CN113573899A - 包含导电性高分子的溶液组合物 - Google Patents
包含导电性高分子的溶液组合物 Download PDFInfo
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- CN113573899A CN113573899A CN202080024981.7A CN202080024981A CN113573899A CN 113573899 A CN113573899 A CN 113573899A CN 202080024981 A CN202080024981 A CN 202080024981A CN 113573899 A CN113573899 A CN 113573899A
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- solution composition
- resin
- conductive polymer
- polyaniline
- film
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- 239000000203 mixture Substances 0.000 title claims abstract description 83
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- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 20
- 229920000767 polyaniline Polymers 0.000 claims description 44
- 239000002019 doping agent Substances 0.000 claims description 34
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
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- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical group OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 claims description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims description 3
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- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 10
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
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- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
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- 239000011593 sulfur Substances 0.000 description 1
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- 229930192474 thiophene Natural products 0.000 description 1
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- 238000007740 vapor deposition Methods 0.000 description 1
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Abstract
溶液组合物,其包含导电性高分子、树脂和溶剂,且其酸值为0.0~14.5mgKOH/g、或者碱值为0.0~1.0mgHCl/g。
Description
技术领域
本发明涉及包含导电性高分子的溶液组合物。
背景技术
以往,已知有包含聚苯胺和作为涂膜成分的环氧树脂的溶液组合物(例如,参照专利文献1)。
此外,公开有一种防锈剂,其为含有分子结构中具有疏水基团和螯合基团的化合物、以及液状橡胶的组合物(例如,参照专利文献2)。
现有技术文献
专利文献
专利文献1:日本特开2007-324143号公报
专利文献2:日本特开2011-99152号公报。
发明内容
对于将如专利文献1那样的包含聚苯胺和作为涂膜成分的环氧树脂的溶液组合物涂布于铜板而形成的膜,若进行盐水喷雾试验(JIS Z 2371),则会剧烈生锈。因此,需求能够形成具有更高防锈性能的膜的溶液组合物。
本发明的课题是提供溶液组合物,其可得到能够进一步减少锈的发生的膜。
本发明人等为了解决上述课题而进行了深入研究,结果发现,通过控制组合物的酸值或碱值,所得的膜的防锈性能显著提高,从而完成了本发明。
根据本发明,可以提供以下的溶液组合物。
1. 溶液组合物,其包含导电性高分子、树脂和溶剂,且其酸值为0.0~14.5mgKOH/g、或碱值为0.0~1.0mgHCl/g。
2. 1所述的溶液组合物,其中,前述导电性高分子为聚苯胺系高分子。
3. 2所述的溶液组合物,其中,前述聚苯胺系高分子是掺杂有掺杂剂的取代或未取代的聚苯胺。
4. 1~3中任一项所述的溶液组合物,其特征在于,溶液组合物的粘度在25℃下为1000cP以上且80000cP以下。
5. 1~3中任一项所述的溶液组合物,其特征在于,溶液组合物的粘度在25℃下为1000cP以上且60000cP以下。
6. 3~5中任一项所述的溶液组合物,其中,前述掺杂剂为磺基琥珀酸衍生物。
7. 1~6中任一项所述的溶液组合物,其中,前述树脂为热固性树脂。
8. 7所述的溶液组合物,其中,前述热固性树脂是选自醇酸树脂、不饱和聚酯、聚酯、三聚氰胺树脂、聚异氰酸酯、丙烯酸类树脂、酚醛树脂、聚胺、聚氨酯和环氧树脂中的1种以上的树脂。
9. 7所述的溶液组合物,其中,前述热固性树脂是聚氨酯或环氧树脂。
10. 由1~9中任一项所述的溶液组合物得到的膜。
11. 金属构件,其包含10所述的膜。
12. 9所述的金属构件,其具有将钢材用前述膜被覆的结构。
根据本发明,可以提供溶液组合物,该组合物可得到能够进一步减少锈的发生的膜。
具体实施方式
作为本发明的一个实施方式的溶液组合物包含导电性高分子、树脂和溶剂。继而,溶液组合物的酸值为0.0~14.5mgKOH/g,或碱值为0.0~1.0mgHCl/g。通过将溶液组合物的酸值或碱值控制于上述范围,在将本实施方式的溶液组合物涂布和干燥而得的膜(固化膜)中,导电性高分子溶解或均匀分散于作为基质的树脂中。籍此,可以减少盐水喷雾试验所致的锈的发生,可得到具有优异防锈性能的膜。
本实施方式中,溶液组合物的酸值为0.0~14.5mgKOH/g。若酸值为14.5mgKOH/g以下(也包括酸值为0.0mgKOH/g的情形),则由于可以减少被防锈物因酸所致的腐蚀,因此可提高膜的防锈性能。酸值优选为0.0~10.0mgKOH/g、更优选为0.0~8.0mgKOH/g、进一步优选为0.2~3.0mgKOH/g。
另一方面,溶液组合物的碱值为0.0~1.0mgHCl/g。只要碱值为1.0mgHCl/g以下(也包括碱值为0.0mgHCl/g的情形),则可以抑制涂布于被防锈物后的干燥步骤中的导电性高分子的凝集,膜的均匀性提高。碱值优选为0.0~0.7mgHCl/g。更优选为0.0~0.5mgHCl/g。
酸值用中和溶液组合物1g中所含的酸性成分所需要的氢氧化钾(KOH)的mg数来表示。碱值用中和溶液组合物1g中所含的碱性成分所需要的盐酸(HCl)的mg数来表示。酸值和碱值通过对溶液组合物进行中和滴定而求出。
在使用如环氧树脂那样将主剂和固化剂混合而使用的树脂时,酸值和碱值通过对除去固化剂的溶液组合物进行中和滴定而求出。
溶液组合物的酸值和碱值可以通过,例如,利用公知的方法向导电性高分子和/或树脂中导入羟基、羧基之类的官能团来调节。此外,还可以通过后述掺杂剂的种类及其添加量来调节。
本发明中,“导电性高分子”意指氧化还原电位为-0.2(V vs. SHE)以上且1.5(Vvs. SHE)以下的氧化还原性物质。氧化还原电位的测定方法是:在溶解有0.1mol/l的支持电解质的电解液中使测定对象物质(化合物)分散或溶解,通过工作电极、参比电极和对电极的3电极式,通过读取工作电极相对于参比电极的自然电位的方法进行测定。此时,工作电极使用金。测定温度设为23℃。测定对象物质的溶解性低时,可以将该物质涂布于工作电极,浸渍于电解液中。在使用标准氢电极(SHE)以外的参比电极时,例如,若为饱和甘汞电极则从测得的电位减去0.24V、若为银氯化银电极则从测得的电位减去0.22V,换算为相对于氢电极电位的电位(V vs. SHE)(参照电化学便览第4版、77页、电化学协会编)。
导电性高分子的氧化还原电位可以为-0.2(V vs. SHE)以上、-0.15(V vs. SHE)以上、-0.1(V vs. SHE)以上、-0.05(V vs. SHE)以上或0(V vs. SHE)以上,此外,还可以为1.5(V vs. SHE)以下、1.3(V vs. SHE)以下、1.0(V vs. SHE)以下或0.8(V vs. SHE)以下。
作为导电性高分子的具体例,可举出聚乙炔、聚甲基乙炔、聚苯乙炔、聚氟乙炔、聚丁基乙炔、聚甲基苯基乙炔等聚乙炔系高分子;聚邻亚苯基、聚间亚苯基、聚对亚苯基等聚亚苯基系高分子;聚吡咯、聚(3-甲基吡咯)、聚(3-乙基吡咯)、聚(3-十二烷基吡咯)、聚(3,4-二甲基吡咯)、聚(3-甲基-4-十二烷基吡咯)、聚(N-甲基吡咯)、聚(N-十二烷基吡咯)、聚(N-甲基-3-甲基吡咯)、聚(N-乙基-3-十二烷基吡咯)、聚(3-羧基吡咯)等聚吡咯系高分子;聚噻吩、聚(3-甲基噻吩)、聚(3-乙基噻吩)、聚(3,4-二甲基噻吩)、聚(3,4-二乙基噻吩)、聚(3,4-乙烯二氧噻吩)等聚噻吩系高分子;聚呋喃;聚硒吩;聚异硫茚;聚苯硫醚;聚苯胺、聚(2-甲基苯胺)、聚(2-乙基苯胺)、聚(2,6-二甲基苯胺)等聚苯胺系高分子;聚亚苯基亚乙烯基、聚噻吩亚乙烯基、聚苝萘(ポリペリナフタレン)、聚蒽、聚萘、聚芘、聚薁、或这些树脂的衍生物等。
导电性高分子可以单独使用1种,或者也可以组合2种以上使用。
从稳定性、可靠性或入手的容易性等观点出发,导电性高分子优选为选自聚吡咯系高分子、聚噻吩系高分子和聚苯胺系高分子中的至少1种,进一步优选为聚苯胺系高分子。聚苯胺系高分子优选为取代或未取代的聚苯胺。
导电性高分子的制造方法没有特别限定,可以采用以往公知的方法。作为制造方法的具体例,可举出例如,化学聚合法、电解聚合法、可溶性前体法、基质(铸模)聚合法、蒸镀法(CVD等)。导电性高分子可以使用市售品。
在一个实施方式中,导电性高分子可以掺杂有掺杂剂。通过将掺杂剂添加至导电性高分子进行掺杂,可以适当且容易地调节溶液组合物的酸值和碱值。
掺杂剂掺杂于导电性高分子中可以通过紫外・可见・近红外分光法、X射线光电子分光法来确认。
作为掺杂剂的具体例,可举出氯离子、溴离子、碘离子等卤素离子;高氯酸根离子;四氟硼酸根离子;六氟砷酸根离子;硫酸根离子;硝酸根离子;硫氰酸根离子;六氟硅酸根离子;磷酸根离子、苯磷酸根离子、六氟磷酸根离子等磷酸根系离子;三氟乙酸根离子;甲苯磺酸根离子、乙基苯磺酸根离子、十二烷基苯磺酸根离子等烷基苯磺酸根离子;甲磺酸根离子、乙磺酸根离子、磺基琥珀酸衍生物的离子等烷基磺酸根离子;二苯并呋喃磺酸根离子、萘磺酸根离子;聚丙烯酸根离子、聚乙烯磺酸根离子、聚苯乙烯磺酸根离子、聚(2-丙烯酰胺-2-甲基丙磺酸)根离子等高分子离子等。应予说明,掺杂剂中除了上述离子之外,还可以含有未离子化的元素或化合物。
掺杂剂可以单独使用1种、或者也可以组合2种以上使用。
上述掺杂剂中,由于表现更高的溶解性,因此更优选聚苯乙烯磺酸、二(2-乙基己基)磺基琥珀酸等磺基琥珀酸衍生物(包括离子)。
在导电性高分子中掺杂的掺杂剂量,以掺杂剂比(掺杂剂/构成导电性高分子的单体单元:摩尔比)计,优选为0.1~1.0、更优选为0.15~0.75。
掺杂剂比意指掺杂剂(抗衡阴离子)相对于构成导电性高分子的单体单元的摩尔比。例如,包含未取代聚苯胺和掺杂剂的聚苯胺复合物的掺杂剂比为0.5意指相对于聚苯胺的单体单元分子2个,掺杂有1个掺杂剂。
掺杂剂比只要聚苯胺复合物中的掺杂剂与聚苯胺的单体单元的摩尔数能够测定就可以算出。例如,掺杂剂为有机磺酸时,通过有机元素分析法对来自掺杂剂的硫原子的摩尔数和来自聚苯胺的单体单元的氮原子的摩尔数进行定量,通过取这些值的比,可以算出掺杂剂比。其中,掺杂剂比的算出方法并不限于该方法。
本发明中,“树脂”意指不具有氧化还原功能、或者氧化还原电位为-0.2(V vs.SHE)以上且1.5(V vs. SHE)以下的范围外的高分子材料。
树脂只要可溶于溶剂则没有特别限定,优选为热固性树脂。热固性树脂通过化学反应,利用树脂分子间或树脂与固化剂间的反应形成的网孔结构而使硬度、耐候性、耐化学药品性、氧阻隔性等提高。此外,热固性树脂的分子量较低,容易处理。
作为热固性树脂,可举出例如,醇酸树脂、不饱和聚酯、聚酯、三聚氰胺树脂、聚异氰酸酯、丙烯酸类树脂、酚醛树脂、聚胺、聚氨酯、环氧树脂。
环氧树脂通过主剂和固化剂的配合来使用,作为主剂,可以从双酚A型、双酚F型、苯酚酚醛清漆型、胺类中适宜组合使用,作为固化剂,可以从酸酐型、脂环式胺型、苯酚型、酮亚胺型、咪唑型等中适宜组合使用。特别是在要求耐高温性的情形中,优选作为主剂的四缩水甘油基氨基二苯基甲烷、作为固化剂的二氨基苯基砜的组合。
热固性树脂可以单独使用1种、或者也可以组合2种以上使用。单独使用1种时,优选为聚氨酯。使用2种以上时,可以从聚酯和三聚氰胺树脂、聚酯和聚异氰酸酯、丙烯酸类树脂和三聚氰胺树脂、丙烯酸类树脂和聚异氰酸酯、环氧树脂和聚胺等组合中,根据用途、使用部位、使用环境而适宜选定。例如,环氧树脂的耐候性差,但是对金属的附着性良好,适于底涂。丙烯酸类树脂、聚酯的光泽、耐候性均优异,适于面涂。
本实施方式的溶液组合物,相对于导电性高分子100质量份,优选以500~100000质量份的范围含有上述树脂,进一步优选以1000~10000质量份的范围含有上述树脂。籍此,能够形成良好的膜,而且可以得到优异的防锈性能。
本实施方式的导电性高分子的分子量优选为5000~75000的范围。通过使导电性高分子的分子量为5000以上,可以维持氧化还原的可逆性,使防锈能力持续。此外,通过使导电性高分子的分子量为75000以下,可以维持溶剂溶解性,提高防锈能力。导电性高分子的分子量更优选为10000~60000的范围,进一步优选为15000~55000的范围。
溶剂只要是将上述导电性高分子和树脂溶解或分散的溶剂,则没有特别限制。作为溶剂的实例,可举出:水;
轻油、灯油、正戊烷、异戊烷、正己烷、异己烷、正庚烷、异庚烷、2,2,4-三甲基戊烷、正辛烷、异辛烷等脂肪族烃系溶剂;
苯、甲苯、二甲苯、苯酚、苯甲醚、苯甲酸、氢化石蜡等芳香族系烃系溶剂;
甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇、叔丁醇、正戊醇、异戊醇、2-甲基丁醇、仲戊醇、叔戊醇、3-甲氧基丁醇、3-甲氧基-3-甲基-1-丁醇、正己醇、2-甲基戊醇、仲己醇、2-乙基丁醇、仲庚醇、3-庚醇、正辛醇、2-乙基己醇、仲辛醇、正壬醇、2,6-二甲基-4-庚醇、正癸醇、仲十一烷醇、三甲基壬醇、仲十四烷醇、仲十七烷醇、苯酚、环己醇、甲基环己醇、3,3,5-三甲基环己醇、苯甲醇、苯基甲基卡必醇、双丙酮醇、甲酚等一元醇系溶剂;乙二醇、1,2-丙二醇、1,3-丁二醇、2,4-戊二醇、2-甲基-2,4-戊二醇、2,5-己二醇、2,4-庚二醇、2-乙基-1,3-己二醇、二甘醇、二丙二醇、三甘醇、三丙二醇、甘油等多元醇系溶剂;
丙酮、甲乙酮、甲基正丙基酮、甲基正丁基酮、二乙基酮、甲基异丁基酮、甲基正戊基酮、乙基正丁基酮、甲基正己基酮、二异丁基酮、三甲基壬酮、环己酮、甲基环己酮、2,4-戊二酮、丙酮基丙酮、双丙酮醇、苯乙酮、葑酮等酮系溶剂;
乙醚、异丙醚、正丁醚、正己醚、2-乙基己醚、环氧乙烷、1,2-环氧丙烷、二氧戊环、4-甲基二氧戊环、二噁烷、二甲基二噁烷、乙二醇单甲醚、乙二醇单乙醚、乙二醇二乙醚、乙二醇单丙醚、乙二醇单正丁醚、乙二醇单正己醚、乙二醇单苯基醚、乙二醇单苯氧基醚、乙二醇单-2-乙基丁醚、乙二醇二丁醚、二甘醇单甲醚、二甘醇单乙醚、二甘醇二乙醚、乙二醇单叔丁醚、乙二醇单异丁醚、二甘醇单正丁醚、二甘醇二正丁醚、二甘醇单正己醚、乙氧基三甘醇、四乙二醇二正丁醚、丙二醇单甲醚、丙二醇单乙醚、丙二醇单丙醚、丙二醇单丁醚、二丙二醇单甲醚、二丙二醇单乙醚、三丙二醇单甲醚、四氢呋喃、2-甲基四氢呋喃等醚系溶剂;
碳酸二乙酯、乙酸甲酯、乙酸乙酯、γ-丁内酯、γ-戊内酯、乙酸正丙酯、乙酸异丙酯、乙酸正丁酯、乙酸异丁酯、乙酸仲丁酯、乙酸正戊酯、乙酸仲戊酯、乙酸3-甲氧基丁酯、乙酸甲基戊酯、乙酸2-乙基丁酯、乙酸2-乙基己酯、乙酸苄酯、乙酸环己酯、乙酸甲基环己酯、乙酸正壬酯、乙酰乙酸甲酯、乙酰乙酸乙酯、乙酸乙二醇单甲醚、乙酸乙二醇单乙醚、乙酸二甘醇单甲醚、乙酸二甘醇单乙醚、乙酸二甘醇单正丁醚、乙酸丙二醇单甲醚、乙酸丙二醇单乙醚、乙酸丙二醇单丙醚、乙酸丙二醇单丁醚、乙酸二丙二醇单甲醚、乙酸二丙二醇单乙醚、二乙酸乙二醇酯、乙酸甲氧基三甘醇酯、丙酸乙酯、丙酸正丁酯、丙酸异戊酯、草酸二乙酯、草酸二正丁酯、乳酸甲酯、乳酸乙酯、乳酸正丁酯、乳酸正戊酯、丙二酸二乙酯、邻苯二甲酸二甲酯、邻苯二甲酸二乙酯等酯系溶剂;
N-甲基甲酰胺、N,N-二甲基甲酰胺、N,N-二乙基甲酰胺、乙酰胺、N-甲基乙酰胺、N,N-二甲基乙酰胺、N-甲基丙酰胺、N-甲基吡咯烷酮等含氮系溶剂;二甲基硫醚、二乙基硫醚、噻吩、四氢噻吩、二甲亚砜、环丁砜、1,3-丙烷磺内酯等含硫系溶剂等。
上述溶剂中,从保存稳定性、操作容易性、入手的容易性等观点出发,优选为正丁醇、3-甲氧基-3-甲基-1-丁醇、乙二醇单丙醚、乙二醇单苯氧基醚、丙二醇单丁醚、乙二醇单正丁醚、乙二醇单叔丁醚、乙二醇单异丁醚、二甘醇单甲醚、二甘醇单乙醚、N,N-二甲基甲酰胺,更优选为丙二醇单丁醚、乙二醇单正丁醚、乙二醇单叔丁醚、乙二醇单异丁醚。
使用水等具有高极性的溶剂时,根据溶剂的极性分别选择适当的导电性高分子和树脂。例如,使用水作为溶剂时,作为树脂,可以使用水溶性丙烯酸类树脂和水溶性聚酯树脂。也可以将以往的油溶性树脂乳液化来使用。作为导电性高分子,聚(3,4-乙烯二氧噻吩)-聚(苯乙烯磺酸)(PEDOT-PSS)等聚噻吩系高分子在可溶性优异方面是优选的。特别是如具有下述式(1)所示的结构单元的自掺杂型的聚噻吩,由于水溶性的维持性能优异,因而优选。
[化1]
式(1)中,L为下述式(2)或式(3)所示的2价的基团,M为氢原子、碱金属原子、或NH(R1)3。R1各自独立地为氢原子、或取代或未取代的碳原子数1~6的烷基。
[化2]
式(2)中,l为6~12的整数。
[化3]
式(3)中,m为1~6的整数。R2为氢原子、碳原子数1~6的直链状或支链状的烷基、或氟原子。
溶剂可以单独使用1种上述溶剂,或者也可以组合2种以上使用。
本实施方式的溶液组合物中的溶剂的量可以根据导电性高分子、树脂和任意的添加剂的种类、溶液组合物的粘度等而适宜调整。通常,相对于导电性高分子100质量份,优选以20~100000质量份的范围含有上述溶剂,进一步优选以100~10000质量份的范围含有上述溶剂。
本实施方式的溶液组合物除了上述导电性高分子、树脂和溶剂之外,在不对防锈性能造成不良影响的范围内,还可以包含例如有色系颜料、增塑剂、颜料分散剂、乳化剂、增稠剂、防飞散剂、流平材料等公知的添加剂。
本发明的溶液组合物本质上由导电性高分子、树脂和溶剂、以及任选的选自有色系颜料、增塑剂、颜料分散剂、乳化剂、增稠剂和防飞散剂中的1种以上的添加剂组成,在不损害本发明效果的范围内还可以包含其它不可避免的杂质。
本发明的组合物的例如90~100质量%、95~100质量%、99~100质量%、99.5~100质量%、99.9~100质量%或100质量%可以为导电性高分子、树脂和溶剂,或者为导电性高分子、树脂、溶剂和添加剂。
本实施方式的溶液组合物可以通过将上述导电性高分子、树脂、溶剂、以及任选的添加剂进行混合、搅拌而容易地制造。在使用如环氧树脂那样将主剂和固化剂混合而使用的树脂时,可以将导电性高分子预先添加至主剂中来使用。混合和搅拌中可以使用例如浅田铁钢株式会社制DESPA(商品名)、Ashizawa Finetech株式会社制HYPER(商品名)、株式会社THINKY制AWATORI RENTARO(商品名)等搅拌装置。
本实施方式的溶液组合物可以通过例如涂布于铜板之类的金属等被防锈物上并实施干燥或固化处理而形成膜。所得膜的防锈性能优异。
涂布例如可以通过喷涂、空气喷涂、刷涂、辊涂等来实施。此外,还可以将溶液组合物分散于水中进行电沉积涂装。
涂布后通过自然干燥、加热干燥等形成干燥的膜。树脂使用热固性树脂时,可以通过加热进行固化。固化条件可以根据热固性树脂适宜设定。
应予说明,在膜中,导电性高分子可以溶解于树脂中,也可以分散于树脂中。从防锈性能的观点出发,优选溶解。此外,溶解的状态和分散的状态可以共存。
从防锈性能的观点出发,膜的厚度在干燥状态下优选为15~60μm。若膜的厚度为15μm以上,则难以受到氧、水的透过的影响,锈的发展难以提前。此外,若膜的厚度为60μm以下,则由于与被防锈物的线膨胀系数之差而产生由温度变化导致的裂纹的风险小。
本实施方式的膜具有防锈性能,因此适合作为钢材等金属构件的涂覆膜。例如,具有用膜被覆钢材的结构的金属构件的被覆面具有优异的防锈性能。
本实施方式的金属构件可以在上述膜之上进一步设置顶涂层。顶涂层优选通过例如聚氨酯系树脂以厚度达到15~60μm的方式形成。
进一步,本实施方式的溶液组合物的粘度在室温、具体地在25℃下,优选为1000cP以上且100000cP以下、更优选为1000cP以上且80000cP以下、进一步优选1000cP以上且70000cP以下、特别优选为1000cP以上且60000cP以下。粘度若为1000cP以上,则在涂布后难以流动,可以维持作为优选厚度的15~60μm。此外,粘度若为100000cP以下,则涂布后的流平能力不降低,难以成为凹凸多的表面形态。此时,导致生锈的水分、盐分难以停留于表面,锈的发展难以提前。
在使用如环氧树脂那样将主剂和固化剂混合使用的树脂时,溶液组合物的粘度是对除去固化剂的溶液组合物进行测定的。
本发明的一个实施方式中,溶液组合物可以用作防锈剂。防锈剂的适用对象只要是需要防腐蚀的对象即可,没有特别限定。可举出例如,房屋、大厦、桥梁、工厂、罐(例如,石油罐、天然气罐)、道路、送电或通信用的铁塔等建筑结构物;船舶、车辆(例如,铁路车辆、大型车辆、小型车辆、混合动力车、电动车)、飞机、火箭等运输媒介;汽车等车辆中的电线、电缆、连接器、车身等的金属部分、高压电力电缆;电气或电子设备部件等的金属部分等。
作为连接器的适用部位,例如有端子压接部。在端子压接部中,端子和电线可以是同种金属,此外也可以是不同种金属。
此外,由本发明的一个实施方式的溶液组合物得到的膜也可以适宜地用作气化性防锈膜、涂装型可剥离塑料膜、热浸渍型塑料膜。
实施例
实施例1
(1)掺杂有掺杂剂的聚苯胺(聚苯胺复合物)的制造
将Aerosol OT(二(2-乙基己基)磺基琥珀酸钠、纯度75%以上、富士胶片和光纯药株式会社制)35.0g和Sorbon T-20(具有聚氧乙烯失水山梨糖醇脂肪酸酯结构的非离子乳化剂、东邦化学工业株式会社制)1.47g溶解于甲苯600mL中,制备溶液。
将所得的溶液加入置于氮气流下的6L的可拆卸烧瓶中,向该溶液中加入22.2g的苯胺。然后,添加1mol/L的磷酸水溶液1800mL,冷却至5℃。溶液具有甲苯和水这2个液相。
溶液的温度达到5℃后,立即以每分钟390转进行搅拌。在搅拌后的溶液中,一边搅拌,一边使用滴液漏斗用2小时滴加将65.7g的过硫酸铵溶解于1mol/L的磷酸600mL中而得的过硫酸铵溶液。从滴加开始18小时,在将溶液内温保持于5℃的情形下进行搅拌。然后,将溶液温度上升至40℃,进一步搅拌1小时。搅拌后,通过静置溶液使其分离为2相。对分离的水相进行分液,回收有机相。
向所得的有机相中追加甲苯1500mL,以1mol/L的磷酸600mL洗涤1次,用离子交换水600mL洗涤3次。使用#5C的滤纸,通过过滤除去不溶物,得到聚苯胺复合物的甲苯溶液。
将所得的甲苯溶液转移至蒸发器中,通过在60℃的热水浴中加热的同时进行减压,将挥发成分蒸发馏去,得到43.0g的粉末状的聚苯胺复合物(分子量60000)。
聚苯胺的重均分子量为60000。应予说明,分子量通过凝胶渗透色谱(GPC)以聚苯乙烯换算进行测定。
聚苯胺复合物的掺杂剂比[(掺杂于聚苯胺中的掺杂剂的摩尔数)/(聚苯胺的单体单元的摩尔数)]为0.63。
掺杂剂比由聚苯胺复合物中的掺杂剂与聚苯胺的单体单元的摩尔数算出。具体地,通过有机元素分析法对来自掺杂剂的硫原子的摩尔数和来自聚苯胺的单体单元的氮原子的摩尔数进行定量,通过取这些值的比来算出掺杂剂比。
(2)溶液组合物的制备
称量上述(1)中得到的聚苯胺复合物1g,一边搅拌一边投入至9g的丙二醇单丁醚中,得到10质量%的聚苯胺复合物溶液。接着,在聚苯胺复合物溶液中追加作为树脂溶液的DAIFERAMINE 90mL(大日精化工业株式会社制、聚氨酯30质量%的γ丁内酯溶液),使用自转型搅拌机(株式会社THINKY制、ARE-250),以2000rpm搅拌5分钟,制备溶液组合物。
使用电位差滴定法评价所得的溶液组合物的酸值或碱值。测定装置使用京都电子工业株式会社制的AT-500,以所得的电位差的拐点为终点。酸值是使用氢氧化钾作为滴定液,通过下述式求出的。
酸值(mgKOH/g)=(V1-V0)×N×f×M/S
式中,V1为本试验中的滴定量(mL)、V0为空试验中的滴定量(mL)、N为滴定液的浓度(mol/L)、f为滴定液的因数(1.010)、M为滴定液的摩尔质量(g/mol)、S为试样质量(g)。
碱值除了使用盐酸作为滴定液之外,与酸值同样地进行测定。
测定结果示于表1。
同样地,在25℃下使用数字粘度计评价所得的溶液组合物的粘度。评价装置使用Brookfield公司的DV2T,评价转速为1rpm时的粘度。测定结果示于表1。
(3)膜的形成
用滴管吸取上述(2)中所得的溶液组合物,使用膜涂机(テスター产业株式会社制、PI-1210),涂布于SPC铜板上。接着在空气中在80℃下干燥2小时,得到具有膜厚30μm的膜的金属构件。
对于所得的具有膜的金属构件,在以下的条件下实施环境循环试验,观察生锈的情况。
盐水喷雾:将35℃的NaCl溶液(浓度5质量%)喷雾2小时
干燥:在温度60℃、湿度20~30RH%的空气中干燥4小时
湿润:在温度50℃、湿度95RH%以上的空气中放置2小时
以上述盐水喷雾、干燥和湿润为1个循环,实施30个循环(10天)。对于环境循环试验后的试样,评价覆盖试样表面的锈的面积的比例。
结果示于表1。
[表1]
实施例2
将Aerosol OT的使用量设为17.8g,除此之外与实施例1相同地制备溶液组合物,进行评价。结果示于表1。
实施例3
将聚苯胺(Sigma Aldrich公司制、分子量20000)2.22g溶解于N甲基吡咯烷酮40mL中后,加入萘磺酸(东京化成工业株式会社制)1.37g进行搅拌,得到聚苯胺复合物。
对于溶液组合物的制备、膜的形成和评价,与实施例1相同地进行。结果示于表1。
实施例4
将萘磺酸的使用量设为0.67g,除此之外与实施例3相同地制备溶液组合物,进行评价。结果示于表1。
实施例5
使用聚苯胺(Sigma Aldrich公司制、分子量5000)2.22g,使用萘磺酸1.37g,除此之外与实施例3相同地制备溶液组合物,进行评价。结果示于表1。
实施例6
将萘磺酸的使用量设为0.67g,除此之外与实施例5相同地制备溶液组合物,进行评价。结果示于表1。
实施例7
未使用萘磺酸,除此之外与实施例3相同地制备溶液组合物,进行评价。结果示于表1。
实施例8
替代萘磺酸而使用浓度99%的磷酸0.18g,除此之外与实施例3相同地制备溶液组合物,进行评价。结果示于表1。
实施例9
替代作为树脂溶液的DAIFERAMINE (聚氨酯30质量%的γ丁内酯溶液),使用环氧树脂溶液90mL(荒川化学工业株式会社制Alkyd 9205、含有环氧基40质量%的溶液),除此之外与实施例1相同地制备溶液组合物,进行评价。结果示于表1。
实施例10
使用化研产业株式会社制的聚苯胺(Regulus、分子量75000),将萘磺酸的添加量设为2.48g,除此之外与实施例3相同地得到聚苯胺复合物。对于溶液组合物的制备、膜的形成和评价,与实施例1相同地进行。结果示于表1。
实施例11
将聚苯胺(Sigma Aldrich公司制、分子量20000)2.22g溶解于N甲基吡咯烷酮40mL中后,加入萘磺酸(东京化成工业株式会社制)2.48g进行搅拌,得到聚苯胺复合物。对于溶液组合物的制备、膜的形成和评价,与实施例1相同地进行。结果示于表1。
实施例12
将聚苯胺(Sigma Aldrich公司制、分子量5000)2.22g溶解于N甲基吡咯烷酮40mL中后,加入萘磺酸(东京化成工业株式会社制)2.48g进行搅拌,得到聚苯胺复合物。对于溶液组合物的制备、膜的形成和评价,与实施例1相同地进行。结果示于表1。
实施例13
替代SPC铜板而使用铝(A6061),除此之外与实施例1相同地得到具有膜的金属构件,进行评价。结果示于表1。
实施例14
替代SPC铜板而使用镀锌铜板,除此之外与实施例1相同地得到具有膜的金属构件,进行评价。结果示于表1。
实施例15
替代SPC铜板而使用镀锡铜,除此之外与实施例1相同地得到具有膜的金属构件,进行评价。结果示于表1。
比较例1
将Aerosol OT的使用量设为200g,除此之外与实施例1相同地制备溶液组合物,进行评价。结果示于表1。
比较例2
替代萘磺酸而使用氢氧化钠5g,除此之外与实施例5相同地制备溶液组合物,进行评价。结果示于表1。
比较例3
替代聚苯胺复合物溶液而使用作为树脂溶液的DAIFERAMINE (聚氨酯30质量%的γ丁内酯溶液),除此之外与实施例1相同地形成膜,进行评价。结果示于表1。
上述详细说明了本发明的几个实施方式和/或实施例,但本领域技术人员容易对这些作为例示的实施方式和/或实施例施加许多改变,而实质上不脱离本发明的新颖教导和效果。因此,这些许多改变也包含在本发明的范围内。
对该说明书中记载的文献和作为本申请的巴黎公约优先权基础的申请的内容全部进行援用。
Claims (12)
1.溶液组合物,其包含导电性高分子、树脂和溶剂,
其酸值为0.0~14.5mgKOH/g、或碱值为0.0~1.0mgHCl/g。
2.权利要求1所述的溶液组合物,其中,所述导电性高分子为聚苯胺系高分子。
3.权利要求2所述的溶液组合物,其中,所述聚苯胺系高分子是掺杂有掺杂剂的取代或未取代的聚苯胺。
4.权利要求1~3中任一项所述的溶液组合物,其特征在于,溶液组合物的粘度在25℃下为1000cP以上且80000cP以下。
5.权利要求1~3中任一项所述的溶液组合物,其特征在于,溶液组合物的粘度在25℃下为1000cP以上且60000cP以下。
6.权利要求3~5中任一项所述的溶液组合物,其中,所述掺杂剂为磺基琥珀酸衍生物。
7.权利要求1~6中任一项所述的溶液组合物,其中,所述树脂为热固性树脂。
8.权利要求7所述的溶液组合物,其中,所述热固性树脂是选自醇酸树脂、不饱和聚酯、聚酯、三聚氰胺树脂、聚异氰酸酯、丙烯酸类树脂、酚醛树脂、聚胺、聚氨酯和环氧树脂中的1种以上的树脂。
9.权利要求7所述的溶液组合物,其中,所述热固性树脂是聚氨酯或环氧树脂。
10.由权利要求1~9中任一项所述的溶液组合物得到的膜。
11.金属构件,其包含权利要求10所述的膜。
12.权利要求11所述的金属构件,其具有将钢材用所述膜被覆的结构。
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- 2020-03-12 WO PCT/JP2020/010857 patent/WO2020195905A1/ja unknown
- 2020-03-12 KR KR1020217030722A patent/KR20210148135A/ko unknown
- 2020-03-12 JP JP2021509032A patent/JP7438192B2/ja active Active
- 2020-03-20 TW TW109109392A patent/TW202043385A/zh unknown
Patent Citations (6)
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JPH06128769A (ja) * | 1992-05-25 | 1994-05-10 | Japan Carlit Co Ltd:The | 金属の防食方法 |
CN1429258A (zh) * | 2000-05-15 | 2003-07-09 | 潘尼珀尔有限公司 | 耐腐蚀涂料 |
CN101035630A (zh) * | 2004-08-03 | 2007-09-12 | 坎梅陶尔股份有限公司 | 用防腐涂层涂覆金属表面的方法 |
KR20100097781A (ko) * | 2009-02-27 | 2010-09-06 | 이동복 | 녹층의 수분 제거 반응으로 전처리 공정이 필요없는 부식억제형 전도성 친환경 코팅제의 제조 방법 |
WO2014106949A1 (ja) * | 2013-01-07 | 2014-07-10 | 出光興産株式会社 | 無電解めっき下地膜形成用組成物 |
WO2015019596A1 (ja) * | 2013-08-06 | 2015-02-12 | 出光興産株式会社 | 無電解めっき下地膜形成用組成物 |
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JPWO2020195905A1 (zh) | 2020-10-01 |
EP3950332A4 (en) | 2022-12-21 |
WO2020195905A1 (ja) | 2020-10-01 |
EP3950332A1 (en) | 2022-02-09 |
KR20210148135A (ko) | 2021-12-07 |
JP7438192B2 (ja) | 2024-02-26 |
US20220154013A1 (en) | 2022-05-19 |
TW202043385A (zh) | 2020-12-01 |
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