CN1620523A - 用于处理金属的聚合物衍生物 - Google Patents
用于处理金属的聚合物衍生物 Download PDFInfo
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- CN1620523A CN1620523A CNA028280458A CN02828045A CN1620523A CN 1620523 A CN1620523 A CN 1620523A CN A028280458 A CNA028280458 A CN A028280458A CN 02828045 A CN02828045 A CN 02828045A CN 1620523 A CN1620523 A CN 1620523A
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- metal
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- polymkeric substance
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- LIBWRRJGKWQFSD-UHFFFAOYSA-M sodium;2-nitrobenzenesulfonate Chemical compound [Na+].[O-][N+](=O)C1=CC=CC=C1S([O-])(=O)=O LIBWRRJGKWQFSD-UHFFFAOYSA-M 0.000 description 1
- AIODYXCONSJORM-UHFFFAOYSA-N sodium;3-(3-sulfopropyldisulfanyl)propane-1-sulfonic acid Chemical compound [Na].OS(=O)(=O)CCCSSCCCS(O)(=O)=O AIODYXCONSJORM-UHFFFAOYSA-N 0.000 description 1
- FTCLAXOKVVLHEG-UHFFFAOYSA-N sodium;3-sulfanylpropane-1-sulfonic acid Chemical compound [Na].OS(=O)(=O)CCCS FTCLAXOKVVLHEG-UHFFFAOYSA-N 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 1
- 230000019635 sulfation Effects 0.000 description 1
- 238000005670 sulfation reaction Methods 0.000 description 1
- 125000004646 sulfenyl group Chemical group S(*)* 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 description 1
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- AOBORMOPSGHCAX-DGHZZKTQSA-N tocofersolan Chemical compound OCCOC(=O)CCC(=O)OC1=C(C)C(C)=C2O[C@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C AOBORMOPSGHCAX-DGHZZKTQSA-N 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- BWHOZHOGCMHOBV-BQYQJAHWSA-N trans-benzylideneacetone Chemical compound CC(=O)\C=C\C1=CC=CC=C1 BWHOZHOGCMHOBV-BQYQJAHWSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- GLFDLEXFOHUASB-UHFFFAOYSA-N trimethyl(tetradecyl)azanium Chemical compound CCCCCCCCCCCCCC[N+](C)(C)C GLFDLEXFOHUASB-UHFFFAOYSA-N 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
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Abstract
本发明涉及用于处理金属表面和使金属或金属合金在塑料表面上沉积的组合物,该组合物包含:a)作为组分A的至少一种聚合物,其由含氨基的聚合物(组分Aa),至少一种芳族化合物(组分Ab)和任选的醛(组分Ac)构成;b)作为组分B的水或适于溶解、分散、悬浮或乳化所述聚合物的其它溶剂;c)任选的作为组分C的表面活性化合物、分散剂、悬浮剂和/或乳化剂。本发明还涉及处理金属表面的方法和使金属或金属合金在塑料表面上沉积的方法,其中使金属表面或塑料表面与聚合物(组分A)接触。本发明还公开了聚合物(组分A)在处理金属表面和使金属或金属合金在塑料表面上沉积中的用途,以及由特定组分A′a、A′b和A′c构成的聚合物。
Description
本发明涉及用于处理金属表面的组合物,处理金属表面以防腐的方法,聚合物在处理金属表面中的用途以及适于处理金属表面的聚合物。本发明进一步涉及用于使金属或金属合金在塑料表面上沉积的组合物和方法。
金属腐蚀在含有金属的制品的生产、加工和应用中引起了问题。为了抑制或防止腐蚀,因此使用保护膜和腐蚀抑制剂。虽然保护膜可永久性地施用于金属,但优选将腐蚀抑制剂加入物质中,尤其加入液体混合物中,后者若与金属接触则将引起或加速腐蚀。保护膜和腐蚀抑制剂均可以包含聚合物,或以聚合物形式存在。尤其令人感兴趣的是其中不需要使用任何有毒的铬酸盐的组合物。这类组合物在现有技术中是已知的。
US 4,992,116描述了水性无铬组合物和处理铝的方法。这些组合物包含磷酸根离子以及含有选自Zr、Ti、Hf和Si中的元素并以氟锆酸、氟钛酸、氟铪酸和氟硅酸为基础的化合物。该类组合物进一步包含由胺与选自聚链烯基酚类和鞣酸类中的化合物的曼尼希反应获得的多酚。根据US4,992,116,用所述组合物处理的铝表面在粘合和耐腐蚀性方面与用铬基组合物处理的铝表面相媲美。
WO 92/07973涉及用于处理铝或铝合金的无铬防腐蚀剂,它们包含水溶性的或水分散性聚合物。WO 92/07973的组合物包含酸性水溶液,该水溶液除了水以外还包含氟锆酸、视需要而定的分散SiO2、非水溶剂、表面活性剂和3-(N-C1-14烷基-N-2-羟乙基氨基甲基)-4-羟基苯乙烯。根据WO92/07973,这些特定组合物特别适于处理铝表面。
DE-A-100 10 758涉及防腐处理具有至少部分由至少90%的锌、铝和/或镁和/或这些金属彼此或与其它合金成分的合金组成的金属表面的车身或家用电器的方法。所述方法包括表面的清洁、钝化和涂覆。为了钝化,使用除了Ti、Zr、Hf、Si和/或B的配位氟化物以外还含有有机聚合物的水溶液。所用有机聚合物优选是聚-4-乙烯基苯酚化合物。这些聚乙烯基化合物可优选通过使聚乙烯基苯酚与甲醛或低聚甲醛和有机仲胺缩合而获得。
鉴于使用金属表面的腐蚀抑制剂和保护膜的重要性和广泛性,对于其性能范围,如对金属表面的粘合,防腐蚀活性和疏水特性满足处理金属表面必需符合的严格要求的保护膜和腐蚀抑制剂存在着巨大需求。而且,保护膜和/或腐蚀抑制剂的各组分应该易于以令人满意的量获得和应该尽可能地便宜。
本发明的目的是提供获得对金属表面的下列改进中的至少一种的用于表面处理金属的组合物:改进的防腐,对于后续增强涂层(例如表面涂覆或金属沉积)的改进粘合、钝化和更平滑的表面(在抛光、酸洗、电抛光的情况下)。本发明的另一个目的是提供表面处理金属的方法以及适于作为本发明组合物的组分并满足上述要求的聚合物。此外,本发明的一个目的是提供用于沉积金属的添加剂。再一个目的是提供用于使金属或金属合金在塑料表面上沉积的组合物和方法。
我们已经发现,这些目的通过用于处理金属表面的组合物得以实现,该组合物包含如下组分:
a)作为组分A的至少一种聚合物,其由如下组分构成:
aa)作为组分Aa的至少一种含氨基的聚合物;
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元;
ac)视需要而定的作为组分Ac的醛;
b)作为组分B的水或适于溶解、分散、悬浮或乳化聚合物(组分A)的其它溶剂;
c)视需要而定的作为组分C的表面活性化合物、分散剂、悬浮介质和/或乳化剂。
本发明组合物可以用于所有金属处理方法中,尤其可以用于可能发生金属表面腐蚀的那些方法中。这些方法的实例是金属表面,优选无铬酸盐的金属表面的钝化,尤其磷酸盐化,金属表面的酸洗,金属表面的封闭,以及例如通过镀镍、镀锌、镀锡、镀铜或沉积合金而使金属在金属表面上的沉积。此外,这些组合物可以用于生产表面涂料或转化型带锈涂料(Rostumwandlern)。在所述方法中,尤其就金属表面的钝化和金属在金属表面上的沉积而言,包含根据本发明使用的聚合物(组分A)的组合物带来了有效的抑制作用和保护膜和/或施涂于其上的增强涂层(例如表面涂层或化学或电化学沉积金属涂层)与金属表面的有效粘合。另外,本发明组合物可以用于使金属在塑料表面上沉积,例如在制造印刷电路板中。
本发明组合物优选包括腐蚀抑制剂组合物,后者用于表面处理其中可能发生金属表面腐蚀的金属的方法中或用于防腐。
合适的金属表面一般是选自铝合金、镁合金、钢、铜、锌、锡、镍、铬和这些金属的普通工业合金中的普通工业材料。其它合适的金属表面是贵金属,尤其金、银及其合金。还合适的一般是可以用化学或电化学方法生产的普通工业金属涂料,其选自锌及其合金,优选金属锌,锌/铁,锌/镍,锌/锰或锌/钴合金,锡及其合金,优选金属锡,含Cu、Sb、Pb、Ag、Bi和Zn的锡的合金,特别优选在例如制造和加工印刷电路板中用作焊剂的那些,以及铜,它们优选呈其在印刷电路板和镀金属塑料部件上使用的形式。
在本发明组合物用于金属表面的酸洗或钝化,尤其磷酸盐化的情况下,所述金属表面优选是钢、铸铁、锌、铝、镁和/或这些金属彼此的合金或与其它合金成分的合金的表面。在这些情况下,特别优选锌和铝以及这些金属与其它合金成分的合金。
在本发明组合物用于使金属在金属表面上沉积的情况下,当镀锌和沉积锌合金时以及当镀铜和镀镍时,优选钢表面,而当镀锡(包括Sn合金)时,优选铜和钢。
可以使用本发明组合物来处理未进行预处理的金属表面。然而,优选金属表面在用本发明组合物处理之前已至少进行过清洗。除了其它操作以外,该清洗优选还包括将金属表面脱脂的操作。合适的清洗和脱脂方法对于所属技术领域的熟练技术人员而言是已知的。还可以在金属表面上的酸洗操作或钝化操作之后的工艺步骤中,例如在表面涂覆步骤中使用本发明组合物。本发明组合物还可以作为包含所属技术领域的熟练技术人员已知的添加剂且可以用于相应方法中的清洗、酸洗和抛光配制剂使用。
本发明组合物还可以用于使金属或金属合金在塑料表面上沉积。本说明书因此进一步提供了用于使金属在塑料表面上沉积的组合物,包含如下组分:
a)作为组分A的至少一种聚合物,其由如下组分构成:
aa)作为组分Aa的至少一种含氨基的聚合物;
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元;
ac)视需要而定的作为组分Ac的醛;
b)作为组分B的水或适于溶解、分散、悬浮或乳化聚合物(组分A)的其它溶剂;
c)视需要而定的作为组分C的表面活性化合物、分散剂、悬浮介质和/或乳化剂。
优选适于对塑料表面镀镍和镀铜,例如在制造印刷电路板中镀铜的组合物。利用普通工业方法对塑料表面进行镀金属操作。本发明组合物用于对塑料镀金属,但视需要而定可以用于镀金属操作的预处理中。
对于本发明而言,术语“组合物”不仅用来指即用组合物,还指浓缩物。下文对于各个组分所述的浓度以即用组合物为基准。然而,所属技术领域的熟练技术人员应该明白,在浓缩物中各组分的浓度相应地更高。
组分A
组分A是由作为组分Aa的至少一种含氨基的聚合物和作为组分Ab的属于酚或醌或含有酚型或醌型结构单元的至少一种芳族化合物构成的聚合物。视需要而定,该聚合物包含作为组分Ac的来源于与醛的反应的结构单元。
术语“聚合物”应该一般理解为指含有至少三个重复单元,优选超过10个重复单元的化合物。本发明使用的聚合物的重均分子量一般是500-5000 000g/mol,优选1000-1 500 000g/mol。该聚合物还可以呈交联形式,因此不能具体规定分子量,尽管该聚合物可以在普通工业溶剂中分散、乳化或悬浮。
组分Aa
组分Aa是含氨基的聚合物。优选使用的聚合物包括聚乙烯亚胺,聚乙烯基胺,聚(乙烯基甲酰胺-乙烯基胺),聚赖氨酸,以及聚氨基苯乙烯。还合适的是仍然含有氨基的聚胺衍生物,实例是聚胺与羧酸和/或磺酸的反应产物,或聚胺的羧甲基化产物。其它合适且特别优选的聚合物是聚羧酸酯的含氨基的衍生物,尤其二胺与含马来酸、丙烯酸或甲基丙烯酸重复单元的共聚物的反应产物,如苯乙烯-马来酸酐共聚物与二胺的反应产物。非常特别优选式(I)和(II)的聚合物:
在这些式中,R是有机基团,优选亚烷基、亚环烷基、亚芳基、芳基亚烷基或烷基亚芳基。该基团可以被杂原子间隔或根据需要被取代,其中合适取代基是烷基、链烯基、芳基、烷芳基或芳烷基,它们进而可以被杂原子间隔或被含有杂原子的基团取代。优选R是C2-32-亚烷基,特别优选它是可以被选自-N-和-O-中的杂原子间隔和可以携带C1-6-烷基或含杂原子的基团-实例是氨基-的C2-14-亚烷基。特别优选的基团是乙基、正丁基和正己基。
R′、R″和R彼此独立表示氢或任何所需的有机基团。合适有机基团一般是烷基、环烷基、链烯基、芳基、烷芳基和芳烷基,视需要而定它们可以被杂原子间隔和/或被含有杂原子的基团取代。优选R′、R″、R彼此独立表示氢或烃,特别优选氢、C1-6烷基、C6-10芳基,非常特别优选甲基、乙基、异丙基、正丙基或苯基。
含氨基的聚合物可以商购(聚乙烯亚胺,聚乙烯基胺),或可以通过所属技术领域的熟练技术人员已知的方法来制备。制备聚乙烯基胺的合适方法例如公开在EP-A 216 387、DE-A 38 42 820、DE-A 195 266 26、DE-A 195159 43中。特别优选使用的式(I)和(II)的聚合物例如可根据在US 4,046,748中公开的方法来制备。
还可以以与低分子量胺类的混合物使用聚合物。在这种情况下,合适的低分子量胺类选自乙二胺;H2N-(C2H4-NH)n-H,其中n=2-4;以及H2N(-CH2)n-H,其中n=1-18,优选n=2、3、4、6、8、10或12。
该含氨基的聚合物一般呈脱盐形式。在含乙烯基胺和乙烯基甲酰胺重复单元的共聚物的情况下,水解度通常为0.5-100%,优选50-100%。
组分Ab
组分Ab是酚或醌,或含有酚型或醌型结构单元的化合物。
合适的醌类或醌衍生物一般是由邻苯醌或对苯醌衍生的体系。优选使用由对苯醌衍生的体系。特别优选的化合物是式(III)的那些:
其中R1、R2、R3和R4彼此独立是氢或烷基、链烯基、环烷基、芳基、烷芳基或芳烷基。优选R1-R4彼此独立是氢或C1-C14烷基、C2-C14链烯基、C6-C14芳基或C5-C16环烷基。还可能的是,R1与R2和/或R3与R4成对形成可以是饱和或不饱和的环基。该环基优选是由总共6个碳原子组成的环,其中两个碳原子来源于式(III)中的母体结构。所述基团进而可以被烷基、链烯基、环烷基、芳基、烷芳基或芳烷基取代和/或可以被杂原子间隔和/或被含有杂原子的基团取代。特别优选的是,式(III)中的基团R1-R4彼此独立表示氢和甲基。特别优选使用的式(III)化合物选自苯醌、2,3,5-三甲基苯醌、2,6-二甲基苯醌、萘醌和蒽醌。
合适的酚类或包含酚型或醌型结构单元的化合物是式(IV)化合物:
在该式中,基团R5、R6、R7、R8和R9彼此独立具有以上对于R1-R4所述的定义。另外,基团R5与R6、R6与R7、R7与R8和/或R8与R9可以成对形成对于R1与R2和R3与R4所定义的环基。此外,基团R5-R9中的一个或两个可以表-O-M+。
在式(IV)中的M+表示氢或阳离子。通常而言,M+是碱金属阳离子,更优选钠或钾离子。然而,还可行的是,M+是具有二价或更高价态的阳离子,优选碱土金属阳离子或Zn、Mn或Cr(III),特别优选镁或钙。
除了上述基团以外,R5-R9还可以表示-SO3 -M+、-NO2、卤素、-COO-M+、-C(O)R″″(其中R″″是氢或烷基、芳基、环烷基、芳烷基或烷芳基)、-N(R″″)2、-OR″″或-SH或所属技术领域的熟练技术人员已知的其它官能团。通常而言,基团R5-R9中仅一个具有最后所述定义之一。
优选的式(IV)化合物是可以被上述基团取代的1价、二价或3价酚类。在本文中,不仅所述酚类化合物是合适的,而且它们的盐也是合适的。
特别优选的式(IV)化合物是苯酚,4,4′-二羟基二苯基硫,二羟基二苯基亚砜,苯酚磺酸,1,4-二羟基萘,硝基苯酚,(N,N-二甲基氨基)-1-苯酚,羟基茴香硫醚,连苯三酚,间苯三酚,1,2,4-三羟基苯,2,2′,4,4′-四羟基二苯甲酮,水杨酸,2,3-二羟基苯甲酸,2,4-二羟基苯甲酸,2,5-二羟基苯甲酸,三羟基苯甲酸如没食子酸,水杨酸烷基酯如水杨酸乙酯,3,4-二羟基苯甲酸烷基酯如3,4-二羟基苯甲酸乙酯,没食子酸烷基酯如没食子酸丙酯,2,3-二羟基苯甲醛,2,4-二羟基苯甲醛,2,5-二羟基苯甲醛,2,3,4-三羟基苯甲醛,((4-叔丁基-2,6-二甲基-3-羟基)苄基)咪唑啉,(s)-2-(3,4-二羟基苄基)-2-肼基丙酸,1,2-二羟基-4-叔丁基苯,2-(4-羟基苯氧基)丙酸,2-(4-羟苯基)乙胺,2-(4-羟苯基)乙胺,2,3,5-三甲基苯-1,4-二醇,2,3-二氢-1,4-二羟基蒽醌,2,4-二氯苯酚,2,5-二羟基甲苯,2,5-二甲苯酚,2,5-二叔戊基氢醌,2,7-二羟基萘,2-烯丙基苯酚,2-氨基-4,6-二硝基苯酚,2-羟基-3-甲基苯甲酸,2-羟基乙酰苯,2-羟基蒽醌,2-羟基苯甲醛,2-羟基苯甲酸甲酯,2-羟基苯基乙酸,甲基氨基甲酸2-羟苯基酯,2-萘酚-3,6-二磺酸,2-叔丁基-4-甲基苯酚,2-叔丁基氢醌,3,5-二叔丁基-4-羟基甲苯,3-氨基苯酚,3-羧基-2-羟基萘,3-甲基苯酚,3-叔丁基-4-羟基茴香醚,4-(2-(3-(4-羟苯基)-1-甲基丙基)氨基)乙基)-1,2-二羟基苯,4,4′-二羟基联苯,4-乙酰氨基-1-羟基苯,4-氯酚,4-重氮基-3-羟基萘-1-磺酸,4-羟基乙酰苯,4-羟基苯甲酸,4-羟基苯甲酸丙酯,4-羟基二苯甲酮,4-羟基扁桃酸,4-甲氧基苯酚,4-甲基苯酚,4-硝基-2-氨基苯酚-6-磺酸,5-氯-2-羟基甲苯,5-硝基-2-氨基苯酚,6-乙酰氨基-2-氨基-1-羟基苯-4-磺酸,6-羟基萘-2-磺酸,8-羟基-2-甲基喹啉,8-羟基喹啉,肾上腺素,α-生育酚,戊基间甲酚,双(4-羟苯基)砜,双酚A,邻苯二酚,多巴胺,雌二醇,氢醌,靛红双甲酚,N,N-双(羟乙基)-4-羟基苯胺,N,N-二乙基间氨基苯酚,N,N-二甲基-2-(4-羟苯基)-乙胺硫酸盐,N,N-二甲基-4-羟基苯基乙胺,N,N′-二水杨醛乙二胺,3-(3,5-二叔丁基-4-羟苯基)丙酸十八烷基酯,十八烷基苯酚,对十二烷基苯酚和对异壬基苯酚。除上述酚类化合物之外,它们的盐也是合适的。
特别优选使用苯酚和邻苯二酚。
组分Ac
视需要而定,聚合物(组分A)还由作为其它组分的醛,即组分Ac构成。例如,当该聚合物通过曼尼希反应来制备时,存在该其它组分。通常而言,合适的醛组分Ac包括全部醛类。优选使用式(V)的醛类。
在该式中,R10表示氢、烷基、链烯基、环烷基、芳基、芳烷基或烷芳基。在这里,基团R10可以被杂原子和/或含杂原子的基团取代。对R10所提及的基团还可以被杂原子间隔。R10优选是氢、C1-14烷基、C1-14链烯基、C5-16环烷基、C6-14芳基、C7-14芳烷基或C7-18烷芳基。这些基团可以被含杂原子并选自卤素-优选氯或溴、NO2、SH、OH、乙酰基、羧基和-C(O)-苯基中的基团取代,或被杂原子间隔。基团R10进而本身可以被烷基、环烷基、芳基、烷芳基或芳烷基取代,这些取代基进而可以携带含杂原子的基团,和/或其链和/环可以被杂原子间隔。
特别优选的组分Ac包括选自甲醛、乙醛、丙醛、丁醛、香茅醛、苯甲醛、2-氯苯甲醛、2-羟基苯甲醛、2-丙烯醛、3,3-二甲基丙烯醛、4-甲基苯甲醛、4-(1,1-二甲基乙基)苯甲醛、茴香醛、4-氯苯甲醛、3-羟基-2,2-二甲基丙醛、7-羟基-3,7-二甲基辛醛、正己醛、2-糠醛、3-甲基-4-氧代-2-丁烯酸甲酯、3-甲基丁醛、2-乙基己醛、2-甲基丙醛、2-苯基丙醛、3,7-二甲基辛-2,6-二烯-1-醛、4-(1,1-二甲基乙基)-α-甲基苯丙醛、戊醛、2-甲基戊醛、2-甲基-2-戊烯醛、3-乙酰氧基-2-甲基丙醛、4-乙酰氧基-2-甲基-2-丁烯醛、3-甲酰基蒎烷、4-苄氧基苯甲醛、2-甲基-4,4-二乙酰氧基-2-丁烯醛、2-甲基-2-丙烯醛、对苯二甲醛、3-(4-甲基苯基)-2-甲基-2-丙烯醛、4-甲酰基苯甲酸、3-硝基苯甲醛、3-甲酰基-4-甲基四氢吡喃、2-甲基-3-甲基硫代丙醛、2-甲酰-2-甲基丙酸甲酯、邻苯二甲醛、视黄醛、3-(4-甲氧基苯基)-2-甲基-2-丙烯醛、2,3-二苯基丙烯醛、3-甲酰基-2-甲基丙酸甲酯和肉桂醛中的至少一种组分。
聚合物(组分A)可以通过所属技术领域的熟练技术人员已知的方法来制备。优选的聚合物是通过迈克尔加成反应(R1)获得的那些和当在曼尼希反应(R2)中添加合适的醛(组分Ac)时获得的那些。以下反应方案示出了以苯醌为例的迈克尔反应(R1):
在该反应方案中,R11表示氢或有机基团,这取决于所用的含氨基的聚合物(组分Aa)。优选R11是氢或甲基。
以下以苯酚为例描述了同样优选用于制备聚合物(组分A)的曼尼希反应(R2):
R10和R11的定义上文中已经给出。
在本发明组合物中,组分A一般以0.01-400g/L,优选0.2-100g/L,特别优选1-50g/L的量使用,在各种情况下以1L组合物为基准计。组分A的精确量取决于用于处理金属表面的各种方法以及所述金属表面。
组分B
组分B是水和适于溶解或分散、悬浮或乳化聚合物(组分A)的其它溶剂。除了水以外的其它合适溶剂是例如脂族或芳族溶剂如苯,甲苯和二甲苯,卤化溶剂如二氯甲烷和氯仿,醇类如甲醇和乙醇,醚类如二乙基醚和四氢呋喃,聚醚,尤其聚乙二醇,酮类如丙酮,以及这些溶剂彼此或与水的混合物。特别优选单独使用水作为溶剂。
pH由应用的类型决定。例如,酸洗和磷酸盐化浴通常是强酸性的,而电镀浴是碱性或酸性的,这取决于浴的类型。适于特定应用的pH值对于所属技术领域的熟练技术人员而言是已知的。
水或其它溶剂的量随本发明组合物是即用组合物还是浓缩物以及各自最终用途而变化。该量基本上是为即用组合物规定的各组分的浓度的函数。
组分C
视需要而定,本发明组合物可以进一步包含表面活性化合物、乳化剂和/或分散剂。合适的表面活性化合物是表面活性剂,它们可以是阳离子的、阴离子的、两性离子的或非离子的。合适的表面活性剂的例子是R-EOn/POm类型的烷基和链烯基烷氧基化物,其中R一般是线性或支化C6-C30烷基,优选C8-C20烷基,EO是氧化乙烯单元,PO是氧化丙烯单元,其中EO和PO的顺序排列是任意的,以及n和m彼此独立是>1且<100,优选>3且<50,实例是Emulan、Lutensol和Plurafac(来自BASF);烷基苯酚乙氧基化物;EO/PO嵌段共聚物(Pluronic,来自BASF);烷基醚硫酸盐;以及烷基铵盐,又称为季铵盐。
这些组分在本发明组合物中的量一般是0.01-100g/L,优选0.1-20g/L。
在一个优选实施方案中,本发明组合物用于处理金属表面,并且除了组分A、B和视需要而定的C以外进一步包含如下组分:
d)作为组分D的以过渡金属阳离子、过渡金属氧合阴离子、含氟金属酸根(Fluorometallaten)或镧系元素为基础的至少一种盐、酸或碱,
和/或
e)作为组分E的选自磷酸、硫酸、磺酸、硝酸、氢氟酸和盐酸中的至少一种酸,和/或
f)作为组分F的至少一种其它腐蚀抑制剂,和/或
g)作为组分G的Ce、Ni、Co、V、Fe、Zn、Zr、Ca、Mn、Mo、W、Cr和/或Bi的化合物,和/或
h)作为组分H的其它助剂和添加剂。
这些组合物尤其适于酸洗或钝化,尤其磷酸盐化,或作为本说明书中所述的金属表面的转化型带锈涂料。
组分D
合适的组分D是以过渡金属阳离子、过渡金属氧合阴离子、含氟金属酸根或镧系元素为基础的盐、酸和碱。合适的过渡金属阳离子尤其是Ti(IV)、Zr(IV)、Hf(IV)和/或Si(IV)的含氟金属酸根,尤其合适的镧系元素是Ce。还合适的是钨酸根和钼酸根。
包含组分D的本发明组合物尤其适于在金属表面上沉积防腐涂层或适于增强已沉积在金属表面上的防腐涂层的防腐效果。在本发明组合物中,本发明使用的聚合物(组分A)具有突出的防腐效果。
在组分D存在于本发明组合物中的情况下,组分D的量优选是0.02-20g/L。
组分E
除了组分D以外,或代替组分D,本发明组合物可以进一步包含选自磷酸,硫酸,磺酸类如甲磺酸、乙烯基磺酸、烯丙基磺酸、间硝基苯磺酸、萘磺酸及其衍生物,硝酸,氢氟酸以及盐酸中的至少一种酸。所用酸的类型取决于金属表面处理的类型。因此,磷酸通常在用于磷酸盐化钢表面的磷酸盐化浴中使用。在该情况下,本发明组合物是磷酸盐化溶液。这里要与称作“非成膜”磷酸盐化溶液,即不含二价金属的溶液进行区分。这些非成膜磷酸盐化溶液例如呈磷酸铁溶液形式。在磷酸盐化溶液含有二价金属离子,例如锌和/或锰离子的情况下,磷酸盐化溶液据说可以是成膜的。包含硝酸的本发明组合物特别适于表面处理锌及其合金,而包含氢氟酸的组合物特别适于表面处理铝及其合金。
酸的用量可因应用领域而异。一般而言,在组分E存在于本发明组合物中的情况下,它以0.2-200g/L,优选2-100g/L的量使用。
组分F
除了组分D和/或E以外,或代替组分D和/或E,本发明组合物可以包含至少一种另外的腐蚀抑制剂。合适的腐蚀抑制剂选自丁炔二醇,苯并三唑,醛类,胺羧化物,氨基苯酚和硝基苯酚,氨基醇,氨基苯并咪唑,氨基咪唑啉类,氨基三唑,苯并咪唑胺类,苯并噻唑类,苯并三唑衍生物,硼酸与各种链烷醇胺的酯类如硼酸二乙醇胺酯,羧酸及其酯,喹啉衍生物,二苄基亚砜,二羧酸及其酯,二异丁烯基丁二酸,二硫代膦酸,脂肪胺和脂肪酸酰胺,胍衍生物,尿素及其衍生物,氯化月桂基吡啶鎓,马来酰胺,巯基苯并咪唑,N-2-乙基己基-3-氨基磺基丙酸,鏻盐,邻苯二甲酰胺,烷基醇的胺-和钠中和的磷酸酯,以及这些磷酸酯本身,聚烷氧基化物、特别是聚乙二醇的磷酸酯,聚醚胺,锍盐,磺酸如甲磺酸,硫醚类,硫脲类,秋兰姆二硫化物(Thiuramidsulfiden),肉桂酸及其衍生物,锌磷酸盐和锌硅酸盐,以及锆磷酸盐和锆硅酸盐。
作为其它腐蚀抑制剂,优选使用丁炔二醇和苯并三唑(尤其用于表面处理铜)。
如果要在组合物中使用,则腐蚀抑制剂以通常0.01-50g/L,优选0.1-20g/L,特别优选1-10g/L的量使用。
组分G
除了上述组分以外,或视需要代替上述组分,还可以使用Ce、Ni、Co、V、Fe、Zn、Zr、Ca、Mn、Mo、W、Cr和/或Bi的化合物。通常而言,根据本发明的组分A在组合物中的使用获得了良好的防腐性能,使得不必添加上述化合物。优选本发明组合物不含Cr(VI)。然而,在使用上述化合物(组分G)的情况下,优选使用选自Fe、Zn、Zr和Ca中的化合物。如果这些化合物存在于本发明组合物中,则它们的量通常是0.01-100g/L,优选0.1-50g/L,特别优选1-20g/L。
组分H
除了上述组分D-G中的一种或多种之外,本发明组合物还可以包含其它助剂和添加剂。合适的助剂和添加剂包括导电性颜料或导电性填料,例如磷化铁、碳化钒、氮化钛、炭黑、石墨、二硫化钼或掺杂锡或锑的硫酸钡,其中磷化铁是优选的。将导电性颜料或导电性填料加入本发明组合物中,是为了改进所要处理的金属表面的可焊性或为了改进用电泳涂料的后续涂覆。此外,还可以使用二氧化硅悬浮体,特别当使用本发明组合物来处理含有铝的表面时。
这些助剂和/或添加剂一般以细碎形式存在,换句话说,它们的平均粒径一般是0.005-5μm,优选0.05-2.5μm。基于本发明组合物的总质量,助剂和添加剂的量一般是0.1-50重量%,优选2-35重量%。
本发明组合物可以进一步包含用于改进成型特性的添加剂,实例是以天然或合成蜡为基础的蜡基衍生物,例如以丙烯酸为基础的蜡,聚乙烯蜡,聚四氟乙烯(PTFE)蜡或蜡衍生物或石蜡以及它们的氧化产物。
取决于应用领域,本发明组合物可以包含以苯乙烯、4-羟基苯乙烯、丁二烯、丙烯酸、丙烯酸酯、丙烯酰胺、丙烯酸盐、甲基丙烯酸、甲基丙烯酸酯、甲基丙烯酰胺、甲基丙烯酸盐以及丙烯酰胺的衍生物为基础的聚合物分散体。还可行的是,本发明组合物包含聚氨酯分散体和聚酯型氨基甲酸酯分散体或聚脲分散体。
可以存在于本发明组合物中的另一组化合物包括聚乙二醇、聚丙二醇、氧化乙烯的共聚物和氧化丙烯的共聚物。
当本发明组合物作为粉末涂料使用时,它们可以进一步包含环氧树脂和/或甲醛与苯酚、尿素、蜜胺、苯酚磺酸或萘磺酸的缩合树脂。
当本发明组合物用于转化型带锈涂料中时,它们可以进一步包含聚乙烯醇缩丁醛。
取决于包含组分A的本发明组合物的确切组成,它们可以用于金属表面处理的全部应用中,尤其用于可能引起金属表面腐蚀问题的那些应用中。这些应用的实例是脱漆,金属酸洗,电抛光,化学去毛刺,化学和电化学金属沉积(特别是Cu、Ni、Pd、Zn、Co、Mn、Fe、Mg、Sn、Pb、Bi、Ag、Au及其合金的沉积),转化型涂覆(尤其无冲洗转化型涂覆,即冲洗操作次数减少的方法,例如在镀锌钢和铝上的无冲洗转化型涂覆),防腐(尤其在铜-例如在制造印刷电路板中-和钢上的防腐)以及润滑和涂油(尤其与冷成型有关)。施用方式按照普通工业方法来进行,额外注意的是,将本发明组合物与用于所述应用的工业上常用的其它组分一起使用,或使它们与金属在额外处理步骤如例如使用本发明的腐蚀抑制剂组合物的合适配制剂如溶液、乳液、分散体、悬浮体或气溶胶的喷涂、浸涂、表面涂覆或电泳涂覆中接触。
本说明书进一步提供了除了组分A、B和视需要而定的C以外还包含如下组分的金属沉积用组合物:
i)作为组分I的至少一种金属氧化物和/或金属盐,
j)视需要而定的作为组分J的至少一种配合剂,
k)视需要而定的作为组分K的至少一种酸或相应酸的碱金属盐或碱土金属盐,和
l)视需要而定的作为组分L的其它添加剂。
本发明组合物特别适于使金属或金属合金在金属或塑料表面上沉积。上文已经说明了合适的金属表面。金属或金属合金在塑料表面上的沉积优选在制造印刷电路板中使用。沉积优选以化学方法或电化学方法进行。
组分I
合适的金属氧化物或金属盐是选自Zn、Ni、Cu、Au、Pd、Sn、Co、Mn、Fe、Mg、Pb、Bi和Ag中金属的氧化物或盐。这些金属可以以所用金属的形式沉积,或当使用不同金属时以所述金属彼此或与其它金属的合金的形式沉积。优选的合金是CuZn、CuSn、CuNi、SnPb、SnAgBiCu、SnAgCu、SnBi、SnAg、SnCu、NiPd、NiP、ZnFe、ZnNi、ZnCo和ZnMn。上述合金的成分可以任何所需的浓度存在于合金中。特别优选沉积Zn、Cu和Ni,以及这些金属与其它金属或彼此的合金。在塑料表面上沉积金属或金属合金时,Ni和Cu是特别优选的。除了作为金属氧化物使用之外,这些金属可以作为选自相应的硫酸盐、磺酸盐、氯化物、碳酸盐、氨基磺酸盐、氟硼酸盐、氰化物和乙酸盐中的金属盐使用。
基于所用金属的量,金属离子在本发明组合物中的浓度通常是0.01-100g/L,优选0.1-50g/L,特别优选2-20g/L。
组分J
视需要而定,本发明组合物可以进一步包含配合剂。合适的配合剂的实例包括乙二胺四乙酸(EDTA)、乙二胺(ED)、柠檬酸和所述化合物的盐。
组分K
视需要而定,本发明组合物可以进一步包含优先选自HNO3、H2SO4、H3PO4、甲酸和乙酸中的至少一种酸,或相应酸的碱金属盐或碱土金属盐。该酸通常以0.5-700g/L,优选5-200g/L的量使用。
组分L
除上述组分之外,本发明组合物还可以包含其它添加剂,并且因意欲用途、所要沉积的金属、目的和所用方法而异。合适的添加剂是1-(2-乙烯基吡啶鎓)-2-乙基磺基甜菜碱,1,1-二甲基-2-丙炔-1-基胺,1-吡啶鎓-2-乙基磺基甜菜碱,1-吡啶鎓-2-羟基-3-丙基磺基甜菜碱,1-吡啶鎓-3-丙基磺基甜菜碱,2,2’-二氯二乙基醚,2,5-二甲基-3-己炔-2,5-二醇,2-丁炔-1,4-二醇,2-丁炔-1,4-二醇乙氧基化物,2-丁炔-1,4-二醇丙氧基化物,3-(2-苯并噻唑基硫基)-1-丙磺酸钠,3,3’-二硫基双(1-丙磺酸)钠,3-[(氨基亚氨基甲基)硫基]-1-丙磺酸,3-[(二甲基氨基)硫代甲基]硫基-1-丙磺酸钠,3-[乙氧基硫代甲基]硫基-1-丙磺酸钾,3-氯-2-羟基-1-丙磺酸钠,3-己炔-2,5-二醇,3-巯基-l-丙磺酸钠,4,4-二羟基二苯基砜,4-甲氧基苯甲醛,醛类,烷基苯基聚氧化乙烯磺基丙基醚钾盐,烷基聚氧化乙烯磺基丙基醚钾盐如十三烷基/十五烷基聚氧化乙烯磺基丙基醚钾盐,烯丙基磺酸钠,氨基磺酸,烷基醇的胺-和钠中和的磷酸酯,胺羧化物,氨基苯酚类和硝基苯酚类,氨基醇类,氨基苯并咪唑,氨基咪唑啉类,氨基三唑,亚苄基乙酸甲酯,亚苄基丙酮,苯并咪唑胺类,苯并噻唑类,苯并三唑及其衍生物,吡啶-3-甲酸苄酯,双酚A,硼酸与各种链烷醇胺的酯如硼酸二乙醇胺酯,羧酸及其酯类,羧乙基异硫脲鎓甜菜碱,喹啉衍生物,乙烯和丙烯酸的共聚物,咪唑和表氯醇的共聚物,咪唑、吗啉和表氯醇的共聚物,N,N’-双[3-(二甲基氨基)丙基]脲和1,1’-氧基双[2-氯乙烷]的共聚物,丙烯酸正丁酯、丙烯酸和苯乙烯的共聚物,二苄基亚砜,二羧酸及其酯,二亚乙基三胺五乙酸及由其衍生的盐,二异丁烯基丁二酸,亚乙基双二硫代氨基甲酸二钠,二硫代膦酸,乙基氨基磺酸,乙二胺四乙酸和由其衍生的盐,乙基甘氨酸二乙酸和由其衍生的盐,乙基己醇乙氧基化物,脂肪胺类和脂肪酸酰胺,甲醛,甘油乙氧基化物,胍衍生物,尿素及其衍生物,羟乙基亚氨基二乙酸和由其衍生的盐,咪唑,异丙基氨基磺酸,异丙基氨基磺酰氯,甲基硫酸月桂基/肉豆蔻基三甲基铵,氯化月桂基吡啶鎓,马来酰胺类,巯基苯并咪唑,甲基氨基磺酸,N,N,N’,N’-四(2-羟丙基)乙二胺,N,N-二乙基-2-丙炔-1-胺,N,N-二乙基-4-氨基-2-丁炔-1-醇,N,N-二甲基-2-丙炔-1-胺,N-2-乙基己基-3-氨基磺基丙酸,氯化N-烯丙基吡啶鎓,硫酸化烷基苯酚乙氧基化物的钠盐,2-乙基己基硫酸钠,烟酸,次氮基三乙酸和由其衍生的盐,硝基苯磺酸钠,氯化N-甲基烯丙基吡啶鎓,邻氯苯甲醛,鏻盐,邻苯二甲酰胺,吡啶甲酸,聚醚胺类,聚乙烯亚胺类,聚乙烯基咪唑,炔丙醇,炔丙醇乙氧基化物,炔丙醇丙氧基化物,丙炔磺酸钠,丙炔酸,丙二胺四乙酸和由其衍生的盐,吡咯,季化聚乙烯基咪唑,2-丁炔-1,4-二醇和表氯醇的反应产物,2-丁炔-1,4-二醇和丙磺酸内酯的反应产物,糖精和丙磺酸内酯的反应产物,烷基乙氧基化物/丙氧基化物与丙磺酸内酯的反应产物,聚乙烯亚胺与丙磺酸内酯的反应产物,β-萘酚乙氧基化物/丙氧基化物与丙磺酸内酯的反应产物,间苯二酚乙氧基化物,糖精,β-萘酚乙氧基化物,β-萘酚乙氧基化硫酸钠,锍盐,磺酸如甲磺酸,硫二甘醇,硫二甘醇乙氧基化物,硫醚,硫脲类,秋兰姆硫化物,乙烯基磺酸钠,肉桂酸及其衍生物,锌磷酸盐和锌硅酸盐,锆磷酸盐和锆硅酸盐,次磷酸盐(例如次磷酸钠),NaBH4,二甲基氨基硼烷,二乙基氨基硼烷,肼,甲醛,乌洛托品,氯化钯,锡酸钠,HFxBF3,分子量为100-1 000 000g/mol的聚乙二醇,氧化乙烯和氧化丙烯的嵌段共聚物-实例是来自BASF Aktiengesellschaft,Ludwigshafen/Rhein的Pluronic品级,以及氧化乙烯和氧化丙烯的无规共聚物-尤其分子量为100-2000g/mol的那些。
使用根据该实施方案的本发明组合物,尤其可以通过电化学或化学方法获得金属沉积物。是进行化学还是电化学沉积取决于金属、金属表面和所需的结果。
处理金属或塑料表面的方法
本说明书进一步提供了一种处理金属表面的方法,该方法包括使金属表面与由如下组分构成的聚合物(组分A)接触:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
在上文已经描述了该聚合物以及该聚合物的优选实施方案和合适的制备方法(参看组分A)。在以上同样描述了合适的金属表面以及金属表面的优选实施方案。
合适的方法包括例如脱漆、金属酸洗、电抛光、化学去毛刺、化学和电化学金属沉积、转化型涂覆(尤其无冲洗转化型涂覆)、防腐(尤其在铜-例如在制造电路板中-和钢上的防腐)、润滑和涂油(尤其在冷成型的情况下)。
在本发明方法中,聚合物可以作为溶液、乳液、悬浮体或气溶胶存在。优选的是,该聚合物(组分A)存在于本发明的上述组合物之一中。
应用的类型对应于普通工业方法,额外注意的是,将根据本发明使用的聚合物(组分A)与用于相应应用的工业上常用的其它组分一起使用,或使它们在额外处理步骤中,例如在使用这些聚合物的合适配制剂的喷涂、浸涂、表面涂覆或电泳涂覆中与金属接触。
在本发明方法的一个优选实施方案中,使金属表面与包含组分A、B和视需要而定的C的组合物接触,或与不仅包含组分A、B和视需要而定的C,而且包含作为其它组分的组分D和/或E和/或F和/或G和/或H的组合物接触。以上已经列举了合适的组分B-H。在本发明方法的优选实施方案中,优选进行金属表面的酸洗或钝化,尤其磷酸盐化。用于金属表面的钝化,尤其磷酸盐化,或酸洗的合适工艺步骤和装置是所属技术领域的熟练技术人员已知的。
通常而言,金属表面处理,尤其钝化,特别优选磷酸盐化或酸洗处理通过将本发明组合物喷雾到金属表面上或通过将金属表面浸入本发明组合物中来进行,这取决于所要处理的部件的数目、尺寸和形状。
在将金属条磷酸盐化时,可以通过辊压(roll-on)或就地干燥或无冲洗方法来施用包含作为组分E的磷酸的本发明组合物,其中将本发明的磷酸盐化组合物施加于金属条上并在没有冲洗的情况下干燥,形成了聚合物膜。
本说明书进一步提供了一种包括如下步骤的方法:
a)视需要而定,清洗金属表面,以便去除油、油脂和灰尘,
b)视需要而定,用水洗涤,
c)视需要而定,在有或无根据本发明使用的聚合物(组分A)存在下进行酸洗,以便去除锈或其它氧化物,
d)视需要而定,用水洗涤,
e)在根据本发明使用的聚合物(组分A)存在下处理金属表面,
f)视需要而定,用水洗涤,
g)视需要而定,在有或无根据本发明使用的聚合物(组分A)存在下进行后处理。
步骤e)中的金属表面的处理可以是根据所属技术领域的熟练技术人员已知的方法的钝化处理,尤其磷酸盐化。将保护涂层、膜或浸渍液施用于金属。在步骤e)中进行磷酸盐化的情况下,可以在步骤g)中用钝化添加剂后处理金属表面。
在各工艺步骤之间用水进行洗涤,以防止后一步骤所需的溶液被在前步骤中使用的溶液的组分污染。然而,本发明方法还可以作为无冲洗方法进行,即没有步骤b)、d)和f)。
清洗步骤(步骤a))和在根据本发明使用的聚合物(组分A)存在下处理金属表面的步骤,优选钝化步骤(步骤e))还可以在一个步骤中进行,即,使用不仅包含常用清洁剂而且包含本发明组合物的配制剂。
在工艺步骤a)-g)之后,金属表面上可以被提供以表面涂料。表面涂覆同样根据所属技术领域的熟练技术人员已知的方法来进行。
本说明书的另一个优选实施方案涉及一种使金属或金属合金在金属表面上沉积的方法,其中使该金属表面与包含组分A、B和视需要而定的C的组合物接触,或与不仅包含组分A、B和视需要而定的C,而且包含作为其它组分的组分I,视需要而定的J,视需要而定的K和视需要而定的L的组合物接触。上文已经描述了合适的组分A、B、C、I、J、K和L。
本说明书的又一个实施方案涉及一种使金属或金属合金在塑料表面上沉积的方法,其中使该塑料表面与由如下组分构成的聚合物(组分A)接触:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
优选的是,在本发明方法中,使塑料表面与包含组分A、B和视需要而定的C的组合物接触,或与不仅包含组分A、B和视需要而定的C,而且包含作为其它组分的组分I,视需要而定的J,视需要而定的K和视需要而定的L的组合物接触。上文已经描述了合适的组分A、B、C、I、J、K和L。
金属或金属合金在塑料表面上的沉积一般在塑料镀金属中,尤其在制造印刷电路板中进行。
在本发明方法的一个特别优选的实施方案中,金属或金属合金在金属或塑料表面上的沉积各自以化学或电化学方法进行。这些方法对所属技术领域的熟练技术人员而言是已知的。特别优选的是,本发明方法包括化学或电化学沉积金、铜或镍,化学沉积钯,电化学沉积锌和/或电化学沉积锡。所述方法不仅包括所述金属的沉积,而且包括它们与其它元素的合金的沉积;这里特别优选的是CuZn、CuSn、CuNi、SnPb、SnAgBiCu、SnAgCu、SnBi、SnAg、SnCu、NiPd、NiP、ZnFe、ZnNi、ZnCo、ZnMn,其中所述合金的各成分以任何所需的浓度存在于合金中。
本发明还包括沉积导电性聚合物的方法,其中这些聚合物在广义上被认为是金属。一种这样的导电性聚合物是聚吡咯。
本发明方法的其它实施方案包括例如其中不仅使用根据本发明的组分A,同时使用酸、氧化剂和腐蚀抑制剂以及溶解的金属盐的清洗、蚀刻、抛光和酸洗方法,以及其中包含组分A的组合物不仅可用于对电路板-包括存在于其中的孔-镀金属,而且用于电路板表面处理的制造印刷电路板的方法。包含组分A的组合物一方面可以用于存在于电路板上的金属的表面处理中,以例如防腐,或用于改进可焊性,以及用于作为金属沉积方法的一部分的用根据本发明使用的包含组分A的组合物处理绝缘表面的方法中,以例如为了镀敷印刷电路板的通孔。
除了根据本发明使用的聚合物(组分A)在上述方法中,尤其在金属表面的酸洗或钝化,尤其磷酸盐化中或在使金属在金属表面或塑料表面上沉积中的用途以外,还可以将根据本发明使用的聚合物(组分A)加入需要防腐的任何地方。
本说明书进一步提供了由如下组分构成的聚合物(组分A)在处理金属中的用途:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
聚合物(组分A)优选用于金属表面的腐蚀抑制。
上文已经详列了优选使用的聚合物,合适的金属表面,合适的腐蚀抑制方法和所述聚合物可用于其中的方法。
另一优选的用途涉及由如下组分构成的聚合物在使金属或金属合金在塑料表面上沉积中的用途:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
根据本发明使用的聚合物(组分A)包含通过使至少一种含氨基的聚合物与芳族化合物和视需要而定的醛反应而获得的聚合物。合适的含氨基的聚合物是如上在组分Aa下所述的那些,包括聚乙烯基胺,聚乙烯基甲酰胺和聚赖氨酸,以及含乙烯基胺、乙烯基甲酰胺和赖氨酸作为重复单元的共聚物。这些含氨基的聚合物与属于酚或醌或含有酚型或醌型结构单元的芳族化合物,尤其与苯醌在迈克尔反应(R1)中的反应产物,或与苯酚或邻苯二酚在醛存在下在曼尼希反应(R2)中的反应产物在现有技术中是未知的。
本说明书因此进一步提供了由如下组分构成的聚合物:
a)作为组分A′a的由选自乙烯基胺、乙烯基甲酰胺和赖氨酸中的至少一种重复单元构成的至少一种聚合物或共聚物,
b)作为组分A′b的苯醌、苯酚或邻苯二酚,和
c)视需要而定的作为组分A′c的醛。
在上文中在组分Ac下已经列举了合适的醛类。同样在上文中已经列举了用于制备本发明聚合物的合适方法。
这些聚合物尤其适用于本发明组合物和用于处理金属或塑料表面的本发明方法中,优选用于处理金属表面,以及用于处理金属或塑料表面,优选用于金属表面的腐蚀抑制。
下列实施例进一步说明本发明。
实施例
组分A的制备实施例
实施例A1-A3
向N1份的聚乙烯基胺水溶液(去离子形式的聚合物,11.15%水溶液,该聚合物的K值)*:36;通过聚乙烯基甲酰胺的水解制备,水解度:96.2%,对应于243.5mmol的胺/100g聚合物)中,先后添加N2份邻苯二酚和N3份的37%浓度的甲醛水溶液。将反应混合物在60℃下加热1小时,在冷却之后用作组分A。
)*K值是用于表征平均分子量的Fikentscher常数;参见H.-G.Elias,大分子(Makromoleküle),第1卷,第5辑,Hüthig & Wepf Verlag,Basel1990,第99页。
份数 | 实施例A1 | 实施例A2 | 实施例A3 |
N1 | 208.3g | 188.3g | 282.5g |
N2 | 0.55g | 0.022g | 0.003g |
N3 | 0.41g | 0.016g | 0.002g |
实施例A4
将0.275g邻苯二酚加入32g聚赖氨酸在62.7g水中的溶液中。将该反应混合物加热到60-70℃,再添加0.203g甲醛水溶液(37重量%)。在冷却之后,将该反应产物用作组分A。
实施例A5
在冷却的同时,将0.081g对苯醌加入50g聚乙烯亚胺(Lupasol PR 8515,来自BASF Aktiengesellschaft,Ludwigshafen/Rhein)和100g水的混合物中。将该反应产物用作组分A。
实施例A6-A9
在冷却的同时,将0.083g邻苯二酚加入N4份的聚合物和100g水的混合物中。在室温下,添加0.203g甲醛水溶液(37重量%),然后将混合物加热到60-70℃。在冷却之后,将该反应产物用作组分A。
实施例A6 | 实施例A7 | 实施例A8 | 实施例A9 | |
N4 | 150g聚乙烯亚胺(LupasolPR 8515,来自BASFAktiengesellschaft,Ludwigshafen/Rhein) | 154g聚乙烯基胺 | 100g聚(乙烯基胺-乙烯基甲酰胺)和20g聚乙烯基甲酰胺的混合物 | 546g聚赖氨酸和150g水的混合物 |
本发明方法的实施例
实施例B1-B4
将电解法镀锌的钢板用下列配制剂通过在50℃下浸渍60秒钟而处理:
实施例B1 | 实施例B2 | 实施例B3 | 实施例B4 | |
实施例A1的反应产物 | 60 | 60 | ||
实施例A2的反应产物 | 50 | |||
实施例A6的反应产物 | 40 | |||
MgCl2 | 8.5 | |||
乙酸钠 | 45 | 8.5 | ||
甲酸钠 | 80 | 64 | ||
65%硝酸 | 40mL/L | |||
H2SO4 | 5.5 | |||
H3PO4 | 16 | |||
NaNO3 | 50 | |||
甲酸 | 75 | |||
乙酸 | 16 |
除非另有规定,表中的数字表示按g/L计的各物质在水中的浓度。
实施例B5-B8
与B1-B4相同,但使用电解法镀有ZnFe(10重量%Fe含量)的钢板。
实施例B9
将铝板于15A/dm2电流密度和100℃下在具有以下组成的溶液中进行阳极化处理:
H3PO4:70重量%,H2SO4:10重量%,HNO3:4重量%,硼酸:0.5重量%,NH5F2:16重量%,实施例(A2)的反应产物:9.5重量%。
实施例B10
将铸铁于室温下在10%H2SO4和30重量%的实施例A5的反应产物的溶液中浸渍15秒钟。
实施例B11
将100g聚合物分散体(30%固体含量,由具有如下组成的共聚物组成:47重量%丙烯酸正丁酯、50重量%苯乙烯和3重量%丙烯酸)与100g水和2g实施例A1的反应产物混合,再用于涂覆用HNO3(0.05重量%)钝化的镀锌钢板。
实施例B12:锌合金的电化学沉积
对于在40℃和1.5A/dm2的电流密度下电化学沉积包含锌和其它金属M的合金涂层,使用具有以下组成的电镀浴:
10g/L 锌,按氧化锌计
2g/L 金属M,按硫酸盐计
100g/L 氢氧化钠
15g/L 羧甲基化聚乙烯亚胺,Na盐,来自实施例1
5g/L 聚乙烯亚胺,LugalvanG20,来自BASF Aktiengesellschaft,
Ludwigshafen/Rhein
5g/L 实施例A3的反应产物
1g/L 吡啶鎓丙基磺基甜菜碱
金属M任选是钴、铁、镍或锰。
性能试验B1-B12
对实施例B1-B11的产物进行盐喷试验,结果具有比不使用聚合物C的对比方法长5-30%的耐久时间。
薄板试验
将1g化合物Al-A9各自加入99g 0.04M NaCl水溶液中。将已知质量的钢板(1.0037)置于溶液中,并在其中保持7天。然后清除钢片上附着的锈,冲洗,干燥并称重。按如下由相对于没有腐蚀抑制剂的储存质量损失Δm0的储存质量损失Δm样品来计算各物质A1-A9的抑制效力:
E=(Δm0-Δm样品)/Δm0
对于化合物A1-A9,E是5-50%。
磷酸盐化试验
将物质A1-A9各自在以下试验中用作试验物质:
磷酸盐化溶液A:25g磷酸(85%),10g乙酸钠,5g试验物质,960g水
磷酸盐化溶液B:25g磷酸(85%),10g乙酸钠,15g试验物质,950g水
磷酸盐化溶液C:25g磷酸(85%),10g乙酸钠,45g试验物质,920g水
磷酸盐化溶液D(对比实验):25g磷酸(85%),10g乙酸钠,965g水
在各自情况下,将钢板按如下进行处理:(1)清洗钢板//(2)在流水下冲洗(20秒)//(3)浸入90℃的磷酸盐化溶液中//(4)在流水下冲洗(20秒)//(5)吹干//(6)在空气(23℃,50%湿度)中贮存1周。
钢板1:在溶液A中1分钟
钢板2:在溶液A中25分钟
钢板3:在溶液B中5分钟
钢板4:在溶液C中1分钟
钢板5:在溶液C中25分钟
钢板6:在溶液D中1分钟
钢板7:在溶液D中25分钟
对于所有物质A1-A9,钢板1-5显示了比钢板6和7明显更少的生锈。
Claims (14)
1、一种用于处理金属表面的组合物,包含如下组分:
a)作为组分A的至少一种聚合物,其由如下组分构成:
aa)作为组分Aa的至少一种含氨基的聚合物;
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元;
ac)视需要而定的作为组分Ac的醛;
b)作为组分B的水或适于溶解、分散、悬浮或乳化聚合物(组分A)的其它溶剂;
c)视需要而定的作为组分C的表面活性化合物、分散剂、悬浮介质和/或乳化剂。
2、一种用于使金属或金属合金在塑料表面上沉积的组合物,包含如下组分:
a)作为组分A的至少一种聚合物,其由如下组分构成:
aa)作为组分Aa的至少一种含氨基的聚合物;
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元;
ac)视需要而定的作为组分Ac的醛;
b)作为组分B的水或适于溶解、分散、悬浮或乳化聚合物(组分A)的其它溶剂;
c)视需要而定的作为组分C的表面活性化合物、分散剂、悬浮介质和/或乳化剂。
3、如权利要求1所要求的组合物,除了组分A、B和视需要而定的C以外进一步包含如下组分:
d)作为组分D的以过渡金属阳离子、过渡金属氧合阴离子、含氟金属酸根或镧系元素为基础的至少一种盐、酸或碱,和/或
e)作为组分E的选自磷酸、硫酸、磺酸、硝酸、氢氟酸和盐酸中的至少一种酸,和/或
f)作为组分F的至少一种其它腐蚀抑制剂,和/或
g)作为组分G的Ce、Ni、Co、V、Fe、Zn、Zr、Ca、Mn、Mo、W、Cr和/或Bi的化合物,和/或
h)作为组分H的其它助剂和添加剂。
4、如权利要求1或2所要求的组合物,除了组分A、B和视需要而定的C以外还进一步包含如下组分:
i)作为组分I的至少一种金属氧化物和/或金属盐,
j)视需要而定的作为组分J的至少一种配合剂,
k)视需要而定的作为组分K的至少一种酸或相应酸的碱金属盐或碱土金属盐,和
l)视需要而定的作为组分L的其它添加剂。
5、一种处理金属表面的方法,包括使金属表面与由如下组分构成的聚合物(组分A)接触:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
6、如权利要求5所要求的方法,其中使金属表面与如权利要求1或3所要求的组合物接触。
7、如权利要求6所要求的方法,包括如下步骤:
a)视需要而定,清洗金属表面,以便去除油、油脂和灰尘,
b)视需要而定,用水洗涤,
c)视需要而定,在有或无根据本发明使用的聚合物(组分A)存在下进行酸洗,以便去除锈或其它氧化物,
d)视需要而定,用水洗涤,
e)在根据本发明使用的聚合物(组分A)存在下处理金属表面,
f)视需要而定,用水洗涤,
g)视需要而定,在有或无根据本发明使用的聚合物(组分A)存在下进行后处理。
8、如权利要求5所要求的方法,其中使金属表面与如权利要求2或4所要求的组合物接触。
9、一种使金属或金属合金在塑料表面上沉积的方法,包括使塑料表面与由如下组分构成的聚合物(组分A)接触:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
10、如权利要求9所要求的方法,其中使塑料表面与如权利要求2或4所要求的组合物接触。
11、如权利要求8或10所要求的方法,其中进行化学或电化学金属沉积。
12、由如下组分构成的聚合物在处理金属表面中的用途:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
13、由如下组分构成的聚合物在使金属或金属合金在塑料表面上沉积中的用途:
aa)作为组分Aa的至少一种含氨基的聚合物,
ab)作为组分Ab的至少一种芳族化合物,其为酚或醌,或含有酚型或醌型结构单元,和
ac)视需要而定的作为组分Ac的醛。
14、一种聚合物,由如下组分构成:
a)作为组分A′a的由选自乙烯基胺、乙烯基甲酰胺和赖氨酸中的至少一种重复单元构成的至少一种聚合物或共聚物,
b)作为组分A′b的苯醌、苯酚或邻苯二酚,和
c)视需要而定的作为组分A′c的醛。
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DE10164671.2 | 2001-12-27 | ||
DE10164671A DE10164671A1 (de) | 2001-12-27 | 2001-12-27 | Derivate von Polymeren für die Metallbehandlung |
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CN1620523A true CN1620523A (zh) | 2005-05-25 |
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CNA028280458A Pending CN1620523A (zh) | 2001-12-27 | 2002-12-27 | 用于处理金属的聚合物衍生物 |
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US (1) | US20050126427A1 (zh) |
EP (1) | EP1461471A2 (zh) |
JP (1) | JP2005513275A (zh) |
KR (1) | KR20040073527A (zh) |
CN (1) | CN1620523A (zh) |
AU (1) | AU2002360089A1 (zh) |
CA (1) | CA2472120A1 (zh) |
DE (1) | DE10164671A1 (zh) |
MX (1) | MXPA04006294A (zh) |
PL (1) | PL371192A1 (zh) |
WO (1) | WO2003056062A2 (zh) |
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-
2001
- 2001-12-27 DE DE10164671A patent/DE10164671A1/de not_active Withdrawn
-
2002
- 2002-12-27 CN CNA028280458A patent/CN1620523A/zh active Pending
- 2002-12-27 AU AU2002360089A patent/AU2002360089A1/en not_active Abandoned
- 2002-12-27 PL PL02371192A patent/PL371192A1/xx not_active Application Discontinuation
- 2002-12-27 CA CA002472120A patent/CA2472120A1/en not_active Abandoned
- 2002-12-27 US US10/500,313 patent/US20050126427A1/en not_active Abandoned
- 2002-12-27 JP JP2003556576A patent/JP2005513275A/ja not_active Withdrawn
- 2002-12-27 EP EP02795278A patent/EP1461471A2/de not_active Withdrawn
- 2002-12-27 WO PCT/EP2002/014786 patent/WO2003056062A2/de not_active Application Discontinuation
- 2002-12-27 KR KR10-2004-7010239A patent/KR20040073527A/ko not_active Application Discontinuation
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2004
- 2004-06-25 MX MXPA04006294A patent/MXPA04006294A/es unknown
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CN117384503A (zh) * | 2023-10-13 | 2024-01-12 | 青岛恩泽化工有限公司 | 一种高效缓释防闪锈剂的制备方法及其应用 |
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Also Published As
Publication number | Publication date |
---|---|
WO2003056062A3 (de) | 2004-01-15 |
JP2005513275A (ja) | 2005-05-12 |
MXPA04006294A (es) | 2004-10-04 |
CA2472120A1 (en) | 2003-07-10 |
EP1461471A2 (de) | 2004-09-29 |
US20050126427A1 (en) | 2005-06-16 |
PL371192A1 (en) | 2005-06-13 |
DE10164671A1 (de) | 2003-07-10 |
WO2003056062A2 (de) | 2003-07-10 |
AU2002360089A1 (en) | 2003-07-15 |
KR20040073527A (ko) | 2004-08-19 |
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