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CN106661303A - 无氟防水组合物 - Google Patents

无氟防水组合物 Download PDF

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Publication number
CN106661303A
CN106661303A CN201580036693.2A CN201580036693A CN106661303A CN 106661303 A CN106661303 A CN 106661303A CN 201580036693 A CN201580036693 A CN 201580036693A CN 106661303 A CN106661303 A CN 106661303A
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China
Prior art keywords
isomers
weight
composition
substrate
wax
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Granted
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CN201580036693.2A
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CN106661303B (zh
Inventor
沃尔夫冈·克瑙普
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Archroma IP GmbH
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Archroma IP GmbH
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Abstract

一种组合物，其至少包含组分(A)和(B)和任选的组分(C)至(E)中的至少一种：(A)在如下单体的聚合反应中获得的聚丙烯酸酯(M1)CH2＝CR3COO‑R1与(M2)CH2＝CR3COO‑R2和任选地(M3)CH2＝CR3‑X‑R4；(B)蜡(C)封端的异氰酸酯(D)有机聚硅氧烷；(E)蜜胺树脂；其中R1是含有1‑8个碳原子的基团；R2是含有9‑40个碳原子的基团；R3是H、CH3或C2H5；X＝COO、CONHR4是缩水甘油基或CH2(CH2)n‑OR5，其中n是1‑10范围内的整数和R5是H或含有1‑6个碳原子的基团；并且其中所述组合物基于水和/或有机溶剂并且是无氟的。

Description

无氟防水组合物
技术领域
本发明涉及包含由两种不同的(甲基)丙烯酸酯制成的聚丙烯酸酯、石蜡和任选的选自封端异氰酸酯、聚硅氧烷和蜜胺树脂的其它成分的组合物，制备这种组合物的方法，用这种组合物处理基材如纺织品以赋予这种基材疏水性能即防水性能的方法，以及所述经处理的基材本身。所述组合物作为无氟的水性分散体提供。
背景技术
已知用水性分散体处理纺织织物例如机织物、针织物或无纺织物以向它们提供期望的性能。
这种期望的性能是例如防水效果，即疏水效果。为了获得纺织品的防水性，通常使用含氟产品的水性分散体。然而，这种含氟分散体可能带来环境有害的影响。
为了避免使用这种对环境有害的物质，已经建议使用无氟组合物来为诸如纺织品的基材提供疏水性能。
DE 10 2013 209 170涉及包含至少一种硅聚合物和蜡的组合物。
EP 2 411 575涉及不含氟或N-羟甲基化合物的水性分散体，其包含(甲基)丙烯酸烷基酯、苯乙烯或α-甲基苯乙烯，偏二氯乙烯和/或氯化乙烯和任选的(甲基)丙烯酸3-氯-2-羟丙基酯和/或(甲基)丙烯酸缩水甘油酯的共聚物、熔点范围为58-80℃的石蜡和(多种)分散剂，优选阳离子分散剂或者阳离子和非离子分散剂的混合物。
EP 1 899 391涉及包含共聚合的单体的聚合物增量剂组合物，其中所述单体选自各种(甲基)丙烯酸酯、(甲基)丙烯酸酰胺、偏二氯乙烯、氯化乙烯、乙酸乙烯酯或它们的混合物。
EP 1 485 533涉及基于水和/或有机溶剂的制剂及其作为纺织织物上的涂层的用途。所述制剂包含基于蜡的疏水性组分和通过组分与未保护或部分保护的二、三或多异氰酸酯反应产生的反应产物。
EP 2 152 957涉及基于水和/或有机溶剂的无氟组合物及其在纺织品应用中的用途，其基于通过组分与未保护或部分保护的二、三或多异氰酸酯反应产生的反应产物和含有C8-C28烷基的有机聚硅氧烷。
EP 1 424 433涉及包含正链烷烃和基于丙烯酸或甲基丙烯酸的C1-12酯的丙烯酸聚合物的水性体系。
发明内容
发明目的
本发明的目的是提供一种赋予基材如纺织品耐久的防水性能并且对环境无害的组合物。
发明内容
该目的通过包含至少组分(A)和(B)的无氟组合物实现，其中组分(A)是通过聚合两种不同的(甲基)丙烯酸酯制备的聚丙烯酸酯，和组分(B)是蜡、水和/或有机溶剂。
因此，在第一方面，本发明涉及一种组合物，其至少包含组分(A)和(B)和任选的组分(C)至(E)中的至少一种：
(A)在如下单体的聚合反应中获得的聚丙烯酸酯
(M1)CH2＝CR3COO-R1与
(M2)CH2＝CR3COO-R2和任选地
(M3)CH2＝CR3-X-R4；
(B)蜡；
(C)封端的异氰酸酯；
(D)有机聚硅氧烷；
(E)蜜胺树脂；
其中
R1是单体(M1)中含有1-8个碳原子的醇部分；
R2是单体(M2)中含有9-40个碳原子的醇部分；
R3是H、CH3或C2H5；
X是COO或CONH；
R4是缩水甘油基或CH2(CH2)n-OR5，
其中
n是1-10范围内的整数和
R5是H或含有1-6个碳原子的基团；
并且其中所述组合物基于水和/或有机溶剂并且是无氟的。
在一个实施方案中，R1含有1至6个碳原子，R2含有12至40个碳原子。
在另一个实施方案中，R1是支化或非支化或环状C1-C6烷基，R2是支化或非支化或环状C12-C40烷基。
在另一个实施方案中，R1选自如下组成的组中的一个或多个：甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基及其异构体、正己基及其异构体、环丙基、环丁基、环戊基、环己基；和R2选自如下组成的组中的一个或多个：正十二烷基(月桂基)及其异构体、正十三烷基及其异构体、正十四烷基(肉豆蔻基)及其异构体、正十五烷基及其异构体、正十六烷基(十六烷基)及其异构体、正十七烷基及其异构体、正十八烷基(硬脂基)及其异构体、正十九烷基及其异构体、正二十烷基及其异构体、正二十一烷基及其异构体、正二十二烷基(山萮基)及其异构体、正二十三烷基及其异构体、正二十四烷基及其异构体、正二十五烷基及其异构体、正二十六烷基(二十六烷基)及其异构体、正二十七烷基及其异构体、正二十八烷基及其异构体、正二十九烷基及其异构体、正三十烷基(蜂蜡基)及其异构体。
在另一个实施方案中，基于(A)的总量(＝100重量％)，在5至45重量％的单体(M1)与55至95重量％的单体(M2)的聚合反应中获得(A)；或基于(A)的总量(＝100重量％)，在5至44重量％的单体(M1)与55至94重量％的单体(M2)和0.1至20重量％的(M3)的聚合反应中获得(A)。
在另一个实施方案中，蜡具有在50至130℃或60至90℃范围内的熔点。
在另一个实施方案中，蜡是石蜡。
在另一个实施方案中，组合物包含
5至90重量％的(A)；
5至90重量％的(B)；
0至40重量％的(C)；
0至40重量％的(D)；
0至40重量％的(E)；
0.1至90重量％的水和/或有机溶剂；
基于组合物的总量(＝100重量％)。
在另一个实施方案中，组合物另外包含具有两性结构的组分，例如甜菜碱和/或胺N-氧化物(组分(F))。
在一个实施方案中，所述组合物包含
5至90重量％的(A)；
5至90重量％的(B)；
0至40重量％的(C)；
0至40重量％的(D)；
0至40重量％的(E)；
0.1至90重量％的水和/或有机溶剂；
0.1至3重量％的具有两性结构的组分[组分(F)]；
基于组合物的总量(＝100重量％)。
在另一个实施方案中，组合物不含具有N-羟甲基或氯基团的化合物。
在第二方面，本发明涉及制备如前述权利要求中任一项所定义的组合物的方法，其包括至少步骤(C1)至(C2)：
(C1)均质化至少包含单体(M1)和(M2)、和组分(B)以及水和/或有机
溶剂的混合物；
(C2)聚合在步骤(C1)中获得的混合物。
在第三方面，本发明涉及处理基材的方法，其至少包括步骤(S1)：
(S1)使基材与第一方面或本文公开的任一实施方案中定义的组合物接触，
或使基材与根据第二方面中定义的方法制备的组合物接触。
在一个实施方案中，基材是纺织品、纤维、织物、纸、无纺织物、皮革或它们中的两种或更多种的组合。
在一个实施方案中，本发明涉及如第一方面所定义的组合物在用于任何纺织品的整理剂中的用途，或作为其整理剂的用途，所述纺织品的形式为线性构成的形式如线和纱线，平面构成的形式例如织物、针织织物、打结织物、无纺织物、毡，或以空间构成的形式例如用于女士、男士和儿童的短袜(hose)和外套。
在另一个实施方案中，本发明涉及蜡在用于任何纺织品的整理剂中的用途，或作为其整理剂的用途，所述蜡包含75-95重量％的量的正链烷烃和5至25重量％的量的异链烷烃和/或环烷烃和/或芳族化合物或由它们组成，基于蜡的总量(＝100重量％)，其中正链烷烃具有20至60个碳原子，优选其中正链烷烃的分子量为300至600，所述纺织品的形式为线性构成的形式如线和纱线，平面构成的形式例如织物、针织织物、打结织物、无纺织物、毡，或以空间构成的形式例如用于女士、男士和儿童的短袜和外套。
在第四方面，本发明涉及一种基材，其至少包含如第一方面中所定义的组分(A)和(B)。
在一个实施方案中，基材是或已经通过如第三方面中定义的方法处理的。
在一个实施方案中，基材是线性构成的形式如线和纱线，平面构成的形式例如织物、针织织物、打结织物、无纺织物、毡，或以空间构成的形式例如用于女士、男士和儿童的短袜和外套；或者是纺织品、纤维、织物、纸、无纺织物、皮革或它们中的两种或更多种的组合。
具体实施方式
第一方面：根据本发明的组合物
在第一方面，本发明涉及一种组合物，其至少包含组分(A)和(B)和任选的组分(C)至(E)中的至少一种：
(A)在如下单体的聚合反应中获得的聚丙烯酸酯
(M1)CH2＝CR3COO-R1与
(M2)CH2＝CR3COO-R2和任选地
(M3)CH2＝CR3-X-R4；
(B)蜡；
(C)封端的异氰酸酯；
(D)有机聚硅氧烷；
(E)蜜胺树脂；
其中
R1是含有1-8个碳原子的基团；
R2是含有9-40个碳原子的基团；
R3是H、CH3或C2H5；
X是COO或CONH；
R4是缩水甘油基或CH2(CH2)n-OR5，
其中
n是1-10范围内的整数和
R5是H或含有1-6个碳原子的基团；
并且其中所述组合物基于水和/或有机溶剂并且是无氟的。
组分(A)
组分(A)是在单体(M1)与单体(M2)的聚合反应中获得的反应产物。任选地，单体(M3)可以另外使用到单体(M1)和单体(M2)中。
术语“在单体(M1)与单体(M2)和任选单体(M3)的聚合反应中获得的聚丙烯酸酯”是指所述聚丙烯酸酯[组分(A)]包含衍生自单体(M1)和(M2)和任选的单体(M3)的部分或由它们组成(在下文中，引号中的所有术语在本发明的含义中定义)。
单体(M1)和单体(M2)是相互不同的丙烯酸酯。术语“相互不同”是指单体(M1)和单体(M2)至少在单体的酯部分不同。
单体(M1)
根据本发明，单体(M1)是丙烯酸酯CH2＝CR3COO-R1，其中R1表示含有1-8个碳原子的基团。R3选自H、CH3或C2H5。
在单体(M1)的定义中使用的术语“基团”表示酯或单体(M1)的醇部分。
在一个实施方案中，R1是可以是饱和或不饱和的支化或非支化或环状的C1-C8烷基。
优选地，R1选自甲基、乙基、正丙基、异丙基、正丁基、仲丁基、异丁基、叔丁基、正戊基及其异构体、正己基和异构体、正庚基及其异构体、正辛基及其异构体、环丙基、环丁基、环戊基、环己基、环庚基和环辛基。
也可以使用不同单体(M1)的混合物。
与R1相关的术语“异构体”涵盖位置异构体。
在一个实施方案中，R1表示含有1-6个碳原子的基团，即所述酯的醇部分。
在一个实施方案中，R1是可以是饱和或不饱和的支化或非支化或环状的C1-C6烷基。
优选地，R1选自甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基及其异构体、正己基及其异构体、环丙基、环丁基、环戊基、环己基。
单体(M2)
根据本发明，单体(M2)是丙烯酸酯CH2＝CR3COO-R2，其中R2表示含有9-40个碳原子的基团，即所述酯的醇部分。R3选自H、CH3或C2H5。
在单体(M2)的定义中使用的术语“基团”表示酯或单体(M2)的醇部分。
在一个实施方案中，R2是可以饱和或不饱和的支化或非支化或环状的C9-C40烷基。
优选地，R2选自正壬基及其异构体、正癸基及其异构体、正十一烷基及其异构体、正十二烷基(月桂基)及其异构体、正十三烷基及其异构体、正十四烷基(肉豆蔻基)及其异构体、正十五烷基及其异构体、正十六烷基(十六烷基)及其异构体、正十七烷基及其异构体、正十八烷基(硬脂基)及其异构体、正十九烷基及其异构体、正二十烷基及其异构体、正二十一烷基及其异构体、正二十二烷基(山萮基)及其异构体、正二十三烷基及其异构体、正二十四烷基及其异构体、正二十五烷基及其异构体、正二十六烷基(二十六烷基)及其异构体、正二十七烷基及其异构体、正二十八烷基及其异构体、正二十九烷基及其异构体、正三十烷基(蜂蜡基)及其异构体。
也可以使用不同单体(M2)的混合物。
与R2相关的术语“异构体”涵盖位置异构体。
在一个实施方案中，R2表示含有12-40个碳原子的基团，即所述酯的醇部分。
在一个实施方案中，R2是可以饱和或不饱和的支化或非支化或环状的C12-C40烷基。
优选地，R2选自如下组成的组中的一个或多个：正十二烷基(月桂基)及其异构体、正十三烷基及其异构体、正十四烷基(肉豆蔻基)及其异构体、正十五烷基及其异构体、正十六烷基(十六烷基)及其异构体、正十七烷基及其异构体、正十八烷基(硬脂基)及其异构体、正十九烷基及其异构体、正二十烷基及其异构体、正二十一烷基及其异构体、正二十二烷基(山萮基)及其异构体、正二十三烷基及其异构体、正二十四烷基及其异构体、正二十五烷基及其异构体、正二十六烷基(二十六烷基)及其异构体、正二十七烷基及其异构体、正二十八烷基及其异构体、正二十九烷基及其异构体、正三十烷基(蜂蜡基)及其异构体。
在一个实施方案中，单体(M1)的R1是支化或非支化或环状C1-C6烷基，且R2是支化或非支化或环状C12-C40烷基，它们分别可以是饱和或不饱和的。
优选地，R1选自如下组成的组中的一个或多个：甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基及其异构体、正己基及其异构体、环丙基、环丁基、环戊基、环己基；和R2选自如下组：正十二烷基(月桂基)及其异构体、正十三烷基及其异构体、正十四烷基(肉豆蔻基)及其异构体、正十五烷基及其异构体、正十六烷基(十六烷基)及其异构体、正十七烷基及其异构体、正十八烷基(硬脂基)及其异构体、正十九烷基及其异构体、正二十烷基及其异构体、正二十一烷基及其异构体、正二十二烷基(山萮基)及其异构体、正二十三烷基及其异构体、正二十四烷基及其异构体、正二十五烷基及其异构体、正二十六烷基(二十六烷基)及其异构体、正二十七烷基及其异构体、正二十八烷基及其异构体、正二十九烷基及其异构体、正三十烷基(蜂蜡基)及其异构体。
在一个实施方案中，单体(M1)的R1是支化或非支化或环状C1-C5烷基，且R2是支化或非支化或环状C14-C40烷基，它们分别可以是饱和或不饱和的。
优选地，R1选自如下组成的组中的一个或多个：甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基及其异构体、环丙基、环丁基、环戊基；和R2选自如下组：正十四烷基(肉豆蔻基)及其异构体、正十五烷基及其异构体、正十六烷基(十六烷基)及其异构体、正十七烷基及其异构体、正十八烷基(硬脂基)及其异构体、正十九烷基及其异构体、正二十烷基及其异构体、正二十一烷基及其异构体、正二十二烷基(山萮基)及其异构体、正二十三烷基及其异构体、正二十四烷基及其异构体、正二十五烷基及其异构体、正二十六烷基(二十六烷基)及其异构体、正二十七烷基及其异构体、正二十八烷基及其异构体、正二十九烷基及其异构体、正三十烷基(蜂蜡基)及其异构体。
在根据本发明的组合物中，基于(A)的总量(＝100重量％)，优选在5至45重量％的单体(M1)与55至95重量％的单体(M2)的反应中获得(A)；或基于(A)的总量(＝100重量％)，在20至40重量％的单体(M1)与60至80重量％的单体(M2)的反应中获得(A)。
单体(M3)
根据本发明，所述组合物可以在单体(M3)的存在下制备，所述单体(M3)是单体CH2＝CR3-X-R4。
在一个实施方案中，单体(M3)是丙烯酸的缩水甘油酯(X＝COO和R4＝缩水甘油基)。
在另一个实施方案中，单体(M3)是丙烯酸的酯，其中酯部分具有醚基团(X＝COO和R4＝CH2(CH2)n-OR5)，其中n是在1-10范围内的整数，R5是H或含有1至6个碳原子的基团，优选支化或非支化或环状烷基。优选n为在1-4范围内的整数，R5为H或含有1至4个碳原子的基团，优选支化或非支化或环状烷基。
在优选的实施方案中，如果R4＝CH2(CH2)n-OR5，n是在1-4范围内的整数和R5是H或正丁基或异丁基。
在一个实施方案中，单体(M3)是(甲基)丙烯酸羟乙酯。术语“(甲基)丙烯酸酯”包括丙烯酸酯和甲基丙烯酸酯。
在另一个实施方案中，单体(M3)是丙烯酸酰胺的缩水甘油酯(X＝CONH和R4＝缩水甘油基)。
在另一个实施方案中，单体(M3)是丙烯酸酰胺的酯，其中酯部分具有醚基团(X＝CONH和R4＝CH2(CH2)n-OR5)，其中n是在1-10范围内的整数，R5是H或含有1至6个碳原子的基团，优选支化或非支化或环状烷基。优选n在1-4范围内，R5为H或含有1至4个碳原子的基团，优选支化或非支化或环状烷基。
也可以使用不同单体(M3)的混合物。
在丙烯酸酯或丙烯酸酰胺的优选实施方案中，如果R4＝CH2(CH2)n-OR5，n是在1-4范围内的整数和R5是H或正丁基或异丁基。
具有缩水甘油基的单体(M3)可赋予具有可与所述缩水甘油基反应的基团(例如羟基或氨基)的基材增加的粘附性。
如果存在单体(M3)，优选在5至44重量％的(M1)与55至94重量％的(M2)和0.1至20重量％的(M3)的反应中获得(A)，基于(A)(＝100重量％)的总量。
组分(B)
根据本发明，组分(B)是蜡，优选具有疏水性即防水性的蜡。
基本上所有已知的蜡可以用于根据本发明的组合物中，即天然蜡、化学改性的蜡和合成蜡，条件是它们具有疏水性。本文所用的术语“蜡”是指在出版物“Chemielexikon，第9版，第6卷，第4972页中给出的定义。
因此，天然蜡可以基于植物蜡、动物蜡、矿物蜡、石化蜡。
植物蜡例如是巴西棕榈蜡，动物蜡例如是蜂蜡。
矿物蜡例如是地蜡。
也可以使用石化蜡，例如凡士林、石蜡和微晶蜡。
化学改性蜡是诸如山萮酯蜡和沙索蜡的蜡。
合成蜡是基于聚亚烷基和聚乙二醇的蜡。
在优选的实施方案中，蜡选择为具有50-100℃，更优选60-90℃，还更优选60-80℃的熔点。熔点根据ASTM D 938-05/DIN ISO 2207：1983测定。
包含具有低于50℃的熔融范围的蜡的根据本发明的组合物有时不太适用于对待用根据本发明的水性分散体处理的纺织品赋予防水性。具有高于100℃的熔融范围的蜡可导致可接受的防水性和织物的耐洗涤性，但它们可导致水性分散体的增加的粘度，使得这些分散体在技术上较不容易处理。因此，基本上，具有在100至130℃范围内的熔点的蜡也适合于根据本发明的组合物。
因此，通常，根据组分(B)的蜡的熔点可以在50至130℃的范围内。
优选地，蜡是石蜡。
石蜡是含有碳原子数20-60的正链烷烃为主要成分并含有少量异链烷烃和/或环烷烃类和/或芳香族化合物的混合物。正链烷烃优选具有300-600的分子量。
分子量使用凝胶渗透色谱法进行测定。正链烷烃、异链烷烃、环烷烃和芳族化合物的分布可以使用13C NMR光谱测定。
在一个实施方案中，蜡包含75-95重量％的量的正链烷烃和5-25重量％的量的异链烷烃和/或环烷烃和/或芳族化合物或由它们组成，基于蜡的总量(＝100重量％)。
例如，熔融范围为68℃至74℃的石蜡是可商购的(CAS号8002-74-2)。
这种合适的蜡是可商购的，例如Sasolwax 8775、Sasolwax 7040、Sasolwax3971、Sasolwax 6805或Sasolwax 2222。
组分(C)(任选地)
根据本发明，组合物可任选地包含封端或部分封端的异氰酸酯。
术语“封端的异氰酸酯”包括其中异氰酸酯基团已经与封端剂反应的单异氰酸酯、二异氰酸酯和多异氰酸酯，其在加热时释放异氰酸酯和封端剂。合适的封端剂是本领域已知的，例如胺、酰胺、具有活性氢原子的化合物或醇。如果所述加热在具有能够与所述异氰酸酯基团反应的官能团(例如合适的基材如纤维的羟基或氨基)的化合物的存在下进行，则可导致改善的粘附性。
因此，存在于根据本发明的组合物中的封端异氰酸酯，特别是封端多异氰酸酯，可以赋予具有可以与所述封端异氰酸酯反应的基团例如胺或羟基的基材增加的粘附性。
组分(C)可以以基于组合物的总量(＝100重量％)为0-40重量％的量存在。
这种合适的封端异氰酸酯是可商购的，例如Arkophob DAN、Arkophob SR，和Cassurit FF(均为Archroma)；Phobol XAN(Huntsman)和Ruco-Guard WEB(Rudolf)。
组分(D)(任选地)
根据本发明，组合物可任选地包含有机聚硅氧烷树脂。
术语“有机聚硅氧烷”包括这样的化合物，其中至少一部分硅原子带有又可以被取代的烷基或芳基。所述聚硅氧烷可以是环状的、线性的或支化的。
可以使用本领域已知的用于向基材提供防水性的任何有机聚硅氧烷树脂。合适产品例如从DE 10 2013 209 170和EP 2 152 957中已知。
组分(D)可以以基于组合物的总量(＝100重量％)为0-40重量％的量存在。
这样的聚硅氧烷制剂是可商购的，例如Ceraperm SFC(Archroma)、Powersoft FE55或Wacker Finish WR 210(均为德国的Wacker Chemie)。
组分(E)(任选地)
根据本发明，组合物可任选地包含蜜胺树脂。
合适的蜜胺树脂例如是其中蜜胺部分的氨基的氢原子被CH2O-烷基或CH2OC2烷基部分或完全取代的树脂。这样的产品从US 3 480 579已知。
其它合适的蜜胺树脂是其中蜜胺部分的氨基的氢原子被饱和或不饱和、线性、支化和/或环状烃部分或完全取代的树脂。这样的产品例如从DE 10 2013 209170中已知。
组分(D)可以以基于组合物的总量(＝100重量％)为0-40重量％的量存在。
含有这种合适的蜜胺树脂的制剂是可商购的，例如Cerol EX(Archroma)或Freepel 1225(Emerald Performance Materials)或Phobotex JVA(Huntsman)。这种蜜胺树脂可包括石蜡如组分(B)。
水和/或有机溶剂
根据本发明，组合物基于水和/或有机溶剂。
术语“基于水和/或有机溶剂”包括在组合物中含有的固体和/或液体化合物在水和/或有机溶剂中的溶液、乳液和分散体。术语“溶液”、“乳液”和“分散体”可互换使用。
术语“水”包括蒸馏水以及管道水。
术语“有机溶剂”优选包括与水混溶或部分水溶性的溶剂。优选的有机水混溶性溶剂是C1-2醇，二醇如乙二醇和丙二醇，二丙二醇或聚乙二醇，酰胺如N-甲基甲酰胺和N,N-二甲基甲酰胺。
部分水溶性溶剂也是合适的。优选的有机溶剂是二丙二醇二甲醚，乙酸甲氧基丙酯，乙酸甲氧基丁酯(丁氧基)和乙酸甲氧基甲基丁酯。
优选地，组合物主要基于水。术语“主要”是指基于水和有机溶剂(＝100重量％)的总重量，有机溶剂的量小于50重量％。在优选的实施方案中，有机溶剂的量小于40重量％，更优选小于30重量％，还更优选小于20重量％，还更优选小于10重量％。在一个实施方案中，组合物不含有机溶剂。
根据本发明的组合物可以包含基于组合物的总量(＝100重量％)的0.1至90重量％的水和/或有机溶剂。
在一个实施方案中，组合物包含5-90重量％的(A)；5-90重量％的(B)；0-40重量％的(C)；0-40重量％的(D)；0-40重量％的(E)；和0.1-90重量％的水和/或有机溶剂，基于组合物的总量(＝100重量％)。
在一个实施方案中，根据本发明的水性组合物的固体含量为10至50重量％，优选20至40重量％，更优选25至35重量％，基于组合物的总量(＝100重量％)。
无氟
术语“无氟”是指组合物由不含氟的组分制成。
此外，在一个实施方案中，为了提供尽可能不对环境有害的组合物，根据本发明的组合物不含一种或多种以下化合物，其通常用于赋予基材疏水性：N-羟甲基化合物如N-羟甲基丙烯酰胺或带有N-羟甲基的蜜胺树脂，因为N-羟甲基化合物具有这样的缺点，即它们在环境气氛中，特别是在升高的温度下可能释放不希望量的甲醛；含氯产物，特别是源于通常用于制备防水组合物的单体如氯化乙烯或偏二氯乙烯。
另外，在优选的实施方案中，根据本发明的组合物不含具有N-羟甲基或氯基团的化合物。
组分(A)至(E)是本领域已知的或可以根据已知方法制备。
第二方面：根据本发明的组合物的制备
根据本发明的组合物可以通过在水和/或有机溶剂中将单体(M1)和(M2)和任选地(M3)聚合并混合组分(B)来制备。所述聚合也可以在组分(B)的存在下进行。如果需要，可以加入一种或多种已知为纺织品处理组合物的组分的其它组分(C)至(E)，优选在聚合反应终止之后。
在优选的实施方案中，根据本发明的组合物可以通过在组分(B)的存在下在水和/或有机溶剂中聚合单体(M1)和(M2)和任选的(M3)来制备。如果需要，可以加入一种或多种已知为纺织品处理组合物的组分的其它组分(C)至(E)，优选在聚合反应终止之后。
在优选的实施方案中，在聚合之前，将(M1)和(M2)和任选的(M3)和组分(B)在水和/或有机溶剂中的混合物均化。该方法示例性地解释如下：
优选在分散剂(作为组分(F))的存在下，将蜡(组分(B))和单体(M1)和(M2)和任选的单体(M3)熔化。例如通过使用Turrax搅拌，将所得混合物分散在热水中，例如85℃的热水中。然后进行高压均化，例如在400巴和80至85℃的温度下。为此，所获得的加热的混合物可以通过喷嘴或均化器的孔口。合适的装置是本领域已知的。在均化之后，可以冷却分散体并加入聚合催化剂，优选分散或溶解在水中：分散体也可以在升高的温度如80℃下聚合。在例如50℃至80℃反应几小时后，终止聚合。
合适的分散剂(组分(F))是已知的，并且可以选自市售产品，例如非离子表面活性剂，乙氧基化产物，例如乙氧基化醇或乙氧基化羧酸。市售的阳离子活性产物可以是季铵盐或与这种阳离子活性产物和非离子产物如单或二丙二醇的混合物。其它合适的分散剂是具有两性结构的化合物，例如具有甜菜碱和/或胺N-氧化物官能团。
根据本发明的组合物优选含有基于组合物总量(＝100重量％)的0.1至3重量％，优选0.5至3重量％的分散剂或分散剂混合物。
通常，共聚反应作为通过使用聚合反应催化剂的自由基共聚反应进行。作为用于自由基聚合的催化剂，使用通常已知的用作自由基引发剂的购买产品。在本发明中，尤其可以使用偶氮化合物作为催化剂。合适的催化剂是例如2,2'-偶氮双(2-脒基丙烷)二盐酸盐。
所使用的聚合催化剂的量可以为基于单体(M1)和(M2)和任选的(M3)(＝100重量％)的混合物计为0.1-5重量％，优选2.5-5重量％。
因此，本发明涉及制备如第一方面所定义的组合物的方法，其包括：
(C1)均质化至少包含单体(M1)和(M2)和任选地(M3)、和组分(B)以及水和/或有机溶剂的混合物；
(C2)聚合在步骤(C1)中获得的混合物。
优选地，均化在100至1,000巴的压力和50至100℃的温度下进行，优选通过使混合物通过喷嘴或孔。
优选地，均化在200-600巴的压力和60-90℃的温度下进行。
合适的均化器是本领域已知的。
第三方面：根据本发明的组合物的用途
根据本发明的组合物特别可用于赋予基材防水性。
术语“防水性”定义纤维、纱线或织物抵抗湿润的特性，如AATCC测试方法11-2010中所定义。
因此，本发明涉及一种处理基材的方法，其至少包括步骤(S1)：
(S1)使基材与第一方面中定义的组合物或根据第二方面中定义的方法制备的组合物接触。
术语“处理基材”包括诸如“整理基材”、“赋予基材疏水性”、“使基材防水”、“使基材耐污染”或“涂布基材”的术语。
基材的接触可以通过通常的常规方法进行，例如将基材浸泡或浸渍到根据本发明的组合物中，或通过将根据本发明的组合物喷雾到基材上，或通过刷涂或海绵涂布或通过强制施用或通过提取方法。在接触之后，可以干燥接触的基材，并且如果合适，在140℃至190℃的温度范围内固化。在低或甚至环境固化条件下也可实现优异的性能，意味着在低于100℃的温度下或甚至在低至50℃的温度下。
优选地，基材是纺织品、纤维、织物、纸、无纺织物、皮革或其两种或更多种的组合。
纺织品优选由棉，聚酯或棉/聚酯共混物，由聚酰胺，聚酰亚胺，聚苯硫醚，芳族聚酰胺，聚氯乙烯，聚丙烯腈，聚乙酸乙烯酯，聚四氟乙烯，聚乙烯，聚丙烯，聚氨酯，弹性纤维，碳纤维，硅酸盐纤维，玻璃纤维，玄武岩纤维，金属纤维或其两种或更多种的混合物制成。纺织品通常是机织物、针织物或无纺织物。
因此，通常，根据本发明的组合物可以用作基材例如纺织织物的整理剂或整理。优选地，基材以线性、平面构成或空间构成的形式提供。
术语“整理剂或整理”包括可用以赋予基材以防水性的组合物。可以在清洗基材之前或之后对基材施加整理剂。
在一个实施方案中，根据本发明的组合物可以用于任何纺织品(＝基材)的整理剂中或用作整理剂。纺织品可以是线性构成的形式如线和纱线，平面构成的形式如织物，针织织物，打结织物，无纺织物，毡，并且空间构成的形式例如用于女士、男士和儿童的短袜和外套。
在一个实施方案中，本发明涉及蜡在用于基材例如纺织织物的整理剂中或作为整理剂的用途，所述蜡包含75-95重量％的正链烷烃和5至25重量％的异链烷烃和/或环烷烃和/或芳族化合物或由它们组成，基于蜡的总量计，其中正链烷烃具有20至60个碳原子，优选其中正链烷烃具有300至600的分子量。优选地，基材以线性、平面构成或空间构成的形式提供。
术语“线性构成(linear formations)”、“平面构成(planar formations)”和“空间构成(spatial formations)”是纺织业中已知的。
根据本发明的组合物也可以作为整理剂施用于待洗涤的外套。
在第四方面，本发明涉及一种基材，其至少包含如第一方面中所定义的组分(A)和(B)。
在一个实施方案中，所述基材是或已经通过如第三方面中定义的方法处理的。
实施例
实施例#1至#9:根据本发明的组合物的制备
将5g甲基丙烯酸叔丁酯和15g丙烯酸硬脂基酯加入到在10g二丙二醇和120g水中的4.8g Genapol ID 100(脂肪醇乙氧基化物(Clariant))和0.4g十六烷基三甲基氯化铵的热混合物中，在大约80℃通过搅拌分散。在另一容器中，将40g石蜡(熔融范围68-74℃)熔融。将上述单体分散体加入熔融石蜡中。进一步分散2分钟后从而通过Manton-Gaulin均化器设备(在400巴，85℃下)将混合物均化两次，直到获得稳定的乳液。温度保持在75-80℃之间，加入在1.8g水中稀释的0.2g的2,2-偶氮双(2-甲基丙脒)二盐酸盐引发剂(Wako V-50)，将混合物在75℃下在N2下在穿戴(donned)回流冷凝器下处理6小时。得到大约200g活性物含量约为33重量％(通过在120℃/2小时干燥测定)的产物。
类似于对实施例#1所述的方法，使用其它单体组合和石蜡类型以产生稳定的分散体。细节示于表1中：
表1
(t-BuMA＝甲基丙烯酸叔丁酯；i-BuMA＝甲基丙烯酸异丁酯；MMA＝甲基丙烯酸甲酯；HexAC＝丙烯酸己基酯；SA＝丙烯酸硬脂基酯；BeMA＝丙烯酸山嵛基酯；LA＝丙烯酸月桂基酯；HEMA＝甲基丙烯酸羟乙基酯；GMA＝甲基丙烯酸缩水甘油基酯；HBAC＝丙烯酸羟丁基酯；石蜡：Sasolwax 8775)
实施例#10:该实施例描述了用根据实施例#1-#9制备的分散体处理纺织品织物
对织造的100％聚酯织物(100g/m2)和织造的100％棉织物(200g/m2)进行处理。棉织物使用含有1g/的乙酸、20g/l的纤维素交联剂和50g/l和70g/l的实施例#1-#9的分散体的浆液(liquor)在轧染机(pad mangle)中进行处理。浆液的典型重量吸收为80％。聚酯织物用含有1g/l的乙酸、1g/l的润湿剂和40和60g/l实施例#1-#9的分散体的浆液进行轧染。典型重量吸收为60％。在轧染后，织物在160℃下干燥3分钟。
将根据实施例#10获得的成品织物在40℃下在初始和10次洗涤循环后(DIN ISO6330)进行根据AATCC 22-2010，ISO 4920(EN 24920)的水喷雾试验。在洗涤循环之后，在喷雾测试之前将织物滚筒干燥。典型的滚筒干燥温度60-65℃下30分钟。根据喷雾测试评级图表，等级100意味着织物的表面没有粘附或润湿，等级90意味着织物表面的轻微随机粘附或润湿，等级80意味着在喷涂点处织物的表面润湿，等级70表示织物的表面部分润湿超过喷涂点，等级50表示织物的整个表面完全润湿。
聚酯
棉
实施例 #1 #2 #3 #4 #5 #6 #7 #8 #9
施用量50g/l
初始 100 100 100 100 100 100 100 100 90
10x洗涤循环 70 50 70 70 70 50-70 70 70 50
施用量70g/l
初始 100 100 100 100 100 100 100 100 90
10x洗涤循环 80 70 80 80 80 70-80 80 90 70
实施例对于聚酯甚至在洗涤之后即便在低添加量时显示非常好的防水效果。对于棉，获得非常好的初始效果。
通过加入另外的交联剂，例如Cassurit FF，对聚酯，但特别是对棉织物的防水效果的耐久性可以进一步提高。
棉
聚酯
通过将20g/l的蜜胺树脂制剂(例如Cerol EX或Freepel 1225)加入到应用浴中，实现了防水效果耐久性的类似改善。
尽管用实施例#1-#9的制剂处理的织物已经具有良好的手感，但是有时期望使处理的织物具有特别的额外柔软的手感。这可以通过除了该应用浴还添加基于有机聚硅氧烷的软化剂制剂，例如Ceraperm SFC，来实现。
聚酯
除了非常柔软舒适的手感之外，还实现了非常好的初始和持久的防水性。

Claims (15)

1.一种组合物，其至少包含组分(A)和(B)和任选的组分(C)至(E)中的至少一种：
(A)在如下单体的聚合反应中获得的聚丙烯酸酯
(M1)CH2＝CR3COO-R1与
(M2)CH2＝CR3COO-R2和任选地
(M3)CH2＝CR3-X-R4；
(B)蜡；
(C)封端的异氰酸酯；
(D)有机聚硅氧烷；
(E)蜜胺树脂；
其中
R1是单体(M1)中含有1-8个碳原子的醇部分；
R2是单体(M2)中含有9-40个碳原子的醇部分；
R3是H、CH3或C2H5；
X是COO或CONH；
R4是缩水甘油基或CH2(CH2)n-OR5，
其中
n是1-10范围内的整数和
R5是H或含有1-6个碳原子的基团；
并且其中所述组合物基于水和/或有机溶剂并且是无氟的。
2.根据权利要求1所述的组合物，其中R1含有1至6个碳原子，且R2含有12至40个碳原子。
3.根据权利要求1或2所述的组合物，其中R1是支化或非支化或环状C1-C6烷基，且R2是支化或非支化或环状C12-C40烷基。
4.根据前述权利要求任一项所述的组合物，其中R1选自如下组成的组中的一个或多个：甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基及其异构体、正己基及其异构体、环丙基、环丁基、环戊基、环己基；和R2选自如下组成的组中的一个或多个：正十二烷基(月桂基)及其异构体、正十三烷基及其异构体、正十四烷基(肉豆蔻基)及其异构体、正十五烷基及其异构体、正十六烷基(十六烷基)及其异构体、正十七烷基及其异构体、正十八烷基(硬脂基)及其异构体、正十九烷基及其异构体、正二十烷基及其异构体、正二十一烷基及其异构体、正二十二烷基(山萮基)及其异构体、正二十三烷基及其异构体、正二十四烷基及其异构体、正二十五烷基及其异构体、正二十六烷基(二十六烷基)及其异构体、正二十七烷基及其异构体、正二十八烷基及其异构体、正二十九烷基及其异构体、正三十烷基(蜂蜡基)及其异构体。
5.根据前述权利要求任一项所述的组合物，其中基于(A)的总量(＝100重量％)，在5至45重量％的单体(M1)与55至95重量％的单体(M2)的聚合反应中获得(A)；或基于(A)的总量(＝100重量％)，在5至44重量％的单体(M1)与55至94重量％的单体(M2)和0.1至20重量％的(M3)的聚合反应中获得(A)。
6.根据前述权利要求任一项所述的组合物，其中蜡具有在50至130℃或60至90℃范围内的熔点。
7.根据前述权利要求任一项所述的组合物，其中所述蜡是石蜡。
8.根据前述权利要求任一项所述的组合物，其中基于组合物的总量(＝100重量％)，所述组合物包含
5至90重量％的(A)；
5至90重量％的(B)；
0至40重量％的(C)；
0至40重量％的(D)；
0至40重量％的(E)；
0.1至90重量％的水和/或有机溶剂。
9.根据前述权利要求任一项所述的组合物，其中所述组合物不含具有N-羟甲基或氯基团的化合物。
10.制备如前述权利要求中任一项所定义的组合物的方法，其包括至少步骤(C1)至(C2)：
(C1)均质化至少包含单体(M1)和(M2)、和组分(B)以及水和/或有机溶剂的混合物；
(C2)聚合在步骤(C1)中获得的混合物。
11.处理基材的方法，其至少包括步骤(S1)：
(S1)使基材与根据权利要求1-9任一项中定义的组合物接触，或使基材与权利要求10中定义的方法制备的组合物接触。
12.一种基材，其至少包含如权利要求1中所定义的组分(A)和(B)。
13.根据权利要求12所述的基材，其通过权利要求11所述的方法进行处理。
14.根据权利要求12或13所述的基材，或根据权利要求11所述的方法，其中所述基材是线性构成的形式如线和纱线，平面构成的形式例如织物、针织织物、打结织物、无纺织物、毡，或以空间构成的形式例如用于女士、男士和儿童的短袜和外套；或者所述基材是纺织品、纤维、织物、纸、无纺织物、皮革或它们中的两种或更多种的组合。
15.根据权利要求1-9任一项中定义的组合物的用途，或蜡的用途，用于任何纺织品的整理剂中或作为其整理剂，基于蜡的总量，所述蜡包含75-95重量％的量的正链烷烃和5至25重量％的量的异链烷烃和/或环烷烃和/或芳族化合物或由它们组成，其中正链烷烃具有20至60个碳原子，优选其中正链烷烃的分子量为300至600，所述纺织品的形式为线性构成的形式如线和纱线，平面构成的形式例如织物、针织织物、打结织物、无纺织物、毡，或以空间构成的形式例如用于女士、男士和儿童的短袜和外套。
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