CN104781351B - 水性聚合物分散体在涂料中用于改善保色性的用途 - Google Patents
水性聚合物分散体在涂料中用于改善保色性的用途 Download PDFInfo
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- CN104781351B CN104781351B CN201380059768.XA CN201380059768A CN104781351B CN 104781351 B CN104781351 B CN 104781351B CN 201380059768 A CN201380059768 A CN 201380059768A CN 104781351 B CN104781351 B CN 104781351B
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- 230000001070 adhesive effect Effects 0.000 claims abstract description 53
- 239000000853 adhesive Substances 0.000 claims abstract description 52
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- -1 (methyl) Hydroxyethyl Chemical group 0.000 claims description 89
- 239000003973 paint Substances 0.000 claims description 63
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 49
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 43
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 30
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- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 claims description 2
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- GHUXAYLZEGLXDA-UHFFFAOYSA-N 8-azido-5-ethyl-6-phenylphenanthridin-5-ium-3-amine;bromide Chemical compound [Br-].C12=CC(N=[N+]=[N-])=CC=C2C2=CC=C(N)C=C2[N+](CC)=C1C1=CC=CC=C1 GHUXAYLZEGLXDA-UHFFFAOYSA-N 0.000 claims description 2
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- YCUBDDIKWLELPD-UHFFFAOYSA-N ethenyl 2,2-dimethylpropanoate Chemical compound CC(C)(C)C(=O)OC=C YCUBDDIKWLELPD-UHFFFAOYSA-N 0.000 claims description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
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- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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Abstract
本发明涉及水性聚合物分散体在涂料中作为粘合剂以改善保色性的用途,所述水性聚合物分散体包含(a)至少两种玻璃化转变温度≥25℃的单体M1,(b)至少两种玻璃化转变温度<25℃的单体M2,以及其他单体M3。
Description
本发明提供水性聚合物分散体在涂料中作为粘合剂用于改善色调(shade)稳定性(保色性)的用途,所述水性聚合物分散体包含(a)至少两种玻璃化转变温度≥25℃的单体M1,(b)至少两种玻璃化转变温度<25℃的单体M2,以及其他单体M3。
水性聚合物分散体是常识的。它们是这样的流体体系,其分散分布于水性分散介质中的分散相包含由多个相互缠绕的聚合物链组成的聚合物线团,这些线团被称为聚合物基体或聚合物颗粒。聚合物颗粒的平均直径的范围通常为10至1000nm,更特别为50至500nm。水性聚合物分散体在很多工业应用中被用作粘合剂。
水性聚合物分散体已成为外部油漆(exterior paints)的标准粘合剂。它们提供稳定的、使用期长的、防水和耐风化的装饰性涂料,常用于无机建筑材料,但也可用于木材和金属表面。长期以来,建筑表面的防护中,应用最广泛的是白色外部油漆。然而,近年来彩色外部油漆的使用已明显增多。随着这种情况发展,出现了新的问题,包括这些外部油漆的褪色。这种褪色指的是房屋正面的这些油漆在一段时间后出现的不想要的消色。对于某些色调(例如红色或蓝色),这种现象仅在一年或两年之后便会出现。
当有机颜料由于其所产生的强烈色彩而使用时,褪色尤为严重。在有机彩色颜料与白色二氧化钛颜料一起混合使用时也能观察到严重的褪色。本领域中将褪色倾向主要归因于有机彩色颜料的不稳定性。相比于例如无机彩色颜料,这些有色颜料自身具有更低的日光UV稳定性。在本领域中,有机粘合剂自身的性质毫无争议地被认为是重要的影响因素。
作为外部油漆和抹灰(renders)的粘合剂的水性聚合物分散体通常由具有高玻璃化转变温度的主要单体(硬单体)和具有低玻璃化转变温度的主要单体(软单体)制备。所选择的硬单体通常为苯乙烯或甲基丙烯酸甲酯;所选择的软单体通常为丙烯酸正丁酯或丙烯酸2-乙基己酯。因此,所述外部油漆粘合剂被称作苯乙烯丙烯酸酯,或者,当使用的硬单体为甲基丙烯酸甲酯时被称作直链的丙烯酸酯。由于良好的室外风化稳定性,大部分粘合剂由苯乙烯/丙烯酸正丁酯组成或由甲基丙烯酸甲酯/丙烯酸正丁酯组成。在各应用情形中,硬单体和软单体的各自用量参照具体使用中所需要的玻璃化转变温度来选择。用于无溶剂型外部油漆的粘合剂通常具有的玻璃化转变温度范围为0至5℃,低溶剂型外部油漆的粘合剂的玻璃化转变温度范围为5至20℃,溶剂型外部油漆的粘合剂的玻璃化转变温度范围为20至40℃。
例如EP771328记载了这种现有技术的粘合剂,如在实施例A、J和K中。
对单体的种类和用量的控制性改变能使技术人员根据本发明来制备其中所述聚合物的玻璃化转变温度在所需范围内的水性聚合物组合物。可借助于Fox方程进行指导。根据Fox(T.G.Fox,Bull.Am.Phys.Soc.1956[Ser.II]1,123页和根据Ullmann’sder technischen Chemie,19卷,18页,第4版,Verlag Chemie,Weinheim,1980),共聚物的玻璃化转变温度可按照如下方程良好地近似计算:
1/Tg=x1/Tg 1+x2/Tg 2+....xn/Tg n,
其中,x1、x2、....xn为单体1、2、....n的质量分数,Tg 1、Tg 2、....Tg n为各自仅由单体1、2、....n中的一种单体构成的聚合物的玻璃化转变温度,单位为开尔文。大部分单体的均聚物的Tg值已知并列于例如Ullmann’s Encyclopedia of Industrial Chemistry,A21卷,169页,第5版,VCH Weinheim,1992中;均聚物的玻璃化转变温度的其他来源包括,例如J.Brandrup,E.H.Immergut,Polymer Handbook,第1版,J.Wiley,New York 1966,第2版,J.Wiley,New York 1975,和第3版,J.Wiley,New York 1989。对于丙烯酸乙酯,所使用的数值为-13℃。
实际的玻璃化转变温度可用差示扫描量热法(ASTM D 3418-08,中点温度)确定。
本发明的目的是提供这样的聚合物分散体,与现有技术的相当的粘合剂相比,其在含有有机粘合剂的外部油漆和抹灰中显示出明显更好的保色性。
所述目的通过一种水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途而实现,所述水性聚合物分散体包含:
(a)至少两种玻璃化转变温度≥25℃的单体M1,
(b)至少两种玻璃化转变温度<25℃的单体M2,
以及,任选地其他单体M3。
褪色有时与粘合剂的UV稳定性有关。然而,出乎意料地,即使在高填充、低粘合剂油漆中使用本发明的粘合剂仍产生明显更低水平的褪色。这之所以是技术人员无法预见的,是因为在高填充油漆中,由于粘合剂分数低,风化(例如保色性或UV稳定性)对外部油漆的影响仅非常低程度地归因于粘合剂性质。
本发明还提供在外部油漆和抹灰中明显提高保色性的水性聚合物分散体,所述水性聚合物分散体包含:
(a)至少两种玻璃化转变温度≥25℃的单体M1,
(b)至少两种玻璃化转变温度<25℃的单体M2,
以及,任选地其他单体M3。已对于不同类型和浓度(信号红、蓝、黄、绿等)的有机颜料均发现了保色性改善。
这是技术人员不能预期的,因为对于外部油漆和抹灰而言,在油漆中的高含量的颜料和填料是为了通过光散射而对少量的粘合剂提供充分保护,因此,根据现有技术,粘合剂的性质是次要的。因此,例如在欧洲,高含量的苯乙烯丙烯酸酯用作外部油漆和抹灰的粘合剂,并且相比于例如直链丙烯酸酯,已知其具有较差的耐UV性。然而,在浅色或白色外部油漆和抹灰的情况下,耐候性测试表明,与直链丙烯酸酯相比苯乙烯丙烯酸酯方面无明显的缺陷。
出乎意料地,在粘合剂中使用至少四种主要单体M1和M2提高了外部油漆的耐久性至这样一个明显的程度,以致保色性明显地提高,并可制备使用寿命延长数年的油漆。
根据本发明,可使用如下单体用于聚合反应:
玻璃化转变温度≥25℃的单体M1的实例为乙烯基芳族化合物,例如乙烯基甲苯、α-甲基苯乙烯和对甲基苯乙烯、α-丁基苯乙烯、4-正丁基苯乙烯;以及优选苯乙烯,甲基丙烯酸C1至C4烷基酯,即MMA、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、丙烯酸叔丁酯、甲基丙烯酸异丁酯、甲基丙烯酸叔丁酯、丙烯酸叔丁酯、甲基丙烯酸环己酯,丙烯酸十八酯,乙酸乙烯酯和/或烯键式不饱和腈。腈的实例为丙烯腈和甲基丙烯腈。乙烯基卤化物为氯、氟、溴取代的烯键式不饱和化合物,优选氯乙烯和偏二氯乙烯。
适于作为玻璃化转变温度<25℃的单体M2的有,例如丙烯酸C1至C20烷基酯,例如丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯和丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸异丁酯和丙烯酸仲丁酯、丙烯酸正戊酯、丙烯酸异戊酯、丙烯酸正己酯、丙烯酸2-乙基己酯、丙烯酸庚酯、丙烯酸辛酯、丙烯酸C10异戊基格尔伯特醇酯(C10isoamyl guerbet acrylate)、丙烯酸2-丙基戊酯、丙烯酸1-丙基庚酯、丙烯酸十二烷基酯;甲基丙烯酸C5至C20烷基酯,例如甲基丙烯酸正戊酯和甲基丙烯酸异戊酯、甲基丙烯酸正己酯、甲基丙烯酸庚酯、甲基丙烯酸辛酯、甲基丙烯酸C10异戊基格尔伯特醇酯、甲基丙烯酸2-丙基戊酯、甲基丙烯酸2-丙基庚酯、甲基丙烯酸十二烷基酯;具有2至11个C原子的非支链或支链的羧酸的乙烯酯,例如丙酸乙烯酯、丁酸乙烯酯、乙酸1-甲基乙烯酯、三甲基乙酸乙烯酯;以及具有9个C原子的α-支链的一元羧酸的乙烯酯(VeoVa9R,壳牌(Shell)的商标名),例如2-乙基己酸乙烯酯、月桂酸乙烯酯;具有10或11个C原子的α-支链的一元羧酸的乙烯酯(VeoVa10R、VeoVa11R,壳牌的商标名);和具有10至13个C原子的支链一元羧酸的乙烯酯(Exxar Neo12);C1-C20乙烯基醚,例如甲基乙烯基醚、乙基乙烯基醚、丙基乙烯基醚、丁基乙烯基醚、戊基乙烯基醚、己基乙烯基醚、庚基乙烯基醚、辛基乙烯基醚、壬基乙烯基醚、癸基乙烯基醚等;丁二烯;偏二氯乙烯及单丙烯酸丁二醇酯。
对于单体M1,优选分别使用一种更亲水性的单体和一种更疏水性的单体,其中特别优选双组分(duos)的苯乙烯/甲基丙烯酸甲酯或甲基丙烯酸环己酯/甲基丙烯酸甲酯。
对于单体M2,优选分别使用一种更亲水性的单体和一种更疏水性的单体,其中特别优选双组分的丙烯酸正丁酯/丙烯酸乙基己酯。
任选地,可额外使用少量例如小于10重量%、优选小于8重量%、更优选小于6重量%的单体M3。
这些其他单体M3的实例为烯键式不饱和一元羧酸和二元羧酸,例如丙烯酸、甲基丙烯酸、衣康酸、富马酸和马来酸、乌头酸、中康酸、巴豆酸、柠康酸、丙烯酰氧基丙酸、甲基丙烯酰氧基丙酸、乙烯基乙酸、衣康酸单甲酯、富马酸单甲酯、富马酸单丁酯、丙烯酸酐、甲基丙烯酸酐、马来酸酐或衣康酸酐,
丙烯酰胺基乙醇酸和甲基丙烯酰胺基乙醇酸;丙烯酰胺;甲基丙烯酰胺及异丙基丙烯酰胺;取代的(甲基)丙烯酰胺,例如N,N-二甲基氨基(甲基)丙烯酸酯、(甲基)丙烯酸3-二甲基氨基-2,2-二甲基丙-1-基酯、N-二甲基氨基甲基(甲基)丙烯酰胺、N-(4-吗啉基甲基)(甲基)丙烯酰胺、二丙酮丙烯酰胺、甲基丙烯酸乙酰乙酰氧基乙酯、N-羟甲基(甲基)丙烯酰胺、聚环氧乙烷(甲基)丙烯酸酯、甲氧基聚环氧乙烷(甲基)丙烯酸酯、丙烯醛、甲基丙烯醛;N-(2-甲基丙烯酰氧基乙基)亚乙基脲、1-(2-(3-烯丙基氧-2-羟基丙基氨基)乙基)咪唑啉-2-酮、(甲基)丙烯酸脲酯以及甲基丙烯酸2-亚乙基脲基乙酯。
其他合适的为下列化合物:烯键式不饱和、羟基烷基官能化的共聚单体,例如丙烯酸和甲基丙烯酸与C1至C5烷基的羟基烷基酯,例如丙烯酸或甲基丙烯酸羟基乙基酯、丙烯酸或甲基丙烯酸羟基丙基酯、或丙烯酸或甲基丙烯酸羟基丁基酯;(甲基)丙烯酸羟基乙酯和(甲基)丙烯酸羟基丙酯;丙烯酸4-羟基丁酯、甲基丙烯酸4-羟基丁酯、(甲基)丙烯酸缩水甘油酯,以及N-乙烯基吡咯烷酮和乙烯基咪唑。
特别优选丙烯酸、甲基丙烯酸、丙烯酰胺、(甲基)丙烯酸羟基乙酯和(甲基)丙烯酸羟基丙酯。
单体M3的其他实例为含磷单体,其实例为乙烯基磷酸和烯丙基磷酸。还合适的是膦酸和磷酸与(甲基)丙烯酸羟基烷基酯的单酯和二酯,特别为单酯。其他合适的为膦酸和磷酸经(甲基)丙烯酸羟基烷基酯酯化一次且再经不同的醇(例如烷醇)酯化一次的二酯。用于这些酯的合适的(甲基)丙烯酸羟基烷基酯为下述作为单独单体的化合物,更具体而言为(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸3-羟基丙酯、(甲基)丙烯酸4-羟基丁酯等。相应的二氢磷酸酯单体包括(甲基)丙烯酸磷酸烷基酯(phosphoalkyl(meth)acrylate),如(甲基)丙烯酸2-磷酸乙酯、(甲基)丙烯酸2-磷酸丙酯、(甲基)丙烯酸3-磷酸丙酯、(甲基)丙烯酸磷酸丁酯和(甲基)丙烯酸3-磷酸-2-羟基丙酯。还合适的为膦酸和磷酸与烷氧基化的(甲基)丙烯酸羟基烷基酯的酯,实例为(甲基)丙烯酸酯的环氧乙烷缩聚物,例如H2C=C(CH3)COO(CH2CH2O)nP(OH)2和H2C=C(CH3)COO(CH2CH2O)nP(=O)(OH)2,其中n代表1至50。还合适的为巴豆酸磷酸烷基酯、马来酸磷酸烷基酯、富马酸磷酸烷基酯、(甲基)丙烯酸磷酸二烷基酯、巴豆酸磷酸二烷基酯和磷酸烯丙酯。其他合适的含磷基团的单体记载于WO 99/25780和US4,733,005,其在此以引用的方式纳入本说明书中。
其他合适的为乙烯基磺酸、烯丙基磺酸、丙烯酸磺乙基酯、甲基丙烯酸磺乙基酯、丙烯酸磺丙基酯、甲基丙烯酸磺丙基酯、2-羟基-3-丙烯酰氧基丙基磺酸、2-羟基-3-甲基丙烯酰氧基丙基磺酸、苯乙烯磺酸和2-丙烯酰胺基-2-甲基丙烷磺酸。合适的苯乙烯磺酸及其衍生物为苯乙烯-4-磺酸和苯乙烯-3-磺酸及其碱土金属盐或碱金属盐,实例为苯乙烯-3-磺酸钠和苯乙烯-4-磺酸钠、聚(烯丙基缩水甘油基醚)及其混合物,购自LaportePerformance Chemicals,UK的名为的各种产品的形式。它们包括例如MPEG 350MA,一种甲氧基聚乙二醇单甲基丙烯酸酯。
单体的官能团有助于向组合物提供胶体稳定性,尤其是当全部制剂还包含填料例如碳酸钙或其他时。在这种情况下,通过彼此反应或通过加入其他交联剂而进行交联。所述交联优选仅在膜实际形成之后进行。
通常增加水性聚合物分散体薄膜的内在强度的单体通常具有至少一个环氧基、羟基、N-羟甲基或羰基,或至少两个非共轭的烯键式不饱和双键。其实例为具有3至10个C原子的α,β-单烯键式不饱和羧酸的N-羟烷基酰胺,以及其与具有1至4个C原子的烷醇的酯,其中特别优选N-羟甲基丙烯酰胺和N-羟甲基甲基丙烯酰胺;具有两个乙烯基的单体、具有两个亚乙烯基的单体以及具有两个烯基的单体。在上下文中,特别有利的是二元醇与α,β-单烯键式不饱和一元羧酸(优选丙烯酸和甲基丙烯酸)的二酯。具有两个非共轭的烯键式不饱和双键的此类单体的实例为二丙烯酸亚烷基二醇酯和二甲基丙烯酸亚烷基二醇酯,如二丙烯酸乙二醇酯、二丙烯酸1,3-丁二醇酯、二丙烯酸1,4-丁二醇酯以及二丙烯酸丙二醇酯、二乙烯基苯、甲基丙烯酸乙烯酯、丙烯酸乙烯酯、甲基丙烯酸烯丙酯、丙烯酸烯丙酯、马来酸二烯丙酯、富马酸二烯丙酯、亚甲基双丙烯酰胺、丙烯酸环戊二烯酯或氰尿酸三烯丙酯。
官能交联剂基团为,例如酮基、醛基和/或乙酰乙酰氧基羰基,并且随后加入的配制交联剂可包括多胺或多酰肼,例如己二酸二酰肼(ADDH)、乙二酸二酰肼、邻苯二甲酸二酰肼、对苯二甲酸二酰肼、异氟尔酮二胺和4,7-二氧杂癸烷-1,1-O-二胺或带有氨基脲或肼官能团的交联剂。可选地,聚合物可带有肼官能团且随后的配制交联剂可含有酮官能团。
所述官能团也可为羧基且随后的配制交联剂可含有氮杂环丙烷基团、环氧基或碳二亚胺官能团,或所述官能团可为硅烷官能团且随后配制交联剂同样可含有硅烷官能团。
所述官能团也可为脲基且随后加入的交联剂为多醛,多醛的实例为含有1至10个C原子的α,ω-二醛,如乙二醛、戊二醛或丙二醛,和/或它们的缩醛或半缩醛,参见EP0789724。
在本发明中,通过彼此反应或通过加入其他交联剂而进行交联。所述交联优选仅在膜实际形成之后进行。
在本发明中,重要的是不使用过多额外的交联剂,因为这可导致剩余的交联剂的残留。另一方面,太少的交联剂可导致可溶性涂层。
在本发明中,重要的是不使用过多额外的交联剂,因为这可导致剩余的交联剂的残留。另一方面,太少的交联剂可导致可溶性涂层。
当然,也可将不同官能团与交联机理相结合。
含有交联基团的乙烯基单体为,例如烯丙基、缩水甘油基或乙酰乙酰氧基酯、乙酰乙酰氧基酰胺、酮官能团的乙烯基单体和醛官能团的乙烯基单体、含酮酰胺如双丙酮乙烯酰胺或硅烷(甲基)丙烯酸单体。
优选的带有交联基团的乙烯基单体为甲基丙烯酸乙酰乙酰氧基乙酯(AAEM)、双丙酮丙烯酰胺(DAAM)和硅烷(甲基)丙烯酸单体;最优选DAAM。
优选的交联机理包括硅烷官能团的交联和酮官能团与肼官能团的交联。
最优选DAAM和ADDH交联的组合。
单体M1与M2与M3的重量比取决于粘合剂的优选应用,且主要通过由全部单体的混合物制备的聚合物的玻璃化转变温度来确定。
优选的混合物的实例包括:
a)非常软的、有弹性的粘合剂(Tg约-24℃):17至27%的单体M1(基于甲基丙烯酸甲酯/苯乙烯计)、68至77%的单体M2和0.1至10%的单体M3(基于丙烯酸正丁酯/丙烯酸2-乙基己酯计),就单体M1而言的苯乙烯的量在5至15%的范围内。
b)软的、自成膜的粘合剂(Tg约0℃):34至44%的单体M1(基于甲基丙烯酸甲酯/苯乙烯计)、49至59%的单体M2和0.1至10%的单体M3(基于丙烯酸正丁酯/丙烯酸2-乙基己酯计),就单体M1而言的苯乙烯的量在10至20%的范围内。
c)用于需要少量成膜助剂的外部油漆和抹灰的粘合剂(Tg约15至20℃):37至47%的单体M1(基于甲基丙烯酸甲酯/苯乙烯计)、48至58%的单体M2和0.1至10%的单体M3(基于丙烯酸正丁酯/丙烯酸2-乙基己酯计),就单体M1而言的苯乙烯的量在10至25%的范围内。
d)用于需要大量成膜助剂的外部油漆和抹灰的粘合剂(Tg约30至40℃):60至70%的单体M1(基于甲基丙烯酸酯/苯乙烯计)、24至34%的单体M2和0.1至10%的单体M3(基于丙烯酸正丁酯/丙烯酸2-乙基己酯计),就单体M1而言的苯乙烯的量在10至25%的范围内。
其他优选的组合根据如上所列可容易地自确定,对于没有指定的玻璃化转变温度。
优选的单体组合M1为二组分苯乙烯/甲基丙烯酸甲酯或甲基丙烯酸环己酯/甲基丙烯酸甲酯,以及,对于单体组合M2,其为二组分丙烯酸正丁酯/丙烯酸乙基己酯。
出于环境原因,目标是使粘合剂在<0至40℃的范围内成膜,从而仅需少量或不需要成膜助剂。
本发明的聚合物分散体通过乳液聚合制备。在乳液聚合的过程中,烯键式不饱和化合物(单体)在水中聚合,通常使用离子型和/或非离子型乳化剂和/或保护胶体或稳定剂作为表面活性化合物来稳定单体液滴以及随后由单体形成的聚合物颗粒。然而,根据本发明,所述聚合反应在低乳化剂状态下进行。优选使用总计小于2.5或小于2.0重量%的乳化剂,更尤其小于1.5重量%,基于聚合物分散体的固体含量计。
聚合物分散体通常在至少一种表面活性化合物的存在下制备。合适的保护胶体的综述见于Houben-Weyl,Methoden der organischen Chemie,XIV/1卷,MakromolekulareStoffe,Georg Thieme Verlag,Stuttgart,1961,第411至420页。合适的乳化剂也见于Houben-Weyl,Methoden der organischen Chemie,14/1卷,Makromolekulare Stoffe,Georg Thieme Verlag,Stuttgart,1961,第192至208页。
合适的乳化剂包括阴离子型乳化剂、阳离子型乳化剂和非离子型乳化剂。作为表面活性物质,优选使用相对分子量通常低于保护胶体的乳化剂。更具体而言,现已确定仅使用阴离子乳化剂,或使用至少一种阴离子乳化剂和至少一种非离子乳化剂的组合。
有用的非离子乳化剂为芳脂族非离子乳化剂或脂族非离子乳化剂,实例为乙氧基化的单烷基苯酚、二烷基苯酚和三烷基苯酚(EO度:3至50,烷基:C4-C10),长链醇的乙氧基化物(EO度:3至100,烷基:C8-C36)和聚环氧乙烷/聚环氧丙烷的均聚物和共聚物。这些共聚物可包括无规分布或嵌段形式共聚的环氧烷单元。高度合适的为例如EO/PO嵌段共聚物。优选使用长链烷醇的乙氧基化物(烷基C1-C30,平均乙氧基化度为5至100),并且,其中,特别优选具有直链C12-C20烷基且平均乙氧基化度为10至50的那些,以及乙氧基化的单烷基苯酚。
合适的阴离子乳化剂为,例如烷基硫酸酯的碱金属盐和铵盐(烷基:C8-C22)、与乙氧基化的烷醇(EO度:2至50,烷基:C12-C18)的硫酸单酯的碱金属盐和铵盐,以及与乙氧基化的烷基苯酚(EO度:3至50,烷基:C4-C9)的硫酸单酯的碱金属盐和铵盐、烷基磺酸(烷基:C12-C18)的碱金属盐和铵盐,以及烷基芳基磺酸(烷基:C9-C18)的碱金属盐和铵盐。其他合适的乳化剂见于Houben-Weyl,Methoden der organischen Chemie,XIV/1卷,MakromolekulareStoffe,Georg-Thieme-Verlag,Stuttgart,1961,第192-208页。同样合适的阴离子乳化剂为双(苯基磺酸)醚和/或其碱金属盐或铵盐,其在一个或两个芳环上具有C4-C24烷基。这些化合物是常识,已知于例如US-A-4,269,749,并且以例如2A1(Dow ChemicalCompany)的形式市售可得。
合适的阳离子乳化剂优选为季铵卤化物,实例为三甲基十六烷基氯化铵、甲基三辛基氯化铵和苄基三乙基氯化铵,或N-C6-C20烷基吡啶的四价化合物、N-C6-C20烷基吗啉的四价化合物、N-C6-C20烷基咪唑的四价化合物,例如N-月桂基氯化吡啶。
所述聚合物分散体还可与常规助剂和添加剂混合。这些包括,例如pH调节物、还原剂、漂白剂如羟基甲烷亚磺酸的碱金属盐(例如购自BASF Aktiengesellschaft的C)、络合剂、除臭剂、添味剂(odorants)和粘度调节剂如醇类(实例为丙三醇、甲醇、乙醇、叔丁醇、乙二醇等)。可将这些助剂和添加剂在初始装料时、在一种进料中或在聚合反应结束后加入聚合物分散体中。
第一聚合物的酸基团的中和优选通过在第二段的聚合之前和/或期间至少部分地引入中和剂而进行。所述中和剂可以与待聚合单体联合进料或分别进料的方式加入。全部单体进料完成后,存在于聚合容器中的中和剂的量优选为中和至少10%、优选25%至100%或50%至95%的酸当量所需的量。
所述乳液聚合可使用水溶性引发剂开始。水溶性引发剂为例如过二硫酸的铵盐和碱金属盐如过二硫酸钠、过氧化氢或有机过氧化物如叔丁基氢过氧化物。还适合作为引发剂的为所谓的还原-氧化(氧化还原)引发剂体系。所述氧化还原引发剂体系由至少一种(通常为无机)还原剂和一种有机或无机氧化剂组成。所述氧化组分包含例如如上所述的乳液聚合引发剂。所述还原组分包含例如亚硫酸的碱金属盐(如亚硫酸钠、亚硫酸氢钠)、焦亚硫酸的碱金属盐(如焦亚硫酸钠)、焦亚硫酸与脂族醛和酮的加成化合物(如丙酮合焦亚硫酸)或诸如羟基甲烷亚磺酸及其盐等还原剂,或抗坏血酸。所述氧化还原引发剂体系可与可溶性金属化合物一起使用,所述可溶性金属化合物的金属组分能以多种价态存在。通常氧化还原引发剂体系为,例如抗坏血酸/硫酸亚铁(II)/过二硫酸钠、叔丁基氢过氧化物/焦亚硫酸钠,以及叔丁基氢过氧化物/羟基甲烷亚磺酸钠。单个组分—例如还原组分—还可为混合物,实例为羟基甲烷亚磺酸的钠盐与焦亚硫酸钠的混合物。
所述引发剂通常以水溶液的形式使用,其下限浓度通过在分散体中可接受的水的量来确定,且上限浓度通过各个化合物在水中的溶解性来确定。一般来说,引发剂的浓度为0.1至30重量%,优选0.2至20重量%,更优选0.3至10重量%,基于待聚合的单体计。乳液聚合还可使用两种以上不同的引发剂。
所述乳液聚合通常在30至130℃下、优选50至90℃下进行。聚合反应的介质可仅由水组成,或由水与水混溶性液体(如甲醇)的混合物组成。优选仅使用水。乳液聚合可以分批操作或进料方法的形式进行,包括分段方式或梯度方式。
在自由基水性乳液聚合反应过程中,将引发剂加入至聚合容器中的方式是本领域普通技术人员已知的。所述引发剂可以全部包含于加入至聚合容器的初始装料中,或者以其在自由基水性乳液聚合过程中的消耗速率连续地或分段地引入。在每种具体情况下,这取决于引发剂体系的化学性质以及聚合温度。优选在初始装料中包含部分引发剂并且将剩余引发剂以其消耗速率供应至聚合区。为了除去残留单体,引发剂通常还在乳液聚合反应阶段结束后,即单体转化至少95%之后加入。对于进料过程而言,所述单个组分可以从顶部、侧部、或下部、通过反应器底部加入反应器中。
乳液聚合反应制备的水性聚合物分散体的固体含量通常为15至75重量%,优选40至75重量%,更优选大于或等于50重量%。为了反应器的高空间/时间产率,优选具有非常高固体含量的分散体。为了能够实现固体含量>60重量%,应当设置双峰颗粒尺寸或多峰颗粒尺寸,因为否则粘度会变得太高,并且不再能够处理分散体。可以例如通过加入种子(EP81083)、通过加入过量的乳化剂或通过加入细乳化剂而实现新一代颗粒的制备。与高固体含量下的低粘度有关的另一优点为高固体含量下提高了涂层性能。制备一代或多代新颗粒可以在任何所需的时间点进行。所述时间点由用于低粘度的目标粒径分布来指导。
通常,如果将聚合阶段结束后获得的水性聚合物分散体进行为减少残留单体含量的后处理是有利的。所述后处理通过化学方法(例如,通过使用更有效的自由基引发剂体系而完成聚合反应(称为后聚合))和/或物理方法(例如,通过用蒸汽或惰性气体来汽提所述水性聚合物分散体)进行。相应的化学和/或物理方法是技术人员熟知的[参见,例如EP-A771 328、DE-A 196 24 299、DE-A 196 21 027、DE-A 197 41 184、DE-A 19741 187、DE-A198 05 122、DE-A 198 28 183、DE-A 198 39 199、DE-A 19840 586和198 47 115]。化学后处理和物理后处理相结合具有的优势为由所述水性聚合物分散体中不仅移除了未反应的烯键式不饱和单体并且还除去了其他破坏性的挥发性有机化合物(已知为VOC或挥发性有机化合物)。本发明的分散体优选不进行化学后处理。
通过本发明的方法获得的水性聚合物分散体包含的聚合物颗粒的重均粒径Dw的范围为≥10且≤500nm,优选≥20且≤200nm,且特别优选≥20至≤100nm。重均粒径的测定是技术人员已知的并可例如通过分析型超速离心方法而完成。在本说明书中的重均粒径意指通过分析型超速离心方法测定的重均Dw50(关于这方面,参见S.E.Harding et al.,Analytical Ultracentrifugation in Biochemistry and Polymer Science,RoyalSociety of Chemistry,Cambridge,Great Britain 1992,第10章,Analysis of PolymerDispersions with an Eight-Cell AUC Multiplexer:High Resolution Particle SizeDistribution and Density Gradient Techniques,W.第147至175页)。
通过本发明方法获得的且具有的重均粒径Dw≤100nm的水性聚合物分散体表现出出人意料地良好的保色性,并因此特别适用于彩色外部油漆的粘合剂。
此外,可由本发明的水性聚合物分散体简单地(例如通过冷冻干燥或喷雾干燥)获得相应的聚合物粉末。这些本发明可获得的聚合物粉末同样可作为一种组分用在有机基底用涂料和用于改性矿物粘合剂的涂料的制备中。
所述水性聚合物分散体通常具有的固体含量为20至70重量%,优选35至60重量%。
获得的水性聚合物分散体不仅可以其本身、还与其他(通常为成膜)聚合物混合而用作水性涂料中的粘合剂组合物。
通过本发明的方法获得的水性聚合物分散体当然还可作为一种组分用在胶粘剂(adhesives)、密封剂、聚合物抹灰、纸张涂浆、纤维非织造物及有机基底用涂料和用于改性矿物粘合剂的涂料的制备中。
本发明还提供一种水性组合物形式的涂料,包含:
-至少一种如上所述的本发明的聚合物分散体,
-任选地,至少一种(无机)有机填料和/或至少一种(无机)有机颜料,
-任选地,至少一种常规助剂,以及
-水。
本发明的粘合剂组合物优选以水性油漆、更特别为外部油漆的形式使用。
填料可用于增加遮盖力和/或节省白色颜料。为了调节色调的遮盖力和颜色的深度,优选使用有色颜料和填料的共混物。
合适的颜料的实例为:无机白色颜料,例如二氧化钛(优选金红石形式)、硫酸钡、氧化锌、硫化锌、碱式碳酸铅、三氧化锑、锌钡白(硫化锌+硫酸钡);或无机有色颜料,实例为氧化铁、炭黑、石墨、锌黄、锌绿、群青、锰黑、锑黑、锰紫、巴黎蓝或巴黎绿。除了无机颜料之外,本发明的乳化漆还可包含有机有色颜料,实例为乌贼墨、藤黄、颜料棕、甲苯胺红、对位红、汉撒黄、靛蓝、偶氮染料、蒽醌和靛类染料以及二嗪、喹吖啶酮、酞菁、异吲哚啉酮和金属配位颜料。具有用于增加光散射的夹气的合成白色颜料,如和分散体,也是合适的。其他合适的为购自BASF SE的商标名为例如Yellow、Brown和Red,特别是透明形式。
合适的填料为,例如,硅铝酸盐,如长石;硅酸盐,如高岭土、滑石、云母、菱镁矿;碱土金属碳酸盐,如碳酸钙(例如方解石或白垩形式)、碳酸镁、白云石;碱土金属硫酸盐,如硫酸钙;二氧化硅等。当然,在油漆中优选细碎的填料。所述填料可用作单独组分。然而,在实际实施中,已发现填料混合物特别合适,实例为碳酸钙/高岭土、碳酸钙/滑石。光泽油漆通常仅具有少量的极细碎的填料或不含有填料。
细碎的填料还可用于提高遮盖力和/或节省白色颜料。为了调节色调的遮盖力和颜色的深度,优选使用有色颜料和填料的共混物。
颜料的分数可通过颜料体积浓度(PVC)来描述。本发明的涂料具有例如在5至85范围内的PVC,当然,其中的粘合剂也适于仅加入极少分数或不加颜料和/或填料的透明涂层/透明清漆应用。
除聚合物分散体之外,本发明的涂料(水性油漆)还可包含其他助剂。
除了在聚合中所用的乳化剂之外,常规助剂还包括润湿剂或分散剂,例如多磷酸钠、多磷酸钾或多磷酸铵;丙烯酸或马来酸酐共聚物的碱金属盐和铵盐;多磷酸盐,如1-羟基乙烷-1,1二磷酸钠;以及萘磺酸盐,更特别是钠盐。
其他合适的助剂是流动调解剂、消泡剂、生物杀灭剂和增稠剂。合适的增稠剂的实例包括缔合型增稠剂(例如聚氨酯增稠剂)。增稠剂的量优选小于1重量%,更优选小于0.6重量%,基于油漆的固体含量计。
其他合适的助剂为成膜助剂或聚结助剂。优选使用,例如石油溶剂油、乙二醇、丙二醇、丙三醇、乙醇、甲醇、水混溶性乙二醇醚及它们的乙酸酯,如二乙二醇、1-甲氧基-2-丙醇、2-氨基-2-甲基-1-丙醇、异辛醇、丁基乙二醇、丁基二甘醇、二乙二醇单丁醚、二丙二醇单甲醚或二丙二醇单丁醚、二丙二醇甲醚、二丙二醇丙醚、二丙二醇正丁醚、三丙二醇正丁醚、丙二醇苯醚、丁二醇乙酸酯、丁基二甘醇乙酸酯、2,2,4-三甲基-1,3-戊二醇单异丁酸酯,长链二羧酸的二异丁酯(如FBH),或三丙二醇单异丁酸酯。
本发明的油漆以已知的方式通过将组分在用于此目的的常规混合装置中混合而制备。已发现,以下方法是合适的:由颜料、水和任选的助剂制备水性糊料或分散体,并且仅在之后将聚合物粘合剂(即通常为聚合物的水性分散体)与颜料糊料或颜料分散体混合。
本发明的油漆通常包含30至75重量%且优选40至65重量%的非挥发性成分。它们应理解为是指制剂中非水的所有成分,但至少是粘合剂、颜料和助剂的总量,基于油漆的固体含量计。非挥发性成分主要是水。
本发明的油漆可以常规的方式施用至基底,例如通过铺展、喷涂、浸涂、辊涂、刮涂。
所述油漆优选用作建筑油漆,即用于涂覆建筑物或建筑物部件。所述基底可为矿物基底,如抹灰、石膏或石膏板、砖石建筑或混凝土,或者可以是木材、木质材料、金属或纸张(如墙纸),或塑料(如PVC)。
本发明的油漆因操作简单、加工性能良好和增强的保色性而引人注意。所述油漆污染物含量低。其具有很好的性能特性,包括例如良好的防水性、高的湿粘附性、高的抗粘连性和高的再涂覆性,并且它们在施用时表现出良好的流动性。所用的设备可易于用水清洗。
本发明通过下列的非限制性实施例来更详细地阐述。
实施例
发明实施例
将下列组分在大气压力下(绝对值)于20至25℃(室温)下装入装配有锚式搅拌器、加热和冷却装置以及多个进料口的4l的玻璃容器中:
423.0g 去离子水,以及
14.0g 20重量%浓度的脂肪醇聚乙氧基化物的水溶液(购自BASF SE的AT 18)
18.7g 15重量%浓度的十二烷基硫酸钠的水溶液
53.2g 单体乳液(见下文)
然后搅拌(140rpm)加热至内部温度为85℃。在达到该温度后,将5重量%的引发剂溶液一次性加入,并将所得混合物搅拌5分钟。然后,同时开始在185分钟内计量加入单体乳液的总量和在195分钟内计量加入引发剂溶液的剩余量,所述计量进料通过空间上分离的进料口以恒定流速连续地进行。
引发剂溶液:
7g 过二硫酸钠
93g 去离子水
单体乳液:
814.0g 去离子水
10.6g 20重量%浓度的脂肪醇聚乙氧基化物的水溶液(购自BASF SE的AT 18)
47.0g 15重量%浓度的十二烷基硫酸钠的水溶液
169.6g 苯乙烯
301.8g 丙烯酸正丁酯
590.2g 甲基丙烯酸甲酯
307.4g 丙烯酸乙基己酯
14g 丙烯酸,以及
28g 50重量%浓度的丙烯酰胺的水溶液。
然后将反应混合物在上述温度下继续反应15分钟,然后,将该混合物冷却至室温。随后,使用25重量%浓度的氢氧化铵水溶液将获得的水性聚合物分散体的pH值调节至8。所得聚合物分散体的固体分数为50.5重量%,数均粒径为130nm,且玻璃化转变温度为17℃。
固体含量通过使用购自Mettler Toledo的HR73水分分析仪,总体上通过将指定量的水性聚合物分散体(约0.8g)在130℃下干燥至恒重(约2小时)而确定。每种情况下测定两次。每种情况下记录的数据代表这些测试的平均值。
聚合物颗粒的数均粒径通过使用购自Malvern Instruments,England的autosizer IIC,总体上通过在23℃下将0.005至0.01重量%的水性聚合物分散体进行动态光散射而确定。所记录的数据为所测得的自相关函数(ISO标准13321)的累计评估(累积z均)的平均直径。
对比实施例
将下列组分在大气压力下(绝对值)于20至25℃(室温)下装入装配有锚式搅拌器、加热和冷却装置以及多个进料口的4l的玻璃容器中:
423.0g 去离子水,以及
14.0g 20重量%浓度的脂肪醇聚乙氧基化物的水溶液(购自BASF SE的AT 18)
18.7g 15重量%浓度的十二烷基硫酸钠的水溶液
53.2g 单体乳液(见下文)
然后搅拌(140rpm)加热至内部温度为85℃。在达到该温度后,将5重量%的引发剂溶液一次性加入,并将所得混合物搅拌5分钟。然后,同时开始在185分钟内计量加入单体乳液的总量和在195分钟内计量加入引发剂溶液的剩余量,所述计量进料通过空间上分离的进料口以恒定流速连续地进行。
引发剂溶液:
7g 过二硫酸钠
93g 去离子水
单体乳液:
821.0g 去离子水
30g 20重量%浓度的脂肪醇聚乙氧基化物的水溶液(购自BASF SE的AT 18)
50.0g 15重量%浓度的十二烷基硫酸钠的水溶液
758.2g 甲基丙烯酸甲酯
694.8g 丙烯酸乙基己酯
18g 丙烯酸,以及
41.8g 50重量%浓度的丙烯酰胺的水溶液。
然后将反应混合物在上述温度下继续反应15分钟,之后将混合物冷却至室温。随后,使用25重量%浓度的氢氧化铵水溶液将获得的水性聚合物分散体的pH值调节至8。所得聚合物分散体具有的固体分数为50.5重量%,数均粒径为130nm,且玻璃化转变温度为17℃。
性能试验
a)制备油漆制剂
基于实施例的水性聚合物分散体的油漆制剂由下表1所示的成分(以g计)以从上至下显示的顺序在室温下用盘式搅拌器以每分钟1000转搅拌而制备。
表1油漆制剂A(略微硅化的外部油漆)
1)购自Elementis PLC,London,GB的Bentone LT
2)Pigmentverteiler MD20,BASF SE,Ludwigshafen
3)25重量%浓度的多磷酸钠水溶液,BK Giulini,Ladenburg
4)Parmetol A26,&Mayr GmbH,Norderstedt
5)购自Byk Chemie GmbH的022
5)购自BASF SE的丙二醇
6)购自Kronos GmbH的二氧化钛2190
7)购自Mondo Minerals B.V.的M 15(talc)
8)Minex 10,Unimin Speciality Minerals Inc.USA
9)Silres 1306,Wacker Chemie AG,Burghausen
10)购自BASF SE的丁基二甘醇
11)购自BASF SE的Collacral PU70
将最后的组分加入后,继续搅拌15分钟,然后将所得油漆制剂无搅拌静置1小时。
油漆制剂的固体含量约为58%,颜料体积浓度为57。
此外,将有色糊料搅拌入油漆制剂中,得到明显深的、柔和的色调。所述油漆优选使用有机颜料着色,因为凭经验,在人工风化试验中,相比于使用无机颜料的油漆,这些油漆的稳定性更差。表现特别敏感的为具有信号红的调色浆(有机)的油漆,因此,这个色调经常用作油漆稳定性测试的测试色调。每1000g的根据上述配方的油漆各自使用15g购自BASFSE的“Luconyl”颜料糊料。
b)制备涂覆的测试基底
用油漆辊筒以每种情况下每单位面积重量(湿)为300g/m2的方式将上述油漆制剂施用至尺寸为20×30cm的纤维水泥板。然后,将所得涂料在50%相对湿度及23℃的恒温箱中干燥7天。
c)风化试验
为了进行纤维水泥板上的油漆的风化稳定性的人工测试,根据DIN EN ISO 11341(cycle A)对油漆进行氙灯测试,且在500小时后(或使用日光测试在150小时后)进行检测。在该氙灯测试中,将尺寸为5*13cm的经涂覆的纤维水泥板各自交替地干燥照射102分钟以及在用细水雾将所述板湿润的过程中照射18分钟。相对湿度设置为50%,并且黑标准温度为65℃。照射强度相当于光波长为300至400nm的60W紫外光或波长为340nm的0.51W/(m2·nm)。
与人工风化平行地,也使纤维水泥板上的涂层经受室外风化。在室外风化中,将涂层朝上的经涂敷的纤维水泥板的朝向确定为与垂直方向呈60°倾角(0°表示垂直,90°表示与地面平行)。涂层的整体方向为西南。在给定的时间后,类似于人工风化的方法用色度计测量涂层,与未风化的参照油漆对比来评估色偏差ΔE。
必须在油漆完全干燥后,测定风化后的色度值。通过根据DIN 6174:"Colorimetric determination of color coordinates and color differences in theapproximately uniform CIELAB color space"测试风化前后的颜色来测试涂层(L*a*b*色度值),由ΔE=根号((L1-L2)^2+(a1-a2)^2+(b1-b2)^2)的数据存储得到色偏差。
表3
风化测试的结果
可以看出,在全部的测试方法中,不论是人工加速风化还是室外风化,与具有现有技术的粘合剂(各自仅具有一种主要单体M1和M2)的对比油漆相比,对于所列的全部有机有色颜料,本发明的测试油漆均具有较少的褪色(基于色差DE(如上所述))。
Claims (20)
1.一种在涂料中作为粘合剂用于改善保色性的水性聚合物分散体,其包含:
(a)至少两种玻璃化转变温度≥25℃的单体M1,
(b)至少两种玻璃化转变温度<25℃的单体M2,
以及,任选地,其他单体M3;
其中对于单体M1和M2,各自使用更亲水性的单体和更疏水性的单体;且
其中单体M1包括苯乙烯和甲基丙烯酸甲酯;且
其中单体M2选自丙烯酸C1至C20烷基酯或甲基丙烯酸C5至C20烷基酯;且
其中单体M3选自丙烯酸、甲基丙烯酸、丙烯酰胺、(甲基)丙烯酸羟基乙酯或(甲基)丙烯酸羟基丙酯。
2.一种水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,所述水性聚合物分散体包含:
(a)至少两种玻璃化转变温度≥25℃的单体M1,
(b)至少两种玻璃化转变温度<25℃的单体M2,
以及,任选地,其他单体M3;
其中对于单体M1和M2,各自使用更亲水性的单体和更疏水性的单体。
3.根据权利要求2所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述涂料为外部油漆。
4.根据权利要求2或3所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M1选自乙烯基芳族化合物、甲基丙烯酸C1至C4烷基酯、甲基丙烯酸环己酯、丙烯酸十八酯、乙酸乙烯酯、氯化乙烯、烯键式不饱和腈、乙烯基卤化物、乙烯基醚或具有4至8个C原子和两个烯式双键的烃。
5.根据权利要求4所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M1选自乙烯基甲苯、α-甲基苯乙烯和对甲基苯乙烯、α-丁基苯乙烯、4-正丁基苯乙烯、MMA、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、丙烯酸叔丁酯、甲基丙烯酸异丁酯、甲基丙烯酸叔丁酯、乙烯基甲基醚或乙烯基异丁基醚。
6.根据权利要求5所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M1选自苯乙烯/甲基丙烯酸甲酯或者甲基丙烯酸环己酯/甲基丙烯酸甲酯。
7.根据权利要求2或3所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M2选自丙烯酸C1至C20烷基酯、甲基丙烯酸C5至C20烷基酯、具有2至11个C原子的非支链或支链的羧酸的乙烯酯、月桂酸乙烯酯、具有10至13个C原子的支链一元羧酸的乙烯酯、C1-C20乙烯基醚、丁二烯、偏二氯乙烯或单丙烯酸丁二醇酯。
8.根据权利要求7所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M2选自具有9个C原子的α-支链的一元羧酸的乙烯酯、具有10或11个C原子的α-支链的一元羧酸的乙烯酯。
9.根据权利要求8所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M2选自丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯和丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸异丁酯和丙烯酸仲丁酯、丙烯酸正戊酯和丙烯酸异戊酯、丙烯酸正己酯、丙烯酸2-乙基己酯、丙烯酸庚酯、丙烯酸辛酯、丙烯酸C10异戊基格尔伯特醇酯、丙烯酸2-丙基戊酯、丙烯酸1-丙基庚酯、丙烯酸十二烷基酯、甲基丙烯酸正戊酯和甲基丙烯酸异戊酯、甲基丙烯酸正己酯、甲基丙烯酸庚酯、甲基丙烯酸辛酯、甲基丙烯酸C10异戊基格尔伯特醇酯、甲基丙烯酸2-丙基戊酯、甲基丙烯酸2-丙基庚酯、甲基丙烯酸十二烷基酯、丙酸乙烯酯、丁酸乙烯酯、乙酸1-甲基乙烯酯、三甲基乙酸乙烯酯、2-乙基己酸乙烯酯、甲基乙烯基醚、乙基乙烯基醚、丙基乙烯基醚、丁基乙烯基醚、戊基乙烯基醚、己基乙烯基醚、庚基乙烯基醚、辛基乙烯基醚、壬基乙烯基醚、癸基乙烯基醚。
10.根据权利要求9所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M2选自丙烯酸正丁酯/丙烯酸2-乙基己酯。
11.根据权利要求3所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述单体M3选自丙烯酸、甲基丙烯酸、丙烯酰胺、(甲基)丙烯酸羟基乙酯或(甲基)丙烯酸羟基丙酯。
12.根据权利要求6、10和11中任一项所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述粘合剂包含17至27%的单体M1,基于甲基丙烯酸甲酯/苯乙烯计;68至77%的单体M2,基于丙烯酸正丁酯/丙烯酸2-乙基己酯计;和0.1至10%的单体M3;就单体M1而言的苯乙烯的量在5至15%的范围内。
13.根据权利要求6、10和11中任一项所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述粘合剂包含34至44%的单体M1,基于甲基丙烯酸甲酯/苯乙烯计;49至59%的单体M2,基于丙烯酸正丁酯/丙烯酸2-乙基己酯计;和0.1至10%的单体M3;就单体M1而言的苯乙烯的量在10至20%的范围内。
14.根据权利要求6、10和11中任一项所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述粘合剂包含37至47%的单体M1,基于甲基丙烯酸甲酯/苯乙烯计;48至58%的单体M2,基于丙烯酸正丁酯/丙烯酸2-乙基己酯计;和0.1至10%的单体M3;就单体M1而言的苯乙烯的量在10至25%的范围内。
15.根据权利要求6、10和11中任一项所述的水性聚合物分散体在涂料中作为粘合剂用于改善保色性的用途,其中所述粘合剂包含60至70%的单体M1,基于甲基丙烯酸酯/苯乙烯计;24至34%的单体M2,基于丙烯酸正丁酯/丙烯酸2-乙基己酯计;和0.1至10%的单体M3;就单体M1而言的苯乙烯的量在10至25%的范围内。
16.一种涂料组合物,其包含:
-至少一种权利要求2至15中任一项的水性聚合物分散体,
-以及常规助剂和任选地水;
其中对于单体M1和M2,各自使用更亲水性的单体和更疏水性的单体;且
其中单体M1包括苯乙烯和甲基丙烯酸甲酯;且
其中单体M2选自丙烯酸C1至C20烷基酯或甲基丙烯酸C5至C20烷基酯;且
其中单体M3选自丙烯酸、甲基丙烯酸、丙烯酰胺、(甲基)丙烯酸羟基乙酯或(甲基)丙烯酸羟基丙酯。
17.根据权利要求16所述的涂料组合物,其中所述常规助剂为成膜助剂、防腐剂、UV保护剂。
18.一种涂料组合物,其包含:
-至少一种权利要求2至15中任一项的水性聚合物分散体,
-任选地至少一种无机或有机填料和/或至少一种无机或有机颜料,
-任选地至少一种常规助剂,和
-水;
其中对于单体M1和M2,各自使用更亲水性的单体和更疏水性的单体;且
其中单体M1包括苯乙烯和甲基丙烯酸甲酯;且
其中单体M2选自丙烯酸C1至C20烷基酯或甲基丙烯酸C5至C20烷基酯;且
其中单体M3选自丙烯酸、甲基丙烯酸、丙烯酰胺、(甲基)丙烯酸羟基乙酯或(甲基)丙烯酸羟基丙酯。
19.根据权利要求18所述的涂料组合物,其中所述涂料组合物为外部油漆。
20.一种包括建筑材料基底的经涂覆的表面,所述建筑材料基底的主表面的至少一部分区域用权利要求2至15中任一项的水性聚合物分散体作为稳定色调的最终外涂层组合物而覆盖;其中对于单体M1和M2,各自使用更亲水性的单体和更疏水性的单体;且
其中单体M1包括苯乙烯和甲基丙烯酸甲酯;且
其中单体M2选自丙烯酸C1至C20烷基酯或甲基丙烯酸C5至C20烷基酯;且
其中单体M3选自丙烯酸、甲基丙烯酸、丙烯酰胺、(甲基)丙烯酸羟基乙酯或(甲基)丙烯酸羟基丙酯。
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