处理后，这些罐先在自来水中清洗30秒，然后在去离子水中清洗90秒，并在210℃下干燥。干燥后，按'351专利中记载的方法测量罐的静态表面摩擦系数。
实施例1
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
25%（重量）的四氯化锡水溶液  300
ETHFACTM136 400
ETHOXTMMI-14 100
25%（重量）的氟化氢铵水溶液  135
DEQUESTTM2010 25
水  9040
实施例2
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
25%（重量）的柠檬酸铁铵  300
水溶液
ETHFACTM136 400
ETHOXTMMI-14 100
25%（重量）的氟化氢铵水溶液  135
DEQUESTTM2010 25
水  9040
实施例3
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
硫酸铈铵  4
ETHFACTM136 30
25%（重量）的氟化氢铵水溶液  16
DEQUESTTM2010 2
硫酸  1
TRITONTMN101 5
水  942
实施例4
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
氯化铝  10
ETHFACTM136 50
25%（重量）的氟化氢铵水溶液  11
TRITONTMN101 6
柠檬酸  6
乙氧基化醇表面活性剂  11
水  906
实施例5
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
氟锆酸  15
一（己基三乙氧基）磷酸酯  70
聚（氧乙烯）异硬脂酸酯（每个硬脂酸酯单元有平均14个氧化烯单元）  20
25%（重量）的氟化氢铵水溶液  19
氨基乙酸  20
水  856
实施例6
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
氟锆酸  15
一（己基三乙氧基）磷酸脂  30
ETHOXTMMI-14 20
25%（重量）的氟化氢铵水溶液  15
丁烷-2-磷酸三羧酸酯  10
水  910
实施例7
本实施例的浓缩物具有下列组成：
成分  在组合物中的重量份数
氟锆酸  10
聚氧乙烯异硬脂酸酯（每摩尔硬脂酸酯有平均14摩尔的-C2H4O-基团） 10
TRITONTMH-66 80
DEQUESTTM2010 2.5
25%（重量）的氟化氢铵水溶液  4
水  893.5
在给出的上述组合物中，DEQUESTTM2010是一种物质的商品名，据报导它主要是1-羟基亚乙基-1-双膦酸，而TRITONTMN101是一种表面活性剂物质的商品名，据报导它主要是壬基苯氧基聚（乙氧基）乙醇，每个分子中平均有9-10个乙氧基基团。
表1给出所用浓缩物的具体含量、处理条件，以及通过吸着用于这些试样的润滑剂和表面调理层在这些罐上达到的静态表面摩擦系数。
表1
由本发明处理达到的表面摩擦系数的改进
实验编号  处理液中的  处理条件  静态表面
浓缩物的重量%  温度(℃)  时间(秒)  摩擦系数
1  1.0  35  20  1.27
2  1.0  35  20  1.47
3  1.0  35  20  1.31
4  1.0  35  20  0.77
5  1.0  35  20  0.77
6  1.0  35  20  1.20
7  1.0  35  20  1.01
未处理  1.67
实施例8
这是一个含有一种优选消泡剂和一种优选杀生物剂的组合物实例，但其他方面是按照'351专利的教导。
第一种浓缩物是通过混合880重量份数（“PBW”）的ETHOXTMMI-14、60PBW的COLLOID999TM（一种高分子量脂肪酸衍生物，可从Colloids，Inc.，394 Frelinghuysen Ave.，Newark，New Jetsey 07114，U.S.A买到）和60 PBW的GP-295TM消泡剂（一种约10%的固体蜡在白色矿物油中的悬浮液，可从Genese Polymers Corp.，Flint，Michigan 48507，U.S.A买到）制备的。ETHOXTMMI-14先在27-32℃下于混合槽中熔化。然后其他两种物质按给出的顺序加入并混合，以形成一种不透明的但肉眼观察均匀的无团块的液体。
第二种适于贮存至少几个月的浓缩物的制备是然后将47PBW的上述第一种浓缩物与917PBW的水，优选是去离子水，和40PBW的37.5%过氧化氢水溶液相混合物。这第二种浓缩物以后在需要制备适于直接处理铝表面的组合物时，通常如在'351专利中一般描述的那样可以稀释。
实施例9和10
这些实施例举出包括含金属的盐和乙氧基化磷酸酯的优选的稳定组合物。下表2中给出的组合物是浓缩物，例如在用50-200倍自身重量的自来水稀释后可适用于处理金属容器。
表2  实施例9和10的组合物
成分  在实施例中的重量份数
9  10
去离子水  920  856
ETHOXTM2684 14 60
TRITONTMDF-16 12 -
TRYCOLTMLF-1 4 30
IGEPALTMCO-880 11 30
DEQUESTTM2010 3 -
氟化氢铵(NH4F·HF) 11 4
氟锆酸(H2ZrF6) 25 20
在表2中以前未说明的成分来源和特性如下：ETHOXTM2684购买于Ethox Chemicals，Inc.，Greenville，South Carolina20606，USA，符合于式Ⅰ，式中X和Z都是O，R2、R3和R5都代表氢，R4代表一种C8-10的直链烷基混合物，而y平均是约15。TRITONTMDF-16，购买于Rohm& Haas，Philadelphia，Pennsylvania 19105，USA，据报导是一种改性聚氧乙基化直链醇。TRYCOLTMLF-1购买于the Emery Chemical Division of Henkel Corporation，Cincinnati，Ohio 45249，USA，据报导是一种烷基聚醚。IGEPALTMCO-880购买于GAF Corp，Wayne，New Jersey 07470，USA，据报导是一种乙氧基化壬基酚。

Claims (6)

1、一种方法，它包括下列步骤：用一中酸性或碱性洗涤水溶液清洁一种铝罐，干燥已洁净的罐，接着借助自动传送设备将已洁净并干燥过的罐送到一个进行喷漆或通过印刷进行装饰或二者都有的位置上，其中改进之处在于，在最后干燥上述外表面和自动传送之前，将所述罐的至少一个外表面与一种含有润滑剂和表面调理剂的组合物接触，该组合物中含有一定量的杀生物剂，它在贮存或使用时可有效地防止该润滑剂和表面调理剂组合物变质，由此在该罐表面形成一种膜，使干燥后的罐表面具有不大于1.5的静态摩擦系数，而且该系数也低于无上述膜层的同类型罐表面达到的静态摩擦系数。
2、根据权利要求1的方法，其中所述润滑剂和表面调理剂组合物是一种水溶液，该水溶液基本上由水、过氧化氢和可溶有机物组成，该有机物选自乙氧基化磷酸酯、乙氧基化醇、乙氧基化脂肪酸、乙氧基化羟基取代脂肪酸、乙氧基化脂肪酸盐、乙氧基化脂肪酸酰胺、乙氧基化羟基取代脂肪酸醚和乙氧基化脂肪酸酯、乙氧基化羟基取代脂肪酸盐、乙氧基化羟基取代脂肪酸酰胺、乙氧基化羟基取代脂肪酸醚和乙氧基化羧基取代脂肪酸酯以及其混合物。
3、根据权利要求2的方法，其中润滑剂和表面调理剂组合物的pH值在约1至约6.5之间，润滑剂和表面调理剂组合物含有一种消泡剂，其有效量在该方法中将泡沫量降到一较低的量，该量低于在同样使用一种润滑剂和表面调理剂、但其中水代替消泡剂的比较组合物时产生的泡沫量，并且可溶有机物选自乙氧基化脂肪酸、乙氧基化脂肪酸盐、具有至少4个碳原子的并含有每摩尔醇最多约20摩尔缩合环氧乙烷的乙氧基化醇、乙氧基化烷基醇的磷酸酯及其混合物。
4、根据权利要求1的方法，其中该润滑剂和表面调理剂组合物的pH值在约1至约6.5之间，该润滑剂和表面调理剂组合物含有一种消泡剂，其有效量在该方法中将泡沫降低到一较低量，该量低于在同样使用一种润滑剂和表面调理剂、但其中水代替该消泡剂的比较组合物时产生的泡沫量，并且可溶有机物选自乙氧基化脂肪酸、乙氧基化脂肪酸盐、具有至少4个碳原子并含有每摩尔醇最多20摩尔缩合环氧乙烷的乙氧基化醇、乙氧基化烷基醇的磷酸酯及其混合物。
5、根据权利要求4的方法，其中消泡剂是一种由固体蜡、液体石蜡和高分子量脂肪酸衍生物分子组成的混合物。
6、根据权利要求2的方法，其中消泡剂是一种由固体蜡、液体石蜡和高分子量脂肪酸衍生物分子组成的混合物。
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