CN101970544A - 含有粘结剂的胶态的有机聚硅氧烷水分散体及其用途 - Google Patents
含有粘结剂的胶态的有机聚硅氧烷水分散体及其用途 Download PDFInfo
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- CN101970544A CN101970544A CN2009801086384A CN200980108638A CN101970544A CN 101970544 A CN101970544 A CN 101970544A CN 2009801086384 A CN2009801086384 A CN 2009801086384A CN 200980108638 A CN200980108638 A CN 200980108638A CN 101970544 A CN101970544 A CN 101970544A
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- Prior art keywords
- silane
- water
- alkyl
- base
- colloidal
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- 229910000077 silane Inorganic materials 0.000 claims abstract description 70
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 69
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Abstract
本发明涉及含粘结剂的胶态的水分散体(B),其包含:(a)由以下通式的单元构成的有机聚硅氧烷:R1 xSi(OR2)yO(4-x-y)/2 (I),其中x是0、1、2或3,且y是0、1或2,条件是x+y的总和≤3,R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,该一价烃基可以任选包括水惰性的取代基,R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,该烃基可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3、-COC2H5或-CH2CH20H,(b)水溶性的或自分散性的含硅烷的聚乙烯醇和/或聚乙烯基酯和/或共聚物,条件是多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷,(c)任选存在的表面活性化合物,例如乳化剂,和(d)水。还公开了一种采用含粘结剂的胶态的水分散体(B)处理纤维状和薄膜状基材的方法,尤其是处理地毯和垫子。
Description
本发明涉及含粘结剂的胶态的有机聚硅氧烷水分散体,及其用于处理纤维型和片型基材的用途,更具体而言,用于天然和/或合成来源的纤维型基材,更优选织物地板覆盖物,例如地毯和地毯地板(carpet flooring)。
有机聚硅氧烷水溶胶是众所周知的,其制备方法描述在例如US3,433,780、US 4,857,582(对应于DE 37 17 075 A1)和US 5,281,657(对应于EP 492 377 A2)中。
相似地,使用有机聚硅氧烷水溶胶作为浸渍和涂布剂也是已知的。DE1 594 985 A要求保护用于处理天然和合成纤维材料的用途。其特别阐述到,在用胶态的有机基倍半硅氧烷悬浮体浸渍后,地毯产品表现出改进的防干污物(dry soil)性。
DE 30 04 824 A1选择有机基倍半硅氧烷与二氧化硅水溶胶的胶态悬浮体的组合,用于织物材料的绒毛稳定化。但是,有机基倍半硅氧烷的薄膜经证实硬且脆;即,有机基倍半硅氧烷在柔韧可弯曲且可出皱纹的基材上的涂层往往易碎,且微粒形式容易因机械应力而剥离。
为此,有机基聚倍半硅氧烷通常要与粘结剂材料一同使用。出于防水和防油性的目的,织物领域中的粘结剂通常包括含碳氟化合物的体系。US6,225,403涉及一种处理织物基材的组合物及方法,以带来防油、防水和防污性。为此,将少于1%的碳氟化合物树脂与例如至多10%的水溶胶形式的有机基倍半硅氧烷共聚物颗粒共同使用。但这种混合比不太可能提供对所述基材的足够粘附性。目前通常期望的是不含全碳氟化合物的粘结剂体系,这种期望源自环境争论以及碳氟化合物可能的在人体内的残留。
用于有机基倍半硅氧烷的不含碳氟化合物的粘结剂体系同样重复地出现在专利文献中。
例如,US 2003/0099844 A1描述了用于制备绝缘薄膜的涂料组合物,其包括烷氧基硅烷和/或其水解产物、有机聚合物、水、醇和任选存在的有机增溶剂。该有机聚合物可以尤其是聚乙烯醇或聚乙烯基酯。聚乙烯醇被用作保护胶,其用于稳定有机聚硅氧烷的水溶胶也在上述US 5,281,657(对应于EP 492 377 A2)中被提及。
在European Polymer Journal 43(2007),1123-1131页的“Preparation andproperties of poly(vinyl alcohol)/silica nanocomposites derived fromcopolymerization of vinyl silica nanoparticles and vinyl acetate”中,Xin Jia等人描述了纳米复合材料的制备。合成通过含乙烯基的二氧化硅与乙烯乙烯酯的原位自由基共聚合进行。随后的皂化导致可成膜的聚乙烯醇,由于共价结合的有机硅颗粒的含量,其具有改进的机械稳定性和热稳定性。二氧化硅颗粒在纳米复合材料中的比例最大高达4重量%。防污性对于采用这种材料的涂层来说是不太可能的。
含硅烷的有机聚合物也见述于文献中。通常,其是通过烯烃有机单体与烯烃官能的硅烷的自由基共聚合而制备的。特别地,乙酸乙烯酯或乙烯基醇的共聚物可以通过这种方法得到。其实例记载在EP 76 490 A1、US2004/0014857A(对应于EP 1 382 621 A1)和DE 10 2005 054 913A1中。
含硅烷的乙酸乙烯酯或乙烯基醇共聚物的涂层具有良好的薄膜质量和基材粘附性,但是有机聚硅氧烷水溶胶的涂层不具有这种防污性。
然而,结合有机聚硅氧烷水溶胶与合适的不含碳氟化合物的有机粘结剂、以便实现在纤维基材上有良好的防污效果及优良的薄膜性能是有问题的。这是因为实际上发现,只有少量的有机粘结剂配制品与有机聚硅氧烷水溶胶相容,即不会导致有机聚硅氧烷水溶胶的凝胶化。有机聚硅氧烷水溶胶的良好薄膜质量和粘附性此时就会要求添加如此多的粘结剂,以至于可以看出的是,没有防污效果或实质上受损了的防污效果。
本发明的目的是提供稳定的、不含碳氟化合物的且成膜的组合物,其基于胶态的有机聚硅氧烷水分散体,该组合物可提供对纤维或片型基材的良好粘附性,更具体而言,是针对织物地板覆盖物,例如地毯和地毯地板,同时,有机聚硅氧烷组分所导致的防污性能够以基本上未改变的形式保留下来。本发明人发现,所述目的可通过以下的发明而得以实现:
含粘结剂的胶态的水分散体(B),其包含:
(a)由以下通式的单元构成有机聚硅氧烷:
R1 xSi(OR2)yO(4-x-y)/2 (I)
其中x是0、1、2或3,且y是0、1或2,
条件是x+y的总和≤3,
R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,其可以任选包括水惰性的取代基,
R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,其可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3、-COC2H5或-CH2CH2OH,
(b)水溶性的或自分散性的含硅烷的聚乙烯醇和/或聚乙烯基酯和/或共聚物,条件是多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷,
(c)任选存在的表面活性化合物,例如乳化剂,和
(d)水。
根据本发明的胶态的水分散体(B)可以任选含有(e):其它的可与水混溶的添加物。
优选地,含粘结剂的胶态的水分散体(B)优选以下面的用量包含以下组分(a)-(e):
100重量份的组分(a),
0.1-70重量份、优选0.5-40重量份、更优选1.0-20重量份的组分(b),
0-70重量份、优选0.1-70重量份、更优选1.0-20重量份的组分(c),
50-10000重量份、优选100-3000重量份的组分(d),以及任选存在的0-20重量份、优选0.0001-20重量份的组分(e)。
本发明还提供一种制备含粘结剂的胶态的水分散体(B)的方法,其通过混合胶态的有机聚硅氧烷的水分散体(A)与组分(b)-水溶性或自分散性的含硅烷的聚乙烯醇和/或聚乙酸乙烯酯和/或其共聚物来制备,其中(A)包含:
(a)由式(I)的单元所构成的有机聚硅氧烷,
(c)任选存在的表面活性化合物,例如乳化剂,和
(d)水,
条件是,多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷。
本发明还提供一种用含粘结剂的胶态的水分散体(B)处理纤维型和片型基材的方法,所述基材优选天然和/或合成来源的纤维型基材,更优选织物地板覆盖物,更优选地毯和地毯地板,(B)包含:
(a)由以下通式的单元构成的有机聚硅氧烷:
R1 xSi(OR2)yO(4-x-y)/2 (I)
其中x是0、1、2或3,且y是0、1或2,
条件是x+y的总和≤3,
R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,其可以任选包括水惰性的取代基,
R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,其可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3、-COC2H5或-CH2CH2OH,
(b)水溶性的或自分散性的含硅烷的聚乙烯醇和/或聚乙烯基酯和/或共聚物,条件是多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,并且其中至少一种单体单元含有连接的硅烷,
(c)任选存在的表面活性化合物,例如乳化剂,和
(d)水。
烃基R1的实例是烷基,例如甲基、乙基、正丙基、异丙基、正丁基、仲丁基、戊基、己基、β-乙基己基和庚基;链烯基,例如乙烯基、烯丙基和丁烯基;炔基;环烷基,例如环丁基、环己基、和甲基环己基;芳基,例如苯基;烷芳基,例如甲苯基;以及芳烷基,例如苄基。特别优选的是甲基、乙烯基和苯基。
取代的烃基R1的实例是卤代烃基;例如氯甲基、3-氯丙基、3-溴丙基、3,3,3-三氟丙基和5,5,5,4,4,3,3-七氟戊基,以及氯苯基、二氯苯基和三氯苯基;巯烷基,例如2-巯乙基和3-巯丙基;氰烷基,例如2-氰乙基和3-氰丙基;氨烷基,例如3-氨丙基、N-(2-氨乙基)-3-氨丙基和N-(2-氨乙基)-3-氨基(2-甲基)丙基;氨基芳基,例如氨基苯基;酰氧基烷基,例如3-丙烯酰氧基丙基和3-甲基丙烯酰氧基丙基;羟烷基,例如羟丙基;以及下式的基:
HOCH2CH(OH)CH2SCH2CH2-,
HOCH2CH2OCH2-,和
优选R2是氢原子,或相同或不同的每个基具有1-4个碳原子的烷基或烷氧基亚烷基。
烃基R2的实例是烷基,例如甲基、乙基、正丙基、异丙基、正丁基、仲丁基、叔丁基;和烷氧基亚烷基,例如甲氧基亚乙基和乙氧基亚乙基。特别优选的是甲基和乙基。
优选地在式(I)中,x平均是1.0-2.0,y平均是0-0.5。
制备胶态的有机聚硅氧烷水分散体(A)的方法对于本领域技术人员来说是已知的,并且描述在US 3,433,780、US 4,857,582(对应于DE 37 17 075A1)和US 5,281,657(对应于EP 492 377 A2)中(通过引用而结合)。
举例来说,胶态的有机聚硅氧烷水分散体(A)可如下得到:当有机硅化合物,例如式R1 xSi(OR2)4-x的硅烷(其中x、R1和R2各自定义如上)和/或其部分水解产物以及任选存在的低聚的有机聚硅氧烷在表面活性化合物的存在下与水混合,以形成分散体时。
制备所用的含硅烷的聚乙烯醇(b)的方法对于所属领域技术人员来说是已知的,并且描述在US 2004/0014857A(对应于EP 1 382 621 A1)和DE 102005 054 913 A1中(通过引用而结合)。
基于部分或完全皂化的乙烯基酯共聚物的含硅烷的聚乙烯醇(b)可通过例如乙烯基酯与烯键式不饱和的含硅烷单体及任选存在的其它可共聚合共聚单体的自由基聚合、以及所得聚合物的皂化而得到。含硅烷的聚乙烯醇(b)也可以例如通过乙烯基醇聚合物与烯键式不饱和的含硅烷单体的自由基接枝聚合而得到。
合适的含硅烷的聚乙烯醇(b)是完全皂化的或部分皂化的乙烯基酯聚合物,其水解度为75-100mol%,含硅烷的共聚单体单元的分数为0.01-10mol%。完全皂化的乙烯基酯聚合物的水解度优选97.5-100mol%,更优选98-99.5mol%。部分皂化的聚乙烯基酯的水解度为优选80-95mol%,更优选86-90mol%。粘度(根据DIN53015,以4重量%的水溶液计)被用于作为部分或完全皂化的、硅烷化的乙烯基酯聚合物的分子量和聚合度的量度,25℃下的该粘度的范围优选2-50mPa·s。
适宜的乙烯基酯是支化的或未支化的具有1-18个碳原子的羧酸的乙烯基酯。优选的乙烯基酯是乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、2-乙基己酸乙烯酯、月桂酸乙烯酯、特戊酸乙烯酯和具有5-13个碳原子的α-支化的一元羧酸的乙烯基酯,优选或(Shell的商品名)。乙酸乙烯酯为特别优选。
含有具有1-6个碳原子的烷基和具有1-6个碳原子的羧酸的优选的1-烷基乙烯基酯是1-甲基乙烯基乙酸酯、1-乙基乙烯基乙酸酯及1-丙基乙烯基乙酸酯。
乙烯基酯单元可以任选地与一种或多种选自以下组中的单体共聚合:具有1-15个碳原子的醇的甲基丙烯酸酯和丙烯酸酯、烯烃、二烯、乙烯基芳族化合物和乙烯基卤化物。源自丙烯酸酯和甲基丙烯酸酯的适宜单体是具有1-15个碳原子的支化或未支化醇的酯。优选的甲基丙烯酸酯或丙烯酸酯是丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸叔丁酯、丙烯酸2-乙基己酯、丙烯酸降冰片烯酯。特别优选的是丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、丙烯酸2-乙基己酯、丙烯酸降冰片烯酯。适宜的二烯是1,3-丁二烯和异戊二烯。可聚合的烯烃的实例是乙烯和丙烯。可用的乙烯基芳族化合物是苯乙烯和乙烯基甲苯。可用的乙烯基卤化物典型地是氯乙烯、偏二氯乙烯或氟乙烯,优选氯乙烯。这些共聚单体的分数确定为能够使乙烯基酯单体在乙烯基酯聚合物中的分数为>50mol%。
如果需要,其它的共聚单体可以以分数优选0.1-25mol%存在。其实例是烯键式不饱和的一羧酸和二羧酸,优选丙烯酸、甲基丙烯酸、富马酸和马来酸;烯键式不饱和的羧酸酰胺和腈,优选N-乙烯基甲酰胺、丙烯酰胺和丙烯腈;富马酸和马来酸的一酯和二酯,例如二乙酯和二丙酯,及马来酸酐;烯键式不饱和磺酸或其盐,优选乙烯基磺酸、2-丙烯酰胺基-2-甲基丙磺酸。其它实例是预交联的共聚单体,例如多烯键式不饱和共聚单体,实例是二乙烯基己二酸酯、二烯丙基马来酸酯、烯丙基甲基丙烯酸酯、二丙烯酸丁二醇酯或三烯丙基氰尿酸酯,或后交联的共聚单体,实例为丙烯酰胺基乙醇酸(AGA)、甲基丙烯酰胺基乙醇酸甲酯(MAGME)、N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺、N-羟甲基烯丙基氨基甲酸酯;烷基醚,例如N-羟甲基丙烯酰胺、N-羟甲基-甲基丙烯酰胺和N-羟甲基烯丙基氨基甲酸酯的异丁氧基醚或酯。
适宜的烯键式不饱和的含硅烷单体为例如以下通式的烯键式不饱和的硅化合物:
R3SiR4 a(OR5)3-a,
其中a是0、1或2,R3是CH2=CR6-(CH2)0-3-或CH2=CR6CO2(CH2)1-3-,R4是C1至C3-的烷基、C1至C3-烷氧基或卤素,优选Cl或Br,R5是支化或未支化的任选取代的具有1-12个碳原子的烷基,优选1-3碳原子,或是具有2-12个碳原子的酰基,在此情形下,R5可任选被醚基插入,R6是H或CH3。
适宜的烯键式不饱和的含硅烷单体还包括含硅烷基的以下通式的(甲基)丙烯酰胺:
CH2=CR7-CO-NR8-R9-SiR10 m-(R11)3-m,
其中m为0-2,R7是H或甲基,R8是H,或具有1-5个碳原子的烷基,R9是具有1-5个碳原子的亚烷基,或二价有机基,其中碳链可任选插入氧或氮原子,R10是具有1-5个碳原子的烷基,R11是具有1-40个碳原子的烷氧基,其可以被其它杂环取代。在其中2个或多个R7或R11基团存在的单体中,这些可以相同或不同。这种(甲基)丙烯酰胺基烷基硅烷的实例有:
3-(甲基)丙烯酰胺基丙基三甲氧基硅烷、3-(甲基)丙烯酰胺基丙基三乙氧基硅烷、3-(甲基)丙烯酰胺基-丙基三(β甲氧基乙氧基)硅烷、2-(甲基)丙烯酰胺基-2-甲基丙基三甲氧基硅烷、2-(甲基)丙烯酰胺基-2-甲基乙基三甲氧基硅烷、N-(2-(甲基)丙烯酰胺基乙基)氨丙基三甲氧基硅烷、3-(甲基)丙烯酰胺基丙基三乙酰氧基硅烷、2-(甲基)丙烯酰胺基乙基三甲氧基硅烷、1-(甲基)丙烯酰胺基甲基三甲氧基硅烷、3-(甲基)丙烯酰胺基丙基甲基二甲氧基硅烷、3-(甲基)丙烯酰胺基丙基二甲基甲氧基硅烷、3-(N-甲基(甲基)丙烯酰胺基)丙基三甲氧基硅烷、3-((甲基)丙烯酰胺基甲氧基)-3-羟丙基三甲氧基硅烷、3-((甲基)丙烯酰胺基甲氧基)丙基三甲氧基硅烷、N,N-二甲基-N-三甲氧基甲硅烷基丙基-3-(甲基)丙烯酰胺基丙基氯化铵和N,N-二甲基-N-三甲氧基甲硅烷基丙基-2-(甲基)丙烯酰胺基-2-甲基丙基氯化铵。
优选的烯键式不饱和的含硅烷单体是γ-丙烯酰基或γ-甲基丙烯酰氧基丙基三(烷氧基)硅烷,α-甲基丙烯酰氧基甲基三(烷氧基)硅烷、γ-甲基丙烯酰氧基丙基甲基二(烷氧基)硅烷;乙烯基硅烷类,例如乙烯基烷基二(烷氧基)硅烷和乙烯基三(烷氧基)硅烷,其中烷氧基可以是例如甲氧基、乙氧基、甲氧基亚乙基、乙氧基亚乙基、甲氧基丙二醇醚或乙氧基丙二醇醚基。优选的含硅烷单体的实例是3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷;乙烯基三甲氧基硅烷、乙烯基甲基二甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基甲基二乙氧基二乙氧基硅烷、乙烯基三丙氧基硅烷、乙烯基三异丙氧基硅烷、乙烯基三(1-甲氧基)异丙氧基硅烷、乙烯基三丁氧基硅烷、乙烯基三乙酰氧基硅烷、甲基丙烯酰氧基甲基三甲氧基硅烷、3-甲基丙烯酰氧基丙基三(2-甲氧基乙氧基)硅烷、乙烯基三氯硅烷、乙烯基甲基二氯硅烷、乙烯基三(2-甲氧基乙氧基)硅烷、三乙酰氧基乙烯基硅烷、烯丙基乙烯基三甲氧基硅烷、烯丙基三乙酰氧基硅烷、乙烯基二甲基甲氧基硅烷、乙烯基二甲基乙氧基硅烷、乙烯基甲基二乙酰氧基硅烷、乙烯基二甲基乙酰氧基硅烷、乙烯基异丁基二甲氧基硅烷、乙烯基三异丙基氧(isopropyloxy)硅烷、乙烯基三丁氧基硅烷、乙烯基三己基氧硅烷、乙烯基甲氧基二己氧基(hexoxy)硅烷、乙烯基三辛基氧硅烷、乙烯基二甲氧基辛基氧硅烷、乙烯基甲氧基二辛基氧硅烷、乙烯基甲氧基二月桂基氧硅烷、乙烯基二甲氧基月桂基氧硅烷,以及聚乙二醇改性的乙烯基硅烷。
最优选的硅烷是乙烯基三甲氧基硅烷、乙烯基甲基二甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基甲基二乙氧基硅烷、乙烯基三(1-甲氧基)异丙氧基硅烷;甲基丙烯酰氧基丙基三(2-甲氧基乙氧基)硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷和甲基丙烯酰氧基甲基三甲氧基硅烷,及其混合物。
根据本发明分散体(B)的制备任选采用乳化剂的表面活性化合物(c),例如具有9-20个碳原子的羧酸;具有至少6个碳原子在脂族取代基中的脂族取代的苯磺酸;具有至少4个碳原子在脂族取代基中的脂族取代的萘磺酸;具有至少6个碳原子在脂族取代基中的脂族磺酸;具有至少6个碳原子在烷基取代基中的甲硅烷基烷基磺酸;具有至少6个碳原子在脂族取代基中的脂族取代的二苯基醚磺酸;具有至少6个碳原子在烷基取代基中的烷基氢硫酸酯;烷基和烷芳基醚硫酸酯,其具有至少6个碳原子在疏水基中,及1-40环氧乙烷(EO)和/或环氧丙烷(PO)单元;氨基乙磺酸(tauride)类;磺基琥珀酸与具有4-15个碳原子的一元醇或烷基酚的酯和单酯,其任选被乙氧基化1-40个EO单元;以及所提及的酸的碱金属盐和铵盐;磷酸部分酯及其碱金属盐和铵盐,尤其是具有8-20个碳原子在有机基中的烷基和烷芳基磷酸酯;分别具有8-20个碳原子在烷基和烷芳基中、和1-40个EO单元的烷基醚和烷芳基醚磷酸酯;具有8-24个碳原子的伯、仲和叔的脂肪胺与乙酸、硫酸、盐酸和磷酸的盐;季烷基-和烷基苯铵盐,更具体而言,是其烷基具有6-24个碳原子的那些,更具体而言是卤化物、硫酸盐;磷酸盐和乙酸盐;季铵氢氧化物;烷基吡啶鎓、烷基咪唑啉鎓和烷基噁唑啉鎓盐;更具体而言是烷基链具有至多18个碳原子的那些,具体来说是卤化物、硫酸盐、磷酸盐和乙酸盐;烷基聚乙二醇醚,优选具有3-40个EO单元和8-20个碳原子的烷基的那些,烷基芳基聚乙二醇醚,优选具有5-40个EO单元和8-20个碳原子在烷基和芳基中的那些;环氧乙烷-环氧丙烷(EO-PO)嵌段共聚物,优选具有8-40个EO和/或PO单元的那些;具有8-22个碳原子的烷基的烷基胺与环氧乙烷或环氧丙烷的加成产物;通式R*O-Zo的烷基多糖苷,其中R*是直链或支链的、饱和或不饱和的平均具有8-24个碳原子的烷基,Zo是低聚糖苷,其平均具有o=1-10个己糖或戊糖单元,或它们的混合物;天然物及其衍生物,例如卵磷脂、羊毛脂、皂角苷、纤维素、纤维素烷基醚和羟烷基纤维素,其每一种的烷基具有至多4个碳原子;直链的含极性基团的有机基(聚)硅氧烷,更具体而言,含有元素O、N、C、S、P,更具体而言,具有至多24个碳原子的烷氧基和/或至多40个环氧乙烷(EO)和/或环氧丙烷(PO)基团的那些有机基(聚)硅氧烷;由长链取代基取代的氨基酸,例如N-烷基二(氨乙基)甘氨酸,或N-烷基-2-氨基丙酸盐;甜菜碱,例如具有C8-C18的酰基的N-(3-酰基酰氨基丙基)-N,N-二甲基铵盐,和烷基咪唑啉鎓甜菜碱。
阳离子或阴离子乳化剂可优选用于表面活性化合物。
所有提及的酸都可以原样使用,或如果需要的话,可以与其盐的掺混物使用。
当使用阴离子乳化剂时,有利的是使用这样的阴离子乳化剂,其脂族取代基包含至少8个、更具体12个碳原子。脂族取代基的具体实例是辛基、癸基、十二烷基、十六烷基、十八烷基、三十烷基、油基、壬烯基、辛炔基、植基(phythyl)和十五二烯基。脂族取代的苯磺酸优选用作阴离子乳化剂。
当使用阳离子乳化剂时,有利的是使用卤化物,更具体而言,使用氯化物和溴化物。
乳化剂在制备胶态的有机聚硅氧烷水分散体(A)中的用量可以非常小。乳化剂的用量优选0.1-70.0重量%,更优选用量为1.0-20.0重量%,全部以胶态的有机聚硅氧烷水分散体(A)制备中所用的有机硅化合物的重量计。
为了制备胶态的有机聚硅氧烷水分散体(A),乳化剂不仅可以与水一同加入,而且可以与有机硅化合物一同加入。
但是,在很多应用中乳化剂都会有破坏性的效果,其中乳化剂可能会被洗掉,或能够在边界层扩散和聚集。因此,除上面所提及的乳化剂,更有利地是使用乙酸加成至3-氨丙基三甲氧基硅烷或3-氨丙基三乙氧基硅烷的盐,尤其有利的是乙酸加成至N-(2-氨乙基)-3-氨丙基三甲氧基硅烷或N-(2-氨乙基)-3-氨丙基三乙氧基硅烷的盐,其优选与所用的有机硅化合物水解和浓缩,并且在所述过程中共同被引入到有机聚硅氧烷骨架中。
可以在本发明的胶态的水分散体(B)中存在的可与水混溶的添加物(e)的实例有酸,例如甲酸、乙酸、丙酸、磷酸、盐酸、硫酸,或碱,例如三乙胺、三乙醇胺、三辛胺、氨水溶液、氢氧化锂、氢氧化钠、氢氧化钾、氢氧化铯,还有乙二醇、聚乙二醇、1,2-丙二醇、1,3-丙二醇、聚丙二醇、二甘醇单丁醚或丙三醇。还可以使用分散体或乳液作为其它的物质(e),实例是可商购的分散体,例如苯乙烯-丁二烯胶乳、丙烯酸类、乙烯基类、聚氨酯或聚乙烯分散体,以及天然或合成油的乳液、树脂或蜡,例如加洛巴蜡、蜂蜡、羊毛蜡、芦荟、维生素E、石蜡油、非反应性硅油、非反应性硅树脂、加州希蒙得木油、米糠油、金盏花油、茶树油、玫瑰油或滇荆芥油(balm oil)乳液。作为其它的物质,可以为分散体添加可商购的防腐剂,例如异噻唑啉酮或对羟基苯甲酸酯,或其含水的配制品。
含硅烷的聚乙烯醇/酯(b)可以以纯状态混合,即以物质状态,或以与准备好的有机聚硅氧烷分散体(A)的水溶液形式,或者在计量加入硅烷之前在开始时与水(d)加入,以及任选地与表面活性化合物(c)一起加入(在制备有机聚硅氧烷分散体(A)的过程中)。
优选的是,使用含硅烷的聚乙烯醇/酯(b)的水溶液,更优选(b)是浓度为1%-30重量%的溶液。
当含硅烷的聚乙烯醇/酯(b)与准备好的有机聚硅氧烷分散体(A)混合时,后者优选以初始温度10°-95℃、更优选50-90℃进料,而含硅烷的聚乙烯醇/酯(b)则通过计量加料加入。
当含硅烷的聚乙烯醇/酯(b)在开始时与水(d)和任选存在的表面活性化合物(c)在制备有机聚硅氧烷的分散体(A)之前进料时,将要分散的有机硅化合物优选以温度1-95℃、更优选以温度30-90℃计量加入。
当使用与水混溶的添加剂(e)时,添加剂(e)可以在混合胶态的有机聚硅氧烷水分散体(A)与组分(b)之前、同时或之后加入。
本发明的含粘结剂的胶态的水分散体(B)可用于处理天然和合成来源的任何需要的纤维材料。原则上,对所有的纤维材料而言,其耐滑性、亚光处理(matt finish)和/或耐干污性都会得到改进。
含粘结剂的胶态的水分散体(B)优选被涂覆到基材上,再使其干燥,涂覆优选在温度为10-200℃下进行。
用本发明的含粘结剂的胶态的水分散体(B)处理的纤维材料例如由以下材料所构成:羊毛、头发、黄麻、亚麻、棉、再生纤维素纤维、人造丝、尼龙、丙烯酸酯类、聚丙烯腈、聚偏二氯乙烯、聚酯、乙酸纤维素、玻璃及其共混物或混合物。该分散体也可以被涂覆至皮革或人造皮革。
本发明的含粘结剂的胶态的水分散体(B)可以以任何需要的方式涂覆至纤维材料。例如,纤维可以浸渍到分散体中或拖拽通过,或可以将分散体通过铺展、涂刷、喷撒、泡沫或喷涂来涂覆。优选的是泡沫涂覆、浸染(pad-mangle)涂覆、接触辊涂覆以及通过排气式方法的涂覆。
就使用而言,本发明的胶态的水分散体可以以任何比例用水稀释;优选的是使用全部以稀释的有机聚硅氧烷水分散体重量计浓度为0.05-10.0重量%的有机硅化合物。
还可以将本发明的胶态的水分散体(B)适用于与清洁剂配制。这特别可用于例如涂覆所述分散体至住宅区或办公室中的长条地毯或地毯,因为这样可在一次操作中提供不仅可用于清洁,而且可增加耐干物污染性。
通常有利的是,使用的分散体浓度使得其中所含的有机聚硅氧烷的量为0.5-15g/m2纤维材料。特别优选的量为1-10g/m2。
在本发明的含粘结剂的胶态的水分散体(B)被涂覆后,干燥纤维材料。干燥可以以任何需要的方式进行。最简单的方法是例如暴露处理过的纤维材料至空气中,以使水分蒸发。但是,干燥也可以通过鼓空气或其它气体,更具体而言,可以通过鼓加热过的气体在纤维材料上而加速干燥。这里的干燥条件各自依赖于纤维材料的种类、量和密度。举例来说,短绒聚酰胺地毯可有利地在100-130℃下干燥10-15分钟。
制备实施例:
不含粘结剂的甲基倍半硅氧烷水溶胶的制备,不是根据本发明:
对比产品1:
将1078g完全不含离子的水、1.7g氢氧化钾(20%,在甲醇中)和20.8g N-烷基(C12-18)-N,N-二甲基-N-苄基氯化铵(50%,在水中)在开始时进料,并加热至50℃。然后,在搅拌下将294g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入157g完全不含离子的水。将混合物加热至90℃,并进一步蒸馏,直到得到量为500g的馏出液。将产物冷却至室温,并采用75μm的聚酰胺滤布(filter fabric)过滤。水溶胶为微乳色(opalescent)的稀液体,其平均粒度为41nm。
对比产品2:
将1182g完全不含离子的水和11.3g 4-C10-13-仲烷基苯磺酸在开始时进料,并加热至50℃。然后,在搅拌下将228g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入770g完全不含离子的水。将混合物加热至90℃,并进一步蒸馏,直到得到量为350g的馏出液。将水溶胶冷却至80℃,并用氨水溶液(25%)调节至pH7。将产物冷却至室温,并采用75μm的聚酰胺滤布过滤。水溶胶为乳色的稀液体,其平均粒度为79nm。
具有不含硅烷的聚乙烯醇的甲基倍半硅氧烷水溶胶的制备,不是根据
本发明,不稳定:
对比产品3:
将1078g完全不含离子的水、1.7g氢氧化钾(20%,在甲醇中)、20.8gN-烷基-(C12-18)-N,N-二甲基-N-苄基氯化铵(50%,在水中)和81g聚乙烯醇水溶液(10%)(LL 2870,购自Wacker Polymers)在开始时进料,并加热至50℃。然后,在搅拌下将294g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入157g完全不含离子的水。混合物加热至90℃,并进一步蒸馏。当得到约150g的馏出液后,形成了坚硬的凝胶(firm gel),其不能进一步进行处理。
含纳米颗粒的聚乙烯醇通过自由基聚合的制备,根据Xin Jia等人的
European Polymer Journal 43(2007),1123-1131页,不是根据本发明:
对比产品4:
中间体:
具有乙烯基的纳米颗粒的官能化
将5.0g胶体二氧化硅(比表面积400m2/g;SiOH含量2SiOH/nm2)搅拌到60ml的甲醇中。将该混合物与10ml乙烯基三乙氧基硅烷惨混,并在慢速搅拌下超声波分散3次,每次30分钟。在超声波处理之间每次继续搅拌10分钟。其后,将分散体通过蓝色色带纸过滤。过滤的剩余物在65℃下干燥16小时,然后在研钵中粉碎。粉碎的粉末用甲醇进行Soxhlet萃取10小时,以除去硅烷残余物。随后,含乙烯基的二氧化硅在65℃下干燥16小时。所述二氧化硅的乙烯基含量通过IR光谱法进行定量验证。
自由基聚合:
将3.2g中间体与76.8g乙酸乙烯酯和50ml甲醇混合,并通过超声波分散30分钟。其后,将混合物加热至60-65℃,并与0.8g过氧化苯甲酰掺混,以引发聚合。混合物在60-65℃下搅拌4小时。接下来用240ml甲醇稀释,温度上升至70-72℃。为了进行皂化,将16ml的氢氧化钠水溶液(25%)加入。过滤掉沉淀的聚乙烯醇,并将其分散到400ml水中。为了完成皂化,将另外的16ml氢氧化钠水溶液加入,接下来在70-72℃搅拌混合物6小时。其后,过滤混合物,除去未结合的二氧化硅部分。完全皂化的聚乙烯醇用约400ml甲醇从清澈的馏出液中沉淀出来。将固体过滤掉,用少量甲醇洗涤,并在60℃下干燥过夜。干燥产品的二氧化硅含量通过IR光谱法进行定量验证。然后在研钵中粉碎聚合物,并进一步在90℃下处理,以形成微黄色的5%的在水中的溶液。
具有含碳氟化合物的粘结剂的甲基倍半硅氧烷水溶胶的制备,不是根
据本发明:
对比产品5:
将2.67g 30%的碳氟化合物分散体(NUVA FB liquid,购自Clariant)混入对比实施例1的100g的甲基倍半硅氧烷水溶胶中。形成了稳定的乳白色的稀混合物。
含硅烷的聚乙烯醇的制备,根据DE 10 2005 054 913 A1(粘结剂,其本
身不是根据本发明):
对比产品6:
在搅拌下,在恒温的实验室装置(容积为2.5升)中在氮气下初始进料1000g 20%的聚乙烯醇水溶液(Mowiol 8-88,源自Kuraray SpecialitiesEurope),接下来在搅拌下将其加热至90℃。初始进料在90℃下搅拌2h,在温度下降至80℃前,将15g乙烯基三乙氧基硅烷(Geniosil GF56,源自Wacker Chemie)添加至聚乙烯醇溶液中。在15分钟的匀化后,通过添加10g3%的过硫酸钾水溶液,使反应开始。将温度保持在80℃下4小时,在该批次物料冷却下来之前,得到了清澈的聚合物溶液,其固含量为21重量%,并具有基于硅烷改性的聚乙烯醇总重量7.0重量%的硅烷分数。
具有含硅烷的聚乙烯醇的甲基倍半硅氧烷水溶胶的制备,根据本发明
实施例1:
将1078g完全不含离子的水、1.7g氢氧化钾(20%,在甲醇中)和20.8gN-烷基(C12-18)-N,N-二甲基-N-苄基氯化铵(50%,在水中)在开始时进料,并加热至50℃。然后,在搅拌下将294g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入157g完全不含离子的水。将混合物加热至90℃,并进一步蒸馏,直到得到量为500g的馏出液。将水溶胶冷却至80℃。其后,将44g根据对比实施例6制备的粘结剂以1克/分钟的速度搅拌进来。将产物冷却至室温,并采用75μm的聚酰胺滤布过滤。该含粘结剂的水溶胶是乳色的稀液体,其平均粒度为97nm。
实施例2:
将1078g完全不含离子的水、1.7g氢氧化钾(20%,在甲醇中)和20.8g N-烷基(C12-18)-N,N-二甲基-N-苄基氯化铵(50%,在水中)及44g根据对比实施例6制备的粘结剂在开始时进料,并加热至50℃。然后,在搅拌下将294g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入157g完全不含离子的水。混合物加热至90℃,并进一步蒸馏,直到得到量为500g的馏出液。将产物冷却至室温,并采用75μm的聚酰胺滤布过滤。含粘结剂的水溶胶是乳色的稀液体,其平均粒度为110nm。
实施例3:
将1182g完全不含离子的水和11.3g的4-C10-13-仲烷基苯磺酸在开始时进料,并加热至50℃。然后,在搅拌下将228g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入770g完全不含离子的水。将混合物加热至90℃,并进一步蒸馏,直到得到量为350g的馏出液。将水溶胶冷却至80℃,并用氨水溶液(25%)调节至pH7。其后,将44g根据对比实施例6制备的粘结剂以1克/分钟的速度搅拌进入。将产物冷却至室温,并采用75μm的聚酰胺滤布过滤。含粘结剂水溶胶为乳色的稀液体,其平均粒度为90nm。
实施例4:
将1182g完全不含离子的水、11.3g 4-C10-13-仲烷基苯磺酸和44g根据对比实施例6制备的粘结剂在开始时进料,并加热至50℃。然后,在搅拌下将228g三甲氧基甲基硅烷以30克/小时的速度计量进料。在加入约一半的硅烷后,施以300hPa的真空,以除去释放的甲醇。硅烷添加后,设置到大气压力,并加入770g完全不含离子的水。混合物加热至90℃,并进一步蒸馏,直到得到量为350g的馏出液。将水溶胶冷却至80℃,并用氨水溶液(25%)调节至pH7。然后将产物冷却至室温,并采用75μm的聚酰胺滤布过滤。该含粘结剂水溶胶为乳色的稀液体,其平均粒度为86nm。
实施例5和对比试验:
a)在聚酰胺片上粘附性和成膜性能的评价:
使用箱形断面的刮刀涂布机,将实施例1-4和对比产品1、2、4、5和6的产品涂覆至聚酰胺片(PA6,厚度为80μm),形成50μm厚的层。薄膜在干燥箱中150℃下干燥并固化10分钟。冷却后,通过用手有力地摩擦所述层来量化薄膜的粘附性和强度。薄膜评价的结果归纳在下表中。
b)在聚酰胺地毯上防干污物性的评价:
将尺寸为15×30cm的聚酰胺地毯片在各种情形下浸渍到600毫升的液体中,液体由50克/升的实施例1-4和对比产品1、2、4、5和6的分散体形成,然后在4巴的双辊式浸染机中挤压。湿涂层量(wet pickup)介于50-60%。随后,地毯片在150℃下干燥箱中干燥15分钟,并储存在23℃、62%的相对湿度下的调理箱中至少24小时。与6.5g的含烟煤的试验污物(源自wfk Testgewebe GmbH的wfk地毯颜料污物)一起,一次一个地将地毯片放置在尺寸为30×40cm的塑料袋中,并彻底摇动90秒钟。其后,从袋中取出地毯试样,并用手将未粘结(unattached)的污物部分在实验室通风橱中抖落三次。然后使用Minolta的CR-200颜色测量仪测量地毯片变黑的程度。每个试样在不同的位置检验9次。测量采用设定至Yxy坐标的CIED65标准光源和颜色系统进行。所用的变黑的量度是以%计的Y值。Y值越高,试样的颜色就越浅。为了对比,将未处理的地毯试验沾污并测量其变黑的情形。防污性结果归纳在下表中。
表1:
表中的结果显示,只有采用本发明的实施例1-4的分散体,才能得到在地毯上均匀耐磨的薄膜及良好的防污性。
只有本发明(含硅烷的聚乙烯醇)的粘结剂,如按照对比产品6的,以及如根据对比产品4的含纳米颗粒的聚乙烯醇产生的是均匀耐磨的薄膜,但是其不具有防污性。当使用不含粘结剂的甲基倍半硅氧烷水溶胶,如根据对比产品1和2的时,得到的结果不是均匀耐磨的薄膜,而是脆的结晶涂层,其容易从聚酰胺片上擦掉。
相似地,根据对比产品5的具有含碳氟化合物的粘结剂的甲基倍半硅氧烷水溶胶得到了不均匀的容易擦掉的涂层,以及不是均匀耐磨的薄膜。
使用聚乙烯醇作为粘结剂,如根据对比产品3来代替根据本发明的含硅烷的聚乙烯醇不会导致稳定的分散体,而是形成坚硬的凝胶,其不能使用。
Claims (9)
1.含粘结剂的胶态的水分散体(B),其包含:
(a)由以下通式的单元构成的有机聚硅氧烷:
R1 xSi(OR2)yO(4-x-y)/2 (I)
其中x是0、1、2或3,且y是0、1或2,
条件是x+y的总和≤3,
R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,该一价烃基可以任选包括水惰性的取代基,
R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,该烃基可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3、-COC2H5或-CH2CH2OH,
(b)水溶性的或自分散性的含硅烷的聚乙烯醇和/或聚乙烯基酯和/或共聚物,条件是多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷,
(c)任选存在的表面活性化合物,例如乳化剂,和
(d)水。
2.权利要求1的含粘结剂的胶态的水分散体(B),其特征在于,它们包含:
(e)可与水混溶的添加物。
3.权利要求1或2的含粘结剂的胶态的水分散体(B),其特征在于,所述含硅烷的聚乙烯醇(b)包括:由乙烯基醇聚合物与烯键式不饱和的含硅烷单体的自由基接枝聚合而制备的含硅烷的聚乙烯醇。
4.权利要求1或2的含粘结剂的胶态的水分散体(B),其特征在于,所述含硅烷的聚乙烯醇(b)包括:通过乙烯基酯与烯键式不饱和的含硅烷单体和任选存在的其它可共聚合的共聚单体的自由基聚合,以及所得聚合物的皂化而制备的含硅烷的聚乙烯醇。
5.一种制备含粘结剂的胶态的水分散体(B)的方法,其是通过混合胶态的有机聚硅氧烷水分散体(A)与(b)水溶性或自分散性的含硅烷的聚乙烯醇和/或聚乙酸乙烯酯和/或其共聚物而制备的,其中(A)包含:
(a)由下式的单元所构成的有机聚硅氧烷:
R1 xSi(OR2)yO(4-x-y)/2 (I)
其中x是0、1、2或3,且y是0、1或2,
条件是x+y的总和≤3,
R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,该一价烃基可以任选包括水惰性的取代基,
R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,该烃基可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3、-COC2H5或-CH2CH2OH,
(c)任选存在的表面活性化合物,例如乳化剂,和
(d)水,
条件是,多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷。
6.一种采用含粘结剂的胶态的水分散体(B)处理纤维型和片型基材的方法,该水分散体(B)包含:
(a)由以下通式的单元构成的有机聚硅氧烷:
R1 xSi(OR2)yO(4-x-y)/2 (I)
其中x是0、1、2或3,且y是0、1或2,
条件是x+y的总和≤3,
R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,该一价烃基可以任选包括水惰性的取代基,
R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,该烃基可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3、-COC2H5或-CH2CH2OH,
(b)水溶性的或自分散性的含硅烷的聚乙烯醇和/或聚乙烯基酯和/或共聚物,条件是多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷,
(c)任选存在的表面活性化合物,例如乳化剂,
(d)水。
7.权利要求6的方法,其特征在于,含粘结剂的胶态的水分散体(B)是通过混合胶态的有机聚硅氧烷水分散体(A)与(b)水溶性或自分散性的含硅烷的聚乙烯醇和/或聚乙酸乙烯酯和/或其共聚物而制备的,其中(A)包含:
(a)由下式的单元所构成的有机聚硅氧烷:
R1 xSi(OR2)yO(4-x-y)/2 (I)
其中x是0、1、2或3,且y是0、1或2,
条件是x+y的总和≤3,
R1在各种情形下相同或不同,并且表示每个基具有1-18个碳原子的SiC-结合的一价烃基,该一价烃基可以任选包括水惰性的取代基,
R2在各种情形下可以相同或不同,并且表示氢原子或每个基具有1-18个碳原子的烃基,该烃基可以插入一个或多个相互分开的氧原子,或表示下式的基:-COCH3,-COC2H5或-CH2CH2OH,
(c)任选存在的表面活性化合物,例如乳化剂,和
(d)水,
条件是,多于50摩尔%的完全或部分皂化的乙烯基酯单元存在,其中至少一种单体单元含有连接的硅烷。
8.权利要求6或7的方法,其特征在于,所用的基材是织物地板覆盖物,优选地毯和地毯地板。
9.权利要求6、7或8的方法,其特征在于,将权利要求6的或根据权利要求7制备的含粘结剂的胶态的水分散体(B)涂敷至所述基材,并使其干燥。
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DE102008000585.1 | 2008-03-10 | ||
PCT/EP2009/052480 WO2009112394A1 (de) | 2008-03-10 | 2009-03-03 | Binderhaltige kolloidale wässrige organopolysiloxandispersionen und deren verwendung |
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US20110009553A1 (en) | 2011-01-13 |
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CN101970544B (zh) | 2013-01-02 |
WO2009112394A1 (de) | 2009-09-17 |
EP2252650B1 (de) | 2011-12-28 |
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