CN1633478A - MoO3作为腐蚀抑制剂的用途,以及含有这种腐蚀抑制剂的涂料组合物 - Google Patents
MoO3作为腐蚀抑制剂的用途,以及含有这种腐蚀抑制剂的涂料组合物 Download PDFInfo
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Abstract
本发明的主题是MoO3作为腐蚀抑制剂的用途以及用于金属零件的防腐蚀涂料组合物,其特征在于含有:至少一种粒状金属;一种有机溶剂;一种增稠剂;一种硅烷基粘合剂,优选为带有环氧官能基;氧化钼(MoO3);可能还含有一种钠、钾或锂的硅酸盐;和水。
Description
本发明的目的是研制一种用于金属零件的防腐蚀涂料,优选为一种不含六价铬的涂料,它具有改良的防腐蚀性能。
本发明适用于任何类型的金属零件,尤其是钢或铸铁制品,它们需要具备良好的防腐蚀性能,例如因为它们要应用于机动车工业。只要防腐蚀组合物能够通过可靠的工业化过程进行使用,要处理的零件的几何形状并不重要。
具体而言,本发明的目的之一是改进用配方中不含六价铬成分的涂料处理的零件的防腐蚀性能。
迄今为止,已经提出了许多以六价铬为原料的防腐蚀处理用溶液。尽管在处理过的金属零件的保护性方面,它们通常是令人满意的,然而,它们正受到越来越多的批评,因为使用它们要承担中毒的风险,尤其因为它们对环境具有负面的影响。
因此,各种不含六价铬的防腐蚀处理组合物已经被推荐使用。这些组合物中的一些是基于一种特定的金属,例如锌或铝。然而,如果这些组合物呈现水分散体形态,那么它们的稳定性就会受到限制。因此不能长期保存和存储。
在本发明中,申请人发现通过加入氧化钼MoO3作为腐蚀抑制剂,可以改进各种防腐蚀涂料组合物的防腐蚀性能和稳定性。
迄今为止,氧化钼MoO3在水相体系中用作腐蚀抑制剂还并不为人所知。某些钼酸盐,例如MoO4 2-离子已经被提出用作腐蚀抑制剂。然而,申请人能够证实在相当多的传统防腐蚀组合物中,加入一种钼酸盐,如钼酸锌,无论如何也不能改进其性能。
更具体地说,本发明涉及氧化钼MoO3作为用于增强涂料组合物的防腐性能的制剂的应用,该涂料组合物基于含锌或锌合金的粒状金属。这一发现甚至已扩展影响到含六价铬的组合物。这是本发明的另一目的。
在一种以粒状金属为原料的防腐蚀涂料组合物的具体情况中,氧化钼MoO3的存在似乎可以改进牺牲阳极保护法的控制,该牺牲阳极保护是通过组合物中悬浮体中的粒状金属进行的。要说明的是,本发明无论如何都不限于这种解释。
本发明的一个具体特征是,粒状金属具有层状形态,其中的薄片厚度在0.05μm和1μm之间,用激光衍射测定的直径当量(diameterequivalent)(D50)在5μm和25μm之间。更确切地说,本发明的主题是氧化钼MoO3在含锌的水相组合物中的使用。
本发明另一特征是使用的氧化钼MoO3基本上是纯净的正交晶体形态,钼含量高于大约60%(质量百分比)。
有益的是,在防腐蚀组合物中使用的氧化钼MoO3的形态是尺寸在1μm和200μm之间的微粒。
更确切地说,本发明的主题是用于金属零件的防腐蚀涂料组合物,其含有:
-至少一种粒状金属;
-一种有机溶剂;
-一种增稠剂;
-一种硅烷基粘合剂,优选为带有环氧官能基;
-氧化钼(MoO3);
-可能还含有一种钠、钾或锂的硅酸盐;和
-水。
在这样的组合物中,各种成分的相对比例可以在很大范围内变动。然而,氧化钼MoO3的含量优选为占整个组合物重量的0.5wt%和7wt%之间,更优选为在2wt%左右。
组合物中的粒状金属可以选自锌、铝、铬、镁、镍、钛、它们的合金和金属间化合物、以及上述物质的混合物。这里要指出的是如果推荐的涂料组合物优选为不含CrVI,但它也可以含有一定比例的金属铬。实际上,结果表明存在锌是非常理想的。
有益的是,粒状金属含量为相对于组合物重量的10wt%至40wt%。
优选地,本发明的防腐蚀涂料组合物中含有锌和/或铝,优选为含有锌。
如上所述,这种类型的组合物主要是水性的,因此优选为含有30wt%至60wt%的水。该组合物中还可以添加一种有机溶剂,优选为一种水溶性有机溶剂,这样可以改进组合物的防腐蚀性能。出于这种目的,该组合物含有,例如占组合物总重量的1wt%至30wt%的有机溶剂。然而,重要的是有机溶剂的含量不要超过大约30%。
在本发明的有利实施方案中,组合物中将使用一种有机溶剂,例如含有一种乙二醇醚,特别是二甘醇、三甘醇和双丙二醇。
本发明的另一特征是,防腐蚀组合物还含有0.005wt%至2wt%的增稠剂,特别是纤维素衍生物,更具体地说是羟甲基纤维素、羟乙基纤维素、羟丙基纤维素、羟丙基甲基纤维素、黄原酸胶或一种聚氨酯或丙烯酸类缔合性增稠剂。
本发明的组合物还含有二氧化硅或亲有机物质的粘土类矿物流变剂。
这种组合物中还使用了一种粘合剂,优选为有机官能硅烷,用量为3wt%至20wt%。有机官能基可以是乙烯基、甲基丙烯酰氧基和氨基,但优选为环氧官能,用以提高涂料性能和组合物的稳定性。有益的是,硅烷可以容易地分散在水介质中,优选为可溶于该种介质。优选地,有用的硅烷是一种环氧官能硅烷,例如β(3,4-环氧环己基)乙基三甲氧基硅烷、4(三甲氧基甲硅烷)丁烷-1,2环氧化物或γ-环氧丙氧基丙基-三甲氧基硅烷。
最后,本发明的防腐蚀涂料组合物还含有,除前述有机溶剂外,最大含量为大约10wt%的石油溶剂,以改进防腐蚀组合物通过喷涂、浸涂、浸渍-离心涂布施用于金属零件的能力。
有益的是,组合物中还含有一种钠、钾或锂的硅酸盐,含量优选为0.05wt%至0.5wt%。
很自然地,本发明也涉及使用前述组合物施用于金属零件的防腐蚀涂层,其通过喷涂、浸涂、浸渍-离心涂布(dip-spinning)技术进行涂布,然后在70℃至350℃之间进行固化,固化时间为大约30分钟。
按照有利实施方案,防腐蚀涂层产自下述操作:在固化操作之前,将已涂布的金属零件干燥,优选为在70℃左右干燥大约20分钟。在这些条件下,涂层的厚度在3μm和15μm之间,优选为在5μm和10μm之间。
下文所述的作为比较的实施例中,对各种腐蚀抑制剂进行测试,以便改进各种组合物,特别是参比组合物GEOMET(在作为参考的美国专利5,868,819中进行了描述)的防腐蚀性能。
这些是主要的可通过商业途径获得的腐蚀抑制剂。它们按照宽的化学类别列于下表,标明产品的来源、名称及其组成。
◆改性的磷酸锌
厂商:Heubach:
HEUCOPHOSZPA: 水合锌铝正磷酸盐
HEUCOPHOSZMP: 水合锌钼正磷酸盐
HEUCOPHOSSAPP:水合锶铝多磷酸盐(SrO:31%;Al2O3:
12%;P2O5:44%;MgSiF6:0.3%)
HEUCOPHOSSRPP:水合锶铝多磷酸盐(SrO:28%;Al2O3:
12%;P2O5:42%)
HEUCOPHOSZCP:水合锌钙锶硅酸盐正磷酸盐
HEUCOPHOSZCPP:水合锌钙铝锶硅酸盐正磷酸盐(ZnO:
37%;SrO:5%;Al2O3:3%;P2O5:18%;
CaO:14%;SiO2:14%)
HEUCOPHOSCAPP:水合钙铝硅酸盐多磷酸盐(Al2O3:7%;
P2O5:26%;CaO:31%;SiO2:28%)
厂商:Devineau:
ACTIROX213:锌铁磷酸盐(ZnO:66%;PO4:48%;Fe2O3:
37%)
厂商:Lawrence Industries:
HALOXSZP 391 锌钙锶磷硅酸盐
HALOXCZ 170 正磷酸锌
厂商:Tayca:
K WHITE84: 三磷酸铝(ZnO:26.5-30.5%;Al2O3:9-13%;
P2O5:36-40%;SiO2:11-15%)
◆钼酸盐
厂商:Devineau:
ACTIROX102: 偶合至磷酸锌改性剂的钼酸锌(ZnO:
63%;PO4:46%;MoO3:1%)
ACTIROX106: 偶合至磷酸锌改性剂的钼酸锌(ZnO:
67%;PO4:46%;MoO3:1%)
厂商:Sherwin Willianms:
MOLY WHITEMAZP: ZnO、CaCO3、Zn3(PO4)2、CaMoO4
MOLY WHITE212: ZnO、CaCO3、CaMoO4
钼酸钠: NaMoO4
◆硼酸盐
厂商:Buckman:
BUTROL23: 偏硼酸钙
BUSAN11M2: 偏硼酸钡
厂商:Lawrence Industries:
HALOXCW 2230 硼硅酸钙
◆掺钙二氧化硅:
厂商:Grace:
SHIELDEXAC5
◆锌盐:
厂商:Henkel:
ALCOPHOR827 有机锌盐
◆有机抑制剂:
厂商:Ciba-Geigy:
IRGACOR1930: 锆和4-甲基-γ-氧苯丁酸的络合物
IRGACOR1405: 4-氧-4-对甲苯丁酸与4-乙基吗啉
CGCI(IRGACOR287): 聚胺盐
厂商:Lawrence Industries:
HALOX FLASHX 硼酸、磷酸、三乙醇胺盐、2-二甲基-氨基
乙醇
◆锌减活剂:
厂商:Ciba-Geigy:
IRGACOR42: 2,2[[(5-甲基-1H-苯并三唑-1-基)甲基]亚
氨基]双乙醇
IRGACORBTA M: 1H-苯并三唑
实施例1
标准参比GEOMET组合物相当于:
去离子水 38.60%
DPG 10.29%
硼酸 0.65%
SYMPERONICNP4 1.51%
SYMPERONICNP9 1.64%
SILQUESTA187 8.66%
锌* 32.12%
铝** 5.08%
SCHWEGO FOAM 0.4%
NIPARS10 0.71%
AEROSOLTR70 0.53%
*在石油溶剂中大约95%的糊状存在的薄片状锌:ECKART WERKE的锌31129/93;
**在DPG中大约70%的糊状存在的薄片状铝:ECKART WERKE的CHROMAL VIII。
为了对前述抑制剂进行各种参比试验,将1g抑制剂加入9ml水中制成不同的浴,将分散液维持1小时,然后将混合物加入90g前述标准GEOMET组合物中,然后搅拌3小时。
使用No.38 Conway棒涂敷被测试的这种组合物的第一层。在70℃干燥大约20分钟,然后在300℃固化大约30分钟。
第二层用同样的方法进行涂敷。
然后将处理过的板在盐喷雾中进行测试。不同涂料的抗盐喷雾结果在下表中列出。
表1
抑制剂种类 | 抑制剂名称 | 在盐雾中无红锈的小时数 |
参比 | GEOMET | 112 |
改性锌磷酸盐 | GEOMET+ZPA | 134 |
GEOMET+ZMP | 122 | |
GEOMET+SAPP | 66 | |
GEOMET+SRPP | 66 | |
GEOMET+ZCP | 66 | |
GEOMET+ZCPP | 88 | |
GEOMET+CAPP | 66 | |
GEOMET+ACTIROX 213 | 66 | |
GEOMET+HALOX 391 | 66 | |
GEOMET+K WHITE 84 | 88 | |
钼酸盐 | GEOMET+ACTIROX 102 | 66 |
GEOMET+ACTIROX 106 | 88 | |
GEOMET+MW 212 | 88 | |
GEOMET+MW MZAP | 88 | |
GEOMET+Na2MoO4 | 66 | |
硼酸盐 | GEOMET+BUTPOL | 44 |
GEOMET+BUSAN | 112 | |
GEOMET+HALOX 2230 | 66 | |
各种各样的 | GEOMET+SHIELDEX | 112 |
GEOMET+ALCOPHOR 827 | 66 |
GEOMET+IRGACOR 1930 | 88 | |
GEOMET+IRGACOR 1405 | 88 | |
GEOMET+CGCI | 88 | |
GEOMET+HALOXFLASHX | 66 | |
GEOMET+IRGAMET 42 | 44 | |
GEOMET+IRGAMET BTAM | 66 | |
本发明的 | GEOMET+MoO3 | 518 |
MoO3:来自CLIMAX公司的POR
此外,更详细的抗盐雾结果与所述浴持续时间的函数图,以及它分别在4℃和20℃时的稳定性,在附图1和2中列出。
这些图都清楚地表明,在每一试验中,一方面,含氧化钼MoO3的组合物的防腐蚀性能明显地提高了,另一方面,当组合物中加入氧化钼时,防腐蚀性能随着时间保持得更好。
实施例2
进行两种其它的参比试验,一种是GEOMET组合物,另一种是六价铬类DACROMET组合物。
这些组合物的配方在下表中列出。
表2
GEOMET
原材料 | 不含MoO3的浓度% | 含MoO3的浓度% |
去离子水 | 38.60 | 37.83 |
DPG | 10.29 | 10.08 |
硼酸 | 0.65 | 0.64 |
SYMPERONICNP4 | 1.51 | 1.48 |
SYMPERONICNP9 | 1.64 | 1.61 |
SILQUESTA187 | 8.66 | 8.47 |
锌* | 32.12 | 31.48 |
铝** | 5.08 | 4.98 |
SCHWEGO FOAM | 0.4 | 0.21 |
NIPARS10 | 0.71 | 0.70 |
AEROSOLTR70 | 0.53 | 0.52 |
MoO3 *** | 0 | 2 |
*在石油溶剂中以大约95%的糊状存在的薄片状的锌:ECKARTWERKE的锌31129/93;
**在DPG中以大约70%的糊状存在的薄片状的铝:ECKART WERKE的CHROMAL VIII;
***MoO3:CLIMAX公司的POR
SYMPERONIC:非离子型表面活性剂
SILQUESTA187:γ-环氧丙氧丙基三甲氧基硅烷
SCHWEGO FOAM:烃类防泡剂
NIPARS10:硝基丙烷
AEROSOLTR70:阴离子表面活性剂
表3
DACROMET
原材料 | 不含MoO3的浓度% | 含MoO3的浓度% |
去离子水 | 47.86 | 44.90 |
DPG | 15.95 | 15.63 |
PGME乙酸盐 | 1.56 | 1.53 |
铬酸 | 3.81 | 3.73 |
REMCOPAL334 | 0.72 | 0.71 |
REMCOPAL339 | 0.72 | 0.71 |
锌* | 23.61 | 23.14 |
铝** | 3.06 | 3.00 |
硼酸 | 1.30 | 1.27 |
ZnO | 1.41 | 1.38 |
MoO3 *** | 0 | 2 |
*在石油溶剂中以大约95%的糊状存在的薄片状的锌:ECKARTWERKE的锌31129/93;
**在DPG中以大约70%的糊状存在的薄片状的铝:ECKART WERKE的CHROMAL VIII;
***MoO3:CLIMAX公司的POR
REMCOPAL:非离子型表面活性剂
必须注意的是氧化钼粉末每次都通过撒粉的方式加入GEOMET或DACROMET浴中的。使用分散叶片以450转每分钟进行搅拌,从而使浴均化。
通过使用Conway棒进行涂布,将试验的防腐蚀组合物涂敷于10cm×20cm冷轧低碳钢板上,随后在70℃预干燥大约20分钟,然后在300℃的烘箱中固化30分钟。
如果是应用于螺丝,则组合物通过浸渍-离心法进行涂敷,然后在与板同样的条件下进行固化。
按照ISO 9227标准观察到的抗盐雾结果在下表中列出:
表4
产品 | 底材 | 涂层重量** | 抗盐雾性* | |
不含MoO3 | 含2%MoO3 | |||
水相GEOMET | 板 | 32 | 288 | >840 |
水相GEOMET | 螺丝 | 30 | 144 | 504 |
DACROMET | 螺丝 | 24 | 600 | 744 |
*暴露在盐雾中直至出现红锈时的小时数
**每平方米涂布表面上的克数,涂层的厚度在大约6μm和8μm之间。
因此,很明显,在水相组合物中,含粒状锌的GEOMET或DACROMET中加入氧化钼MoO3,非常充分地改进了所述组合物的抗盐雾性。
本发明的另一方面在于,在组合物中加入0.05wt%至0.5wt%的碱性硅酸盐。
碱性硅酸盐,例如硅酸钠的加入,出人意料地在相当程度上增强了薄膜粘结力。
在表5中列出的参比例中对此进行了详细的阐述。
实施例3
在此实施例中,将一张透明粘合纸粘在涂层表面,然后迅速将其撕去。按照0(涂层膜完全脱落)至5(涂层膜没有任何脱落)的等级评估粘结力。
表5
原材料 | 不含硅酸盐的组合物(浓度%) | 含硅酸盐的组合物(浓度%) |
去离子水 | 38.13 | 37.96 |
双丙甘醇 | 10.08 | 10.08 |
硼酸 | 0.64 | 0.64 |
Sympéronic NP4 | 1.48 | 1.48 |
Sympéronic NP9 | 1.61 | 1.61 |
硅烷A187 | 8.47 | 8.47 |
锌31129/93 | 31.48 | 31.48 |
铝CHROMAL VIII | 4.98 | 4.98 |
Schwegofoam | 0.21 | 0.21 |
NIPARS10 | 0.7 | 0.7 |
AEROSOLTR70 | 0.52 | 0.52 |
MoO3 *** | 1 | 1 |
级别为42的纳的硅酸盐 | 0 | 0.17 |
黄原酸胶(1) | 0.7 | 0.7 |
(1)在使用过程中用来控制组合物粘度的增稠剂
将组合物用Conway棒涂敷在已经去除油脂的钢板上,以使涂层重量为30g/m2。然后将板在前述条件下进行固化。
然后按照ISO 9227对它们进行盐雾试验和粘结力试验。结果列在下表6中。
表6
不含碱性硅酸盐 | 含碱性硅酸盐 | |
盐雾(红锈出现前的小时数) | 694 | 720 |
粘结力 | 1/5 | 5/5 |
此表表明尽管抗蚀性能没有显著改善,但反之粘结力却得到高度改善。
Claims (24)
1.MoO3作为增强水相防腐蚀涂料组合物的防腐蚀性能的制剂的应用,该涂料组合物基于一种含锌或锌合金的粒状金属。
2.如权利要求1所述的应用,用于改进粒状金属,优选以薄片状形式使用的金属发挥出的牺牲阳极保护的效力。
3.如权利要求1或2所述的应用,其特征在于所述防腐蚀涂料组合物含有30wt%至60wt%的水。
4.如权利要求1-3任一项所述的应用,其特征在于所述防腐蚀涂料组合物含有硅烷基粘合剂,优选带有环氧官能基。
5.如权利要求1-4任一项所述的应用,其特征在于氧化钼MoO3是基本上纯净的正交晶体形态,钼含量高于大约60质量%。
6.如权利要求1-5任一项所述的应用,其特征在于氧化钼MoO3是尺寸在1μm和200μm之间的微粒。
7.如权利要求1-6任一项所述的应用,其特征在于所述防腐蚀涂料组合物含有一种钠、钾或锂的硅酸盐,优选为含量在0.05wt%和0.5wt之间。
8.用于金属零件的防腐蚀涂料组合物,其特征在于它含有:
-至少一种粒状金属;
-一种有机溶剂;
-一种增稠剂;
-一种硅烷基粘合剂,优选带有环氧官能基;
-氧化钼(MoO3);
-可能还含有一种钠、钾或锂的硅酸盐;和
-水。
9.如权利要求8所述的金属零件防腐蚀涂料组合物,其特征在于它含有0.5wt%和7wt%,优选为大约2wt%的氧化钼(MoO3)。
10.如权利要求8所述的金属零件防腐蚀涂料组合物,其特征在于它含有10wt%和40wt%的至少一种粒状金属。
11.如权利要求8-10任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述粒状金属选自锌、铝、铬、镁、镍、钛、它们的合金和金属间化合物、以及上述物质的混合物。
12.如权利要求8-11任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述粒状金属选自薄片状锌和/或薄片状铝,优选为含有薄片状锌。
13.如权利要求8-12任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述有机溶剂的含量为组合物总重量的1wt%至30wt%。
14.如权利要求12所述的金属零件防腐蚀涂料组合物,其特征在于所述有机溶剂是一种乙二醇醚,特别是二甘醇、三甘醇和双丙二醇。
15.如权利要求8-14任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述组合物含有0.005wt%至2wt%的增稠剂,特别是纤维素衍生物,更具体地说是羟甲基纤维素、羟乙基纤维素、羟丙基纤维素、羟丙基甲基纤维素、黄原酸胶或一种聚氨酯或丙烯酸类缔合性增稠剂。
16.如权利要求8-15任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述组合物含有3wt%至20wt%的硅烷。
17.如权利要求8-16任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述硅烷包括γ-环氧丙氧基丙基-三甲氧基硅烷。
18.如权利要求8-17任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述有机溶剂还含有高达大约10wt%的石油溶剂。
19.如权利要求8-18任一项所述的金属零件防腐蚀涂料组合物,其特征在于所述组合物含有大约30wt%至60wt%水。
20.用于金属零件的防腐蚀涂层,其特征在于它是通过将权利要求8至19任一项所述的涂料组合物利用喷涂、浸涂、浸渍-离心涂布技术进行涂布获得的,所述涂层优选为在70℃至350℃之间进行固化处理。
21.如权利要求20所述的金属零件防腐蚀涂层,其特征在于所述固化处理进行大约30分钟。
22.如权利要求20所述的金属零件防腐蚀涂层,其特征在于在所述固化处理之前,将已涂层的金属零件进行干燥,优选为在70℃左右干燥大约20分钟。
23.如权利要求20-22任一项所述的金属零件防腐蚀涂层,其特征在于所述金属零件涂层的厚度在3μm和15μm之间,优选为在5μm和10μm之间。
24.一种由权利要求20-23任一项所述的防腐蚀涂层形成的已涂层金属底材。
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