CN101978006B - 多功能涂覆液组合物 - Google Patents
多功能涂覆液组合物 Download PDFInfo
- Publication number
- CN101978006B CN101978006B CN200980109363.6A CN200980109363A CN101978006B CN 101978006 B CN101978006 B CN 101978006B CN 200980109363 A CN200980109363 A CN 200980109363A CN 101978006 B CN101978006 B CN 101978006B
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- China
- Prior art keywords
- functional
- silver
- coat film
- compound
- coating liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000576 coating method Methods 0.000 title claims abstract description 98
- 239000011248 coating agent Substances 0.000 title claims abstract description 94
- 239000000203 mixture Substances 0.000 title claims abstract description 56
- 229910052709 silver Inorganic materials 0.000 claims abstract description 40
- 239000004332 silver Substances 0.000 claims abstract description 39
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 36
- 150000001875 compounds Chemical class 0.000 claims abstract description 31
- 229940100890 silver compound Drugs 0.000 claims abstract description 7
- 150000003379 silver compounds Chemical class 0.000 claims abstract description 7
- -1 salt compound Chemical class 0.000 claims description 63
- 239000007788 liquid Substances 0.000 claims description 52
- 239000000126 substance Substances 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 25
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- 238000002360 preparation method Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 8
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims description 7
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- C09D131/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Coating compositions based on derivatives of such polymers
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Abstract
本发明涉及一种含有银化合物作为主要成分的多功能涂覆液组合物，更具体而言，涉及一种含有具有特定结构的银络合物以及金属或非金属化合物或至少一种其混合物的多功能涂覆液组合物。本发明的多功能涂覆液组合物能够呈现多种颜色，以及简单的银色，并表现出多功能的效果，即，表现出以下性质中的至少一种性质：导电性和/或导热性、抗菌性、抗静电性、阴离子和远红外线辐射性和反射性。
Description
技术领域
以下公开涉及一种基于银化合物的多功能涂覆液组合物，特别是，涉及一种含有具有特定结构的银络合物以及金属化合物、非金属化合物或包含它们中的至少一种的混合物的多功能涂覆液组合物。
背景技术
银(Ag)因其独特的性质，包括高导电性和抗菌活性，已被广泛应用于各种工业领域，包括贵金属饰物或硬币、器皿、电学、电器、照明、复印机、显示电极、电子波屏蔽、抗菌剂等。近来，具有多功能涂覆层的商品受到青睐，所述多功能涂覆层除具有如导电性、抗菌性、光泽、抗静电性以及阴离子和远红外线发射性等银所独有的性质外，还能够实现各种颜色。
一般说来，本领域技术人员已知的涂覆方法包括镀覆、磁控溅射、离子等离子沉积、化学气相沉积、物理气相沉积、浸涂、流化床涂覆、原子层沉积(ALD)、喷涂、旋涂、电极沉积、静电涂覆或凹版涂覆等。当然，这些方法可应用于银涂覆。当基于银前体的还原而使用银涂覆液组合物时，为实现除银的基本性质外作为多功能涂层的各种特性，需要涂布能够对基材赋予功能性的底涂层或者在银涂层上涂布另外的功能涂层。若以上述方式使银涂层多功能化，如传导性、抗菌性、抗静电性、阴离子和远红外线发射或光泽等银所独有的性质会劣化。近来，相关领域已经进行了积极的研究。然而，相关领域中所提出的多功能化方法繁琐且复杂。
发明内容
技术问题
如上所述，根据所述相关领域的银涂覆组合物需要复杂的方法来实现多功能涂层，因而成本效率低或会造成银涂层自身品质劣化。因此，本发明的一个实施方式涉及提供一种涂覆液组合物及其制备方法，所述涂覆液组合物能够实现各种颜色并可通过简单的方法获得，同时提供有多功能，包括导电和/或导热性、抗菌性、抗静电性、阴离子和远红外线发射线性或反射性。
本发明的另一个实施方式涉及提供一种制造多功能涂覆膜的方法，所述方法包括使用多功能涂覆液组合物在各种基材上形成多功能涂覆膜。
技术方案
为解决上述技术问题，本发明人进行了深入研究，并发现当向包含具有特定结构的银络合物的涂覆液中加入不同类型和量的金属化合物或非金属化合物时，除显色性外还可以实现选自导电和/或导热性、抗菌性和反射性中的一种或多种不同功能。本发明基于这一发现。
在一个一般性的方案中，提供了一种基于银络合物的多功能涂覆液组合物。更具体而言，提供了一种含银多功能涂覆液组合物及其制备方法，所述组合物包含具有特定结构的银络合物和金属化合物、非金属化合物或含有它们中的至少一种的混合物。此处所用的术语“多功能”是指涂覆组合物除显色性外还具有选自导电和/或导热性、抗菌性、抗静电性、阴离子和远红外线发射性和反射性的一种或多种功能。
在另一个一般性的方案中，提供了一种制备多功能涂覆膜的方法，所述方法包括使用所述多功能涂覆液在许多种基材的表面上形成涂覆膜，所述涂覆膜能够实现各种颜色，并具有选自导电和/或导热性、抗菌性和反射性中的一种或多种不同功能。
此处所公开的多功能涂覆液可以涂布于氧化铝、二氧化钛涂覆的云母或玻璃片，从而提供具有各种颜色和银所独有的性质的珠光颜料。也可以将所述多功能涂覆液涂覆在丙烯腈-丁二烯-苯乙烯(ABS)或聚碳酸酯(PC)上来提供主要芯料(master chip)，再将它们以适当比例混合并进行如注射或挤出等成型加工。以此方式，可以获得具有各种颜色和抗菌性的塑料产品。此外，当将多功能涂覆液涂覆在铝或铜超细粉上时，可以获得具有优异的导电性和氧化稳定性的导电性材料，并且所述材料的成本效率很高。
在一个具体实施方式中，提供了一种用于生成多功能涂覆膜的多功能涂覆液组合物，所述多功能涂覆膜能够实现各种颜色，并具有选自导电和/或导热性、抗菌性和反射性的一种或多种不同功能。所述多功能涂覆液组合物包含：银络合物；和选自金属化合物、非金属化合物及其混合物的显色剂。
在另一具体实施方式中，提供了一种用于制备具有优异的表面性质的多功能涂覆膜的方法，所述方法包括：
(i)形成含有银络合物的银涂覆液；
(ii)向所述银涂覆液中加入显色剂以提供多功能涂覆液；和
(iii)将所述多功能涂覆液涂布在基材上以形成多功能涂覆膜。
此处所使用的银络合物是指具有Ag[氨基甲酸铵化合物、碳酸铵化合物或碳酸氢铵化合物]络合物结构的银络合物，所述银络合物通过将银化合物与选自氨基甲酸铵化合物、碳酸铵化合物、碳酸氢铵化合物及其混合物中的至少一种物质反应而获得。本申请人提交的韩国专利申请第2006-0011083号中公开了这种银络合物。
通过以下对实施方式的描述，本发明的优点、特征和方案将会变得显而易见。
在一个方案中，提供了一种多功能涂覆液组合物，所述多功能涂覆液组合物包含：通过将由化学式1表示的银化合物与选自由化学式2表示的氨基甲酸铵化合物、由化学式3表示的碳酸铵化合物、由化学式4表示的碳酸氢铵化合物中的化合物或其混合物反应而获得的银络合物；和选自金属化合物、非金属化合物及其混合物的显色剂。
在另一方案中，提供了一种用于制备具有优异的表面性质的多功能涂覆膜的方法，所述方法包括：
(i)形成含有银络合物的银涂覆液，所述银络合物通过将由化学式1表示的银化合物与选自由化学式2表示的氨基甲酸铵化合物、由化学式3表示的碳酸铵化合物、由化学式4表示的碳酸氢铵化合物中的化合物或其混合物反应而获得；
(ii)向所述银涂覆液中加入显色剂以提供多功能涂覆液；和
(iii)将所述多功能涂覆液涂布在基材上以形成多功能涂覆膜。
[化学式1]
AgnX
[化学式2]
[化学式3]
[化学式4]
在以上化学式中，X是选自由氧、硫、卤素、氰基、氰酸根、碳酸根、硝酸根、亚硝酸根、硫酸根、磷酸根、硫氰酸根、氯酸根、高氯酸根、四氟硼酸根、乙酰丙酮基、羧酸根及其衍生物所组成的组的取代基；
n为1至4的整数；并且
R1至R6独立地表示氢、羟基、C1-C30烷氧基、C1-C30烷基、C3-C30环烷基、C6-C20芳基、(C6-C20)芳基(C1-C30)烷基、官能团取代的C1-C30烷基、官能团取代的C6-C20芳基、杂环化合物、聚合物或其衍生物，其中，当R1至R6表示没有取代基或取代有官能团的烷基或芳烷基时，各碳链还可以包含选自N、S和O的杂原子，并且R1和R2或者R4和R5可以独立地通过带有或不带有杂原子的C1-C10亚烷基彼此连接以形成环。
由化学式1表示的银化合物的具体实例包括但不限于：氧化银、硫氰酸酸、硫化银、氯化银、氰化银、氰酸银、碳酸银、硝酸银、亚硝酸银、硫酸银、磷酸银、高氯酸银、四氟硼酸银、乙酰丙酮银、乙酸银、乳酸银、草酸银及其衍生物。
在化学式2至4中，R1至R6的具体实例包括但不限于氢、甲基、乙基、丙基、异丙基、丁基、异丁基、戊基、己基、乙基己基、庚基、辛基、异辛基、壬基、癸基、十二烷基、十六烷基、十八烷基、二十二烷基、环丙基、环戊基、环己基、烯丙基、羟基、甲氧基、羟乙基、甲氧基乙基、2-羟基丙基、甲氧基丙基、氰基乙基、乙氧基、丁氧基、己氧基、甲氧基乙氧基乙基、甲氧基乙氧基乙氧基乙基、六亚甲基亚氨基、吗啉、哌啶、哌嗪、乙二胺、丙二胺、六亚甲基二胺、三亚乙基二胺、吡咯、咪唑、吡啶、羧甲基、三甲氧基甲硅烷基丙基、三乙氧基甲硅烷基丙基、苯基、甲氧基苯基、氰基苯基、苯氧基、甲苯基、苄基、及其衍生物、聚合物如聚烯丙胺或聚乙烯亚胺及其衍生物。
由化学式2表示的氨基甲酸铵化合物的具体实例包括选自由氨基甲酸铵、乙基氨基甲酸乙铵、异丙基氨基甲酸异丙铵、正丁基氨基甲酸正丁铵、异丁基氨基甲酸异丁铵、叔丁基氨基甲酸叔丁铵、2-乙基己基氨基甲酸2-乙基己铵、十八烷基氨基甲酸十八烷基铵、2-甲氧基氨基甲酸2-甲氧基乙铵、2-氰基乙基氨基甲酸2-氰基乙铵、二丁基氨基甲酸二丁铵、双十八烷基氨基甲酸双十八烷基铵、甲基癸基氨基甲酸甲基癸铵、六亚甲基亚氨基氨基甲酸六亚甲基亚氨基铵、吗啉氨基甲酸吗啉鎓、乙基己基氨基甲酸吡啶鎓、异丙基双氨基甲酸三亚乙基二铵、苄基氨基甲酸苄基铵、三乙氧基甲硅烷基丙基氨基甲酸三乙氧基甲硅烷基丙铵及其衍生物组成的组中的至少一种化合物或其混合物。由化学式3表示的碳酸铵化合物的具体实例包括选自由碳酸铵、乙基碳酸乙铵、异丙基碳酸异丙铵、正丁基碳酸正丁铵、异丁基碳酸异丁铵、叔丁基碳酸叔丁铵、2-乙基己基碳酸2-乙基己铵、2-甲氧基乙基碳酸2-甲氧基乙铵、2-氰基乙基碳酸2-氰基乙铵、十八烷基碳酸十八烷基铵、二丁基碳酸二丁铵、双十八烷基碳酸双十八烷基铵、甲基癸基碳酸甲基癸铵、六亚甲基亚氨基碳酸六亚甲基亚氨基铵、吗啉碳酸吗啉铵、苄基碳酸苄基铵、三乙氧基甲硅烷基丙基碳酸三乙氧基甲硅烷基丙铵、异丙基碳酸三亚乙基二铵及其衍生物组成的组中的至少一种化合物或其混合物。由化学式4表示的碳酸氢铵化合物的具体实例包括选自由碳酸氢铵、碳酸氢异丙铵、碳酸氢叔丁铵、碳酸氢2-乙基己铵、碳酸氢2-甲氧基乙铵、碳酸氢2-氰基乙铵、碳酸氢双十八烷基铵、碳酸氢吡啶鎓、碳酸氢三亚乙基二铵及其衍生物组成的组中的至少一种化合物或其混合物。
此处所用的银络合物通过本申请人递交的韩国专利申请第10-2006-0011083号中所公开的方法获得。银络合物可以作为固体从溶液中分离。据认为，获得的固体是包含银离子(Ag+)、阴离子(Xn-)和选自化学式2至4的氨基甲酸盐或碳酸盐化合物的络合物，或通过部分还原其银离子而由该络合物转变来的聚集体，由以下实验式表示：
[实验式]
Ag[A]m
其中，A为由化学式2至4中的任一化学式表示的化合物，并且m为0.7至2.5。
在所述方法中，含有银络合物的步骤(i)的银涂覆液除银络合物外还可包含溶剂。溶剂的具体实例包括水、如甲醇、乙醇、异丙醇或丁醇等醇、如乙二醇等二醇或甘油、如乙酸乙酯、乙酸丁酯或乙酸卡必醇酯等乙酸酯、如乙醚、四氢呋喃或二氧六环等醚、如甲乙酮或丙酮等酮、如己烷或庚烷等烃溶剂、如苯或甲苯等芳香溶剂、如氯仿、二氯甲烷或四氯化碳等卤代溶剂或其混合物。
步骤(ii)通过向含有银络合物的银涂覆液中加入选自金属化合物、非金属化合物及其混合物的显色剂而进行，从而提供多功能涂覆液组合物。
可加入银涂覆液中的金属化合物的具体实例包括含有如Li、Na、K、Rb、Cs、Be、Mg、Ca、Sr、Ba、Ti、V、Mn、Fe、Co、Ni、Cu、Zn、Y、Nb、Mo、Ru、Rh、Pd、Ag、Cd、Hf、Ta、W、Re、Os、Ir、Pt、Au、Hg、Al、Ga、In、Tl、Ge、Sn、Pb、Sb、Bi、As、Se、Eu、Sm、Th、Ac、Ce和Pr等金属的金属前体、金属有机酸盐、金属氧化物和合金氧化物。更具体而言，金属化合物可以包括但不限于草酸锰、乙酸金、草酸钯、2-乙基己酸铜、辛酸钴、辛酸锆、硬脂酸钴、萘二甲酸镍、萘二甲酸钴、2-乙基己酸铜、硬脂酸铁、甲酸镍、环烷酸钙、柠檬酸锌、新癸酸钡、氰化铜、碳酸钴、氯化铂、氯金酸、四丁氧基钛、二甲氧基二氯化锆、异丙醇铝、乙酰烷氧基二异丙醇铝、四氟硼酸锡、氧化钒、氧化铟锡、甲醇钽、醋酸铋、巯基金酸十二烷基酯、或乙酰丙酮铟等。
所述金属化合物可以以球形、线状、片状或其组合的形式提供。它们也可以以各种形式使用，如包括纳米颗粒的颗粒、粉末、薄片、胶体、混合物、浆料、溶胶、溶液或其组合。
可加入到银涂覆液中的非金属化合物的具体实例包括：硅化合物，如3-氨基丙基三乙氧基硅烷、甲基三乙氧基硅烷、正硅酸四乙酯、乙烯基三乙氧基硅烷、乙烯基甲基二甲氧基硅烷、辛基三乙氧基硅烷、苯基γ-氨基丙基三甲氧基硅烷、氨基新己基三甲氧基硅烷等；氟化合物，如2，2-双(4-羟基苯基)六氟丙烷、3，5-双(三氟甲基)苯胺、十二氟-1-庚醇、2，4-二氟苯胺、4-氟苯基酯、二己酰二苯甲酮(dicaprobenzophenone)、2-氟联苯、四氟氢醌等；和有机聚合树脂，如聚丙烯、聚碳酸酯、聚丙烯酸酯、聚甲基丙烯酸甲酯、乙酸纤维素、聚氯乙烯、聚氨酯、聚酯、醇酸树脂、环氧树脂、三聚氰胺树脂、酚醛树脂、苯酚改性醇酸树脂、环氧改性醇酸树脂、乙烯基改性醇酸树脂、硅改性醇酸树脂、丙烯酸三聚氰胺树脂、聚异氰酸酯树脂和环氧酯树脂等。在本发明范围内也可以使用其它非金属化合物。
在银涂覆液中可以加入需要量的显色剂，只要其不会对获得的涂覆液组合物的特性产生不利影响即可。一般而言，基于组合物的总重，显色剂的用量可以为0.01重量％至30重量％，更特别为0.1重量％至10重量％。若显色剂的用量低于0.01重量％，则不能充分显示所需要的颜色。另一方面，若显色剂的用量大于30重量％，则银络合物或其它成分的量相对降低，导致获得的涂覆膜的其它特性劣化。
步骤(ii)获得的多功能涂覆液组合物除包含银络合物和显色剂之外，还可以包含其它添加剂，如溶剂、稳定剂、分散剂、粘合剂树脂、还原剂、表面活性剂、湿润剂、触变剂或流平剂。
可用在涂覆液中的溶剂可选自水、醇、二醇、乙酸酯、醚、酮、脂肪烃、芳香烃或卤代烃溶剂。溶剂的具体实例包括选自水、甲醇、乙醇、异丙醇、1-甲氧基丙醇、丁醇、乙基己醇、萜品醇、乙二醇、甘油、乙酸乙酯、乙酸丁酯、乙酸甲氧基丙酯、乙酸卡必醇酯、乙酸乙基卡必醇酯、甲基溶纤剂、丁基溶纤剂、乙醚、四氢呋喃、二氧己环、甲乙酮、丙酮、二甲基甲酰胺、1-甲基-2-吡咯烷酮、二甲亚砜、己烷、庚烷、十二烷、石蜡油、溶剂油、苯、甲苯、二甲苯、氯仿、二氯甲烷、四氯化碳和乙腈中的至少一种。
可用在涂覆液中的稳定剂选自：带有或不带有羟基的伯胺、仲胺或叔胺化合物；选自氨基甲酸铵化合物、碳酸铵化合物和碳酸氢铵化合物的铵盐化合物；选自膦化合物、亚磷酸酯(盐)化合物和磷酸酯(盐)化合物的磷化合物；选自硫醇或硫化物的硫化合物；或其混合物。可用作稳定剂的胺化合物的具体实例包括甲胺、乙胺、正丙胺、异丙胺、正丁胺、异丁胺、异戊胺、正己胺、2-乙基己胺、正庚胺、正辛胺、异辛胺、壬胺、癸胺、十二烷胺、十六烷胺、十八烷胺、二十二烷胺(docodecylamine)、环丙胺、环戊胺、环己胺、烯丙胺、羟胺、氢氧化铵、甲氧基胺、2-乙醇胺、甲氧基乙基胺、2-羟基丙胺、2-羟基-2-甲基丙胺、甲氧基丙胺、氰基乙胺、乙氧基胺、正丁氧基胺、2-己氧基胺、甲氧基乙氧基乙胺、甲氧基乙氧基乙氧基乙胺、二乙胺、二丙胺、二乙醇胺、六亚甲基亚胺、吗啉(morphiline)、哌啶、哌嗪、乙二胺、丙二胺、六亚甲基二胺、三亚乙基二胺、2，2-(亚乙二氧基)双乙胺、三乙胺、三乙醇胺、吡咯、咪唑、吡啶、氨基乙醛、二甲基缩醛、3-氨基丙基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、苯胺、茴香胺、氨基苄腈、苄胺及其衍生物和聚合物，如聚烯丙胺或聚乙烯亚胺及其衍生物。
步骤(iii)通过将由步骤(ii)获得的多功能涂覆液涂布在基材上而进行，以形成多功能涂覆膜。
此处所用的基材可以是允许涂覆的任何基材。基材的具体实例包括但不限于：塑料，如聚酰亚胺(PI)、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、尼龙、聚四氟乙烯(PTFE)、聚醚醚酮(PEEK)、聚碳酸酯(PC)、多芳基化合物(PAR)等；树脂，如各种丙烯酸树脂、氨基甲酸乙酯树脂、氟树脂、有机硅环氧树脂、乙烯基树脂等；聚合橡胶材料，如丁基橡胶、氯丁橡胶、苯乙烯-丁二烯橡胶(SBR)、乙丙橡胶(EPR)、苯乙烯-异戊二烯-苯乙烯(SIS)橡胶等；各种陶瓷材料，如二氧化硅、氧化铝、二氧化钛、粘土、石、滑石、云母等；各种金属或合金材料，如铝、铜、镍、铁、锌、黄铜等；非金属材料，如碳、碳纳米管(CNT)、硅、硫等；金属盐化合物，如盐、磺酸钡等；各种纸，如合成纸、印相纸(photographic paper)、包装纸、纸板等；和由上述材料获得的各种复合材料。
另外，基材可以以粉末、薄片、珠、球、纤维、膜、片材、碎片、棒、线、须等形式提供，不过不限于这些形式。
本文所公开的多功能涂覆液组合物可以对各种基材赋予均一的涂覆特性，因此可通过银络合物与显色剂的组合，在如上所述的具有各种形式和材料的基材表面上实现优异的显色。同时，根据银组分和显色剂的特定类型，所述多功能涂覆液组合物可形成具有如导电性和/或导热性、抗菌性、抗静电性、阴离子和远红外线发射性或反射性等一种以上性质的多功能涂覆膜。
根据涂覆液的物理性质和基材的特定类型，所述多功能涂覆液可以通过选自旋涂、辊涂、喷涂、浸涂、流涂、刮板涂覆、滴涂(dispensing)、喷墨印刷、胶版印刷、丝网印刷、移印(pad printing)、凹版印刷、柔版印刷、刻版印刷、盖印(imprinting)、静电印刷、光刻、流化涂覆、原子层沉积(ALD)涂覆、化学气相沉积(CVD)、物理气相沉积(PVD)、离子等离子体涂覆、静电涂覆、电沉积涂覆等中的任何一种方法来涂布。
在步骤(iii)中将多功能涂覆液涂布在基材上之后，可以将其干燥、烘烤或干燥并烘烤，以形成涂覆膜。当基材为塑料、树脂或橡胶基材时，可以在涂布后干燥涂覆液，以形成涂覆膜。当基材为由选自各种陶瓷材料、金属材料、非金属材料如碳、碳纳米管(CNT)、硅或硫、金属盐化合物和各种纸中的任一种制成的基材时，可以烘烤或者干燥并烘烤涂覆液，以形成涂覆膜。干燥和烘烤可以根据基材的特定类型在适当的温度范围内进行。涂覆液可以在80℃至200℃的温度干燥，或者在300℃至700℃的温度烘烤。当干燥温度低于80℃时，涂覆液会因干燥速率低而无法得到有效干燥。另一方面，当干燥温度过高时，某些类型的基材可能会劣化。当烘烤温度低于300℃时，涂膜对于基材的粘合不充分，并且不会形成均一的涂覆膜。另一方面，超过700℃的过高的烘烤温度会导致基材的劣化并且成本效益较低。
有利效果
本文所公开的多功能涂覆液组合物能够实现各种颜色和银色，还可以提供如导电性和/或导热性、抗菌性、抗静电性、阴离子和远红外线发射性和反射性等性质中的一种以上性质。
另外，还可以根据加入到多功能涂覆液组合物中的金属或非金属化合物的具体类型和量，来提供不同的颜色和功能，同时避免了需要采用复杂的方法。
具体实施方式
下面描述实施例。以下实施例仅出于说明性目的，并不意在限制本公开的范围。
[实施例1]
在配备有搅拌器的反应器中，将2.1kg(6.94mol)2-乙基己基氨基甲酸2-乙基己铵和0.825kg(5.08mol)异丁基氨基甲酸异丁铵溶解在5.2kg异丙醇中。接下来，向其中加入1kg(4.31mol)氧化银，并使反应在室温进行。观察到，最初作为黑色浆料存在的反应混合物随着反应进行而颜色变浅，之后变得透明，从而产生络合物。反应进行2小时后，获得无色透明溶液。向该溶液中加入0.125kg作为稳定剂的2-羟基-2-甲基丙胺，然后搅拌。之后，通过0.45μm的膜过滤器过滤反应混合物。进行热重量分析(TGA)后，获得银含量为10.05重量％的银涂覆液。
[实施例2]
向100g由实施例1获得的银涂覆液中加入5重量％的量的辛酸锆(Jinyang Chemical，Corp.)，并在室温进行反应12小时，获得稳定的多功能涂覆液。
[实施例3]
以与实施例1相似的方式获得多功能涂覆液，不同之处在于，以20重量％的量向由实施例1获得的银涂覆液中加入环烷酸钙(JinyangChemical，Corp.)。
[实施例4]
以与实施例1相似的方式获得多功能涂覆液，不同之处在于，以30重量％的量向由实施例1获得的银涂覆液中加入3-氨基丙基三乙氧基硅烷(Aldrich)。
[实施例5]
以与实施例1相似的方式获得多功能涂覆液，不同之处在于，以10重量％的量向由实施例1获得的银涂覆液中加入聚氨酯树脂HW-1217(Hosung Chemex)。
[实施例6]
以与实施例1相似的方式获得多功能涂覆液，不同之处在于，以5重量％的量向由实施例1获得的银涂覆液中加入丁醇钛(Aldrich)。
[实施例7]
以与实施例1相似的方式获得多功能涂覆液，不同之处在于，以5重量％的量向由实施例1获得的银涂覆液中加入乙酰烷氧基二异丙醇铝(Ajinomoto fine-techno，AL-M)。
多功能涂覆膜的制备
由实施例1至7获得的多功能涂覆液用于制备下述各种多功能涂覆膜，并对这些涂覆膜进行表征。
[实施例8]
为制备多功能涂覆膜，制备旋涂用玻璃基材，并使用乙醇清洁该玻璃基材以除去其表面上的灰尘，然后在干燥器中于50℃干燥。对玻璃基材干燥至少30分钟后，将玻璃基材放置在旋涂机中，并将20mL由实施例2获得的组合物倾注在玻璃基材上，然后以500rpm的速度旋转，以形成涂覆膜，继而在500℃处理所述涂覆膜5分钟。获得的涂覆膜呈闪亮的黑色，并显示出12.4Ω/□的表面电阻和40％的反射率。
[实施例9]
通过喷涂，使用由实施例3获得的涂覆液在除去了灰尘的玻璃基材上形成涂覆膜。在500℃处理该涂覆膜5分钟。获得的涂覆膜呈闪亮的黄色，并显示出150Ω/□的表面电阻和40％的反射率。
[实施例10]
通过微凹版涂覆，使用由实施例4获得的涂覆液在PET膜上形成涂覆膜。在150℃处理该涂覆膜5分钟。获得的涂覆膜呈淡红色。
[实施例11]
首先，将1kg玻璃薄片(NGF Canada Ltd.，RCF-150)引入流化床反应器中，并将反应器的内部温度升高至110℃。接下来，在使由实施例5获得的涂覆液组合物流化的同时，以所述涂覆液组合物涂覆该玻璃薄片20分钟。然后，在150℃对所获得的涂覆膜进行干燥，产生灰色珠光颜料，继而将该灰色珠光颜料引入烘烤炉中，以在500℃进行为时10分钟的烘烤。在此方式下，获得了闪亮的浅灰色珠光颜料，其表面电阻为300Ω/□并且反射率为50％。
[实施例12]
首先，将1kg铝粉(ECKA 20T，eckagranules)引入流化床反应器中，并将反应器的内部温度升高至110℃。接下来，在使由实施例1获得的涂覆液组合物流化的同时，以所述涂覆液组合物涂覆所述铝粉20分钟。然后，在150℃对所获得的涂覆膜进行干燥，产生银色导电颗粒，其表面电阻为200mΩ/□并且反射率为85％。
[实施例13]
通过浸涂，使用由实施例6获得的涂覆液在玻璃基材上形成涂覆膜。在500℃处理该涂覆膜5分钟。获得的涂覆膜呈闪亮的黑色，并显示出100Ω/□的表面电阻和35％的反射率。
[实施例14]
通过微凹版涂覆，使用由实施例7获得的涂覆液在PET膜上形成涂覆膜。在500℃处理该涂覆膜5分钟。获得的涂覆膜成暗蓝色，并显出2KΩ/□的表面电阻。
工业实用性
本文所公开的多功能涂覆液组合物能够实现各种颜色和银色，还可以提供如导电性和/或导热性、抗菌性、抗静电性、阴离子和远红外线发射性和反射性等性质中的一种以上性质。
另外，还可以根据加入到多功能涂覆液组合物中的金属或非金属化合物的具体类型和量，来提供不同的颜色和功能，同时避免了需要采用复杂的方法。
Claims (7)
1.一种具有优异的表面性质的多功能涂覆膜的制备方法，所述方法包括：
(i)通过过滤含有银络合物和稳定剂的反应混合物，来形成含有所述银络合物和稳定剂的银涂覆液，所述银络合物通过将由化学式1表示的银化合物与由化学式2表示的氨基甲酸铵化合物、由化学式3表示的碳酸铵化合物、由化学式4表示的碳酸氢铵化合物或其混合物反应而获得；
(ii)向所述银涂覆液中加入显色剂，并进行反应以提供多功能涂覆液；和
(iii)将所述多功能涂覆液涂布在基材上以形成多功能涂覆膜：
[化学式1]
[化学式2]
[化学式3]
[化学式4]
其中
X是选自由氧、硫、卤素、氰基、氰酸根、碳酸根、硝酸根、亚硝酸根、硫酸根、磷酸根、硫氰酸根、氯酸根、高氯酸根、四氟硼酸根、乙酰丙酮基及羧酸根所组成的组的取代基；
n为1至4的整数；并且
R1、R2、R3、R4、R5和R6独立地为选自由氢、羟基、C1-C30烷氧基、 C1-C30烷基、C3-C30环烷基、C6-C20芳基、(C6-C20)芳基(C1-C30)烷基、官能团取代的C1-C30烷基、官能团取代的C6-C20芳基、杂环化合物及聚合物组成的组中的取代基，其中，当R1、R2、R3、R4、R5和R6为没有取代基或取代有官能团的烷基或芳烷基时，碳链能够包含选自N、S和O的杂原子，并且R1和R2或者R4和R5能够独立地通过带有或不带有杂原子的C1-C10亚烷基彼此连接以形成环；并且
所述显色剂选自辛酸锆、环烷酸钙、四丁氧基钛、3-氨基丙基三乙氧基硅烷和乙酰烷氧基二异丙醇铝，其中，基于所述多功能涂覆液的总重，所述显色剂的含量为0.01重量%至30重量%。
2.如权利要求1所述的多功能涂覆膜的制备方法，其中，所述多功能涂覆液还包含选自溶剂、分散剂、粘合剂树脂、还原剂、表面活性剂、湿润剂、触变剂和流平剂中的至少一种。
3.如权利要求2所述的多功能涂覆膜的制备方法，其中，所述溶剂为选自水、醇、二醇、乙酸酯、醚、酮、脂肪烃、芳香烃和卤代烃溶剂中的至少一种。
4.如权利要求1所述的多功能涂覆膜的制备方法，其中，所述基材以粉末、薄片、珠、球、纤维、膜、片材、碎片、棒、线或须的形式提供。
5.如权利要求1所述的多功能涂覆膜的制备方法，所述方法还包括其涂布后的干燥、烘烤或干燥并烘烤。
6.如权利要求5所述的多功能涂覆膜的制备方法，其中，所述干燥在80℃至200℃的温度进行，所述烘烤在300℃至700℃的温度进行。
7.一种多功能涂覆膜，所述多功能涂覆膜通过如权利要求1至6中任一项所述的方法获得。
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| WO2007126276A1 (en) * | 2006-04-29 | 2007-11-08 | Inktec Co., Ltd. | Compositions for forming reflecting layer having organic silver complexes,and method for preparing reflecting layer using same |
| WO2008018719A1 (en) * | 2006-08-07 | 2008-02-14 | Inktec Co., Ltd. | Manufacturing methods for metal clad laminates |
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| JPS53134759A (en) * | 1977-04-28 | 1978-11-24 | Fujikura Kasei Kk | Production of copmosite metal powder |
| US4652465A (en) * | 1984-05-14 | 1987-03-24 | Nissan Chemical Industries Ltd. | Process for the production of a silver coated copper powder and conductive coating composition |
| US6387542B1 (en) * | 2000-07-06 | 2002-05-14 | Honeywell International Inc. | Electroless silver plating |
| KR100727466B1 (ko) * | 2005-02-07 | 2007-06-13 | 주식회사 잉크테크 | 유기 은 착체 화합물, 이의 제조방법 및 이를 이용한박막형성방법 |
| KR100701851B1 (ko) * | 2006-03-14 | 2007-03-30 | 주식회사 잉크테크 | 유기 은 착체 화합물을 포함하는 항균성 조성물, 이를이용한 항균처리방법 및 항균성형품 |
| EP2052043B1 (en) * | 2006-08-07 | 2016-10-12 | Inktec Co., Ltd. | Process for preparation of silver nanoparticles, and the compositions of silver ink containing the same |
| KR100832002B1 (ko) * | 2006-08-07 | 2008-05-23 | 주식회사 잉크테크 | 저저항 금속 패턴 형성방법 |
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| WO2007126276A1 (en) * | 2006-04-29 | 2007-11-08 | Inktec Co., Ltd. | Compositions for forming reflecting layer having organic silver complexes,and method for preparing reflecting layer using same |
| WO2008018719A1 (en) * | 2006-08-07 | 2008-02-14 | Inktec Co., Ltd. | Manufacturing methods for metal clad laminates |
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| WO2009116782A2 (ko) | 2009-09-24 |
| WO2009116782A3 (ko) | 2009-12-23 |
| CN103665995B (zh) | 2016-05-04 |
| CN103665995A (zh) | 2014-03-26 |
| CN101978006A (zh) | 2011-02-16 |
| KR20090099646A (ko) | 2009-09-23 |
| KR101675493B1 (ko) | 2016-11-14 |
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