CN106536663B - 用于地毯涂层组合物的具有高填料相容性的水性聚乙烯醇稳定的乙酸乙烯酯-乙烯-共聚物分散体 - Google Patents
用于地毯涂层组合物的具有高填料相容性的水性聚乙烯醇稳定的乙酸乙烯酯-乙烯-共聚物分散体 Download PDFInfo
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- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
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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
本发明涉及用于地毯涂层组合物的水性乙酸乙烯酯‑乙烯共聚物分散体，其是通过乙酸乙烯酯和乙烯以及可选的其它烯属不饱和共聚单体，在水性介质中的自由基引发乳液聚合获得的，其特征在于，为了稳定所述分散体，基于共聚单体的总重量，含有5至10wt％的一种或多种部分皂化的和低分子量的聚乙烯醇，该部分皂化的和低分子量的聚乙烯醇具有80至95mol％的水解度以及在4％的水性溶液中为1至5mPas的粘度(在20℃下，根据DIN 53015
Description
技术领域
本发明涉及具有高填料相容性的聚乙烯醇稳定的水性乙酸乙烯酯-乙烯共聚物分散体(aqueous vinyl acetate-ethylene dispersion)，并且还涉及含有这种高填料相容性的乙酸乙烯酯-乙烯共聚物分散体的地毯涂层组合物用于固结地毯，并且还涉及用这种高填料相容性的乙酸乙烯酯-乙烯共聚物分散体涂布的地毯。
背景技术
地毯，例如连续片材产品或方块地毯(小方地毯，carpet tile)，通过由簇绒(tufts)，例如以环的形式插入到编织或非编织的第一底布(primary backing)中形成地毯绒面(carpet pile)制造。在簇绒地毯中，片状第一底布附着环，但较松散。针刺毡地毯(needlefelt carpet)是通过针刺簇绒(needling the tufts)制成的。在编织地毯中，簇绒与第一底布(主衬里，primary backing)交织。
为了改善地毯绒面与片状第一底布的连接，将粘合剂施加到第一底布的背面。填充有填料，例如白垩(chalk)的水性类型的聚合物分散体可以含有另外的添加剂，例如增稠剂，并且通常预涂布为泡沫，或者处于未发泡状态。
特别地为了改善地毯的尺寸稳定性，地毯设置有另外的第二底布(次级衬里，secondary backing)。第二底布通常包括处于制造的纤维形式，例如聚丙烯的织造织物，或者处于天然纤维形式，例如黄麻中的织造织物。通过进一步施加粘合剂将第二底布连接到预涂敷的地毯上。再次，填充有填料，例如白垩的水性类型的聚合物分散体可以含有另外的添加剂，例如增稠剂，并且通常以泡沫或未发泡状态施用以形成次级涂层(secondarycoating)。
WO 90/00967A1描述了在地毯制造中使用以下各项的水性分散体代替PVC增塑溶胶作为粘合剂：乙酸乙烯酯-乙烯共聚物、或苯乙烯-丁二烯共聚物、或苯乙烯-丙烯酸酯共聚物。
美国专利US 3,779,799描述了用粘合剂组合物预涂布的簇绒地毯，其中粘合剂是乙酸乙烯酯-乙烯共聚物分散体(VAE共聚物分散体)、或聚乙烯分散体、或羧化苯乙烯-丁二烯共聚物的分散体。
美国专利US 5,026,765描述了包含乙酸乙烯酯-乙烯共聚物分散体的地毯涂层组合物，其中共聚物进一步含有单体单元，该单体单元的均聚物的Tg为至少50℃。
英国专利GB 1,298,155描述了地毯涂层组合物，其包括基于以下各项的水性混合物的可交联粘合剂：乙酸乙烯酯-乙烯共聚物、聚乙烯醇(PVOH)和乙二醛。
WO 2010/089142A1公开了在地毯制造中用作粘合剂的乙酸乙烯酯-乙烯共聚物分散体。该共聚物仅含有1至4wt％的乙烯，并且仅是乳化剂稳定的，但是如果需要的话，可以配合使用少量的保护胶体用于稳定化。
为了改善对聚乙烯醇缩丁醛片材(作为第二底布)的粘附性，WO2006/007157A1提出了使用乙酸乙烯酯-乙烯共聚物，其进一步包含1至10wt％的共聚单体单元，该共聚单体单元含有官能团，如羧基、酰胺、N-羟甲基或羟烷基基团。该共聚物通过使用乳化剂和0.05至4wt％的保护胶体的混合物来制备。
美国专利6,359,076提出通过使用可交联的乙酸乙烯酯-乙烯共聚物改善地毯涂层的耐水性，所述共聚物包括与交联剂结合的OH-官能单体单元。
WO 2011/139267 A1和WO 2011/140065 A2提出通过避免利用保护胶体的稳定化，而仅通过乳化剂的稳定化，并且共聚官能性可交联共聚单体，如硅烷官能或多官能共聚单体，来提高基于乙酸乙烯酯-乙烯共聚物的地毯涂层的质量。
WO 2012/020319 A2或WO 2012/020321 A2公开了因低可燃性或优良的可洗性而著名的地毯。所使用的粘合剂是乙酸乙烯酯-乙烯共聚物分散体，其具有平均粒径dw为50-500nm，通过乳化剂稳定化制备，但是如有必要的话，可以另外地使用最高3％的保护胶体作为共稳定剂。
WO 2013/093547A2涉及具有优化的组合物的地毯粘合剂用于具有炭黑作为填料的制剂。该粘合剂包含利用乳化剂和纤维素醚稳定的乙酸乙烯酯-乙烯共聚物分散体。
WO 2013/123210A1涉及通过使用由乙酸乙烯酯-乙烯共聚物分散体，以及由苯乙烯-丁二烯共聚物分散体形成的粘合剂混合物制造的地毯。改进两种不同聚合物分散体的相容性的建议包括在VAE分散体中避免聚乙烯醇，并且在粘合剂混合物的制备中，至多使用基于共聚单体至多1.5wt％的聚乙烯醇的保护胶体。
WO 2014/031579 A2涉及地毯涂层组合物，其通过粘合剂可以包括，尤其是乳化剂稳定的VAE分散体，并且如果必要可以额外含有至多1.5wt％的聚乙烯醇作为共稳定剂。将该分散体与α-烯烃-羧酸共聚物和交联剂共混。
WO 99/10396A1提出通过在由大于3wt％(优选4至5wt％)的低分子量聚乙烯醇和1至4wt％具有限定HLB的非离子乳化剂形成的稳定剂混合物的存在下制备VAE分散体，改善具有至少65wt％高固体含量(solids content)的VAE分散体的流变性。
WO 2013/001379 A2描述了聚乙烯醇稳定的VAE分散体。为了优化它们的粘度，所用的稳定化聚乙烯醇包含0.5至3wt％完全水解的聚乙烯醇和1.5至4wt％部分水解的聚乙烯醇。
美国专利US 4,921,898涉及基于乙酸乙烯酯-乙烯共聚物分散体的水性粘合剂组合物(adhesive composition)，所述分散体在2至4wt％的低分子量聚乙烯醇与2至4wt％乳化剂的稳定剂组合的存在下制备。所述粘合剂组合物值得注意的是快速凝固。
US 4,239,563描述了可用作粘合剂用于固结地毯的的水性乙酸乙烯酯-乙烯共聚物分散体。强调了挥发性有机化合物(VOC)相对于苯乙烯-丁二烯胶乳的较低排放。VAE分散体通过经由使用乳化剂和/或保护胶体(尤其是聚乙烯醇)的乳液聚合来制备。VAE共聚物基于总的共聚单体具有30至80wt％的高乙烯含量。
通过用于地毯粘合剂的现有技术，美国专利4,735,986描述了这样的组合物，其包含用5wt％聚乙烯醇稳定的乙酸乙烯酯-乙烯共聚物分散体，其中所述聚乙烯醇部分包含低粘度的部分水解的PVOH和中粘度的部分水解的PVOH的混合物。描述的缺点是填料相容性的水平不充分、缺乏与具有不同规格的白垩的相容性，以及与苯乙烯-丁二烯共聚物分散体的相容性低。认为在部分水解的PVOH、完全水解的PVOH和非离子聚烷氧基化乳化剂的稳定剂混合物的存在下聚合时，特性概况(性能特征，property profile)得到了改善。
至今用作地毯涂层组合物中的粘合剂的单独的聚乙烯醇稳定的乙酸乙烯酯-乙烯共聚物分散体的缺点是，它们在高度填充的制剂中的填充剂相容性(例如，与白垩)不充分。事实上，乳化剂在聚合或随后的乳化剂混合过程中的共同使用改善了水性乙酸乙烯酯-乙烯共聚物分散体的填料相容性，但是乳化剂的混合物也降低了以此获得的涂层的机械特性。
因此，本发明解决的问题是提供聚乙烯醇稳定的水性乙酸乙烯酯-乙烯共聚物分散体，其在用作地毯涂层组合物中的粘合剂时，即使使用大量的填料(基于VAE共聚物，高达1400wt％的填料，干/干)也可进行加工，并且无论是用在预涂层还是用于次级涂层中都会产生高的机械强度。
发明内容
本发明提供了用于地毯涂层组合物的水性乙酸乙烯酯-乙烯共聚物分散体，其通过在水性介质中，经由乙烯基乙酸酯和乙烯以及可选的另外的烯属不饱和共聚单体的，自由基引发的乳液聚合而获得，其特征在于所述分散体包含稳定体系，所述稳定体系包含基于总的共聚单体的5至10wt％的一种或多种部分水解的和低分子量的聚乙烯醇，所述聚乙烯酸具有水解度为80至95mol％，以及在4％水性溶液(aqueous solution)中的粘度为1至5mPas(DIN 53015方法，在20℃)。
这种水性乙酸乙烯酯-乙烯共聚物分散体值得注意的是其高填料相容性。高填料相容性应理解为是指这些水性乙酸乙烯酯-乙烯共聚物分散体提供这样的地毯涂层组合物，其组合了以下各项：基于VAE共聚物为600wt％至1400wt％填料的填料水平(干/干)、和在混合增稠剂之前为75至85wt％的固体含量，其中Brookfield RV粘度≤3000mPas(使用Brookfield RV测量仪器，使用转子4，20rpm，在25℃下测量)。
当在混合增稠剂之前的地毯涂层组合物的粘度较高时，填料的掺入时间在工业规模上不可接受地长，并且存在能够破坏地毯织物的未分散的填料块的风险。
乙酸乙烯酯通常以65至99wt％，优选80至95wt％的量共聚，所有组分均基于总单体。乙烯通常以1至30wt％，优选5至20wt％的量共聚，所有组分均基于总单体。另外的最高10wt％，优选0.1至10wt％的是可选的可共聚的另外的共聚单体，所有组分均基于总单体。在每种情况下，共聚单体的wt％加起来为100wt％。
合适的另外的共聚单体是来自羧酸部分中具有3至12个碳原子的乙烯基酯基团的共聚单体，如丙烯酸乙烯酯、月桂酸乙烯酯、具有9至11个碳原子的α-支链羧酸的乙烯基酯(如VeoVaR9、VeoVaR10、VeoVaR11)。还合适的是具有1至15个碳原子的支化或非支化醇的甲基丙烯酸酯或丙烯酸酯，如丙烯酸甲酯、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、甲基丙烯酸正丁酯、丙烯酸2-乙基己酯、丙烯酸降冰片基酯。乙烯基卤化物，如氯乙烯也是合适的。
合适的另外的共聚单体还包括烯属不饱和单羧酸和二羧酸，优选丙烯酸、甲基丙烯酸、富马酸和马来酸；烯属不饱和羧酰胺和腈，优选丙烯酰胺和丙烯腈；富马酸和马来酸的单酯和二酯，如二乙酯和二异丙酯，以及马来酸酐，烯属不饱和磺酸和/或盐，优选乙烯基磺酸、2-丙烯酰胺基-2-甲基丙磺酸。另外的实例是预交联共聚单体，如聚烯属不饱和单体，实例为己二酸二乙烯酯、马来酸二烯丙酯、甲基丙烯酸烯丙酯或氰脲酸三烯丙酯，或后交联单体，实例为丙烯酰胺乙醇酸(AGA)、甲基丙烯酰胺乙醇酸甲基酯(MAGME)、N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺(NMMA)、N-羟甲基烯丙基氨基甲酸酯，烷基醚，如以下各项的异丁氧基醚或酯类：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。
具有羟基或羧基的基团的单体也是合适的，实例为甲基丙烯酸和丙烯酸的羟烷基酯，例如丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、丙烯酸羟丁酯或甲基丙烯酸羟丁酯，以及1,3-二羰基化合物，如丙烯酸乙酰乙酰氧基乙酯、甲基丙烯酸乙酰乙酰氧基丙酯、甲基丙烯酸乙酰乙酰氧基乙酯、甲基丙烯酸乙酰乙酰氧基丁酯、甲基丙烯酸2,3-二(乙酰乙酰氧基)丙酯和乙酰乙酸烯丙酯。
合适的另外的共聚单体还包括环氧官能共聚单体，如甲基丙烯酸缩水甘油酯、丙烯酸缩水甘油酯、烯丙基缩水甘油醚、乙烯基缩水甘油醚。合适的另外的共聚单体的另外的实例是硅官能共聚单体，如丙烯酰氧基丙基三(烷氧基)硅烷和甲基丙烯酰氧基丙基三(烷氧基)硅烷、乙烯基三烷氧基硅烷和乙烯基甲基二烷氧基硅烷，优选地其中，烷基和/或烷氧基各自具有1或2个碳原子，实例为乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷。
通过乳液聚合法制备所述乙酸乙烯酯-乙烯共聚物分散体，其中聚合温度通常在40℃至120℃的范围内，优选在60℃至90℃的范围内，并且所使用的压力通常在5至100巴绝对压力范围内。聚合优选使用常规用于乳液聚合的氧化还原引发剂组合来引发。合适的氧化引发剂的实例是过氧二硫酸的钠、钾和铵盐，过氧化氢，叔丁基过氧化物，叔丁基过氧化氢，过氧二磷酸钾，过氧化新戊酸叔丁酯，氢过氧化枯烯，异丙基苯单过氧化物，偶氮二异丁腈。优选过氧二硫酸的钠盐、钾盐和铵盐以及过氧化氢。所列举的引发剂通常以基于总的单体的0.01至2.0wt％的量使用。合适的还原剂是碱金属和铵的亚硫酸盐和亚硫酸氢盐，实例为亚硫酸钠，亚磺酸的衍生物，如甲醛次硫酸锌或碱金属甲醛次硫酸盐，实例为羟基甲亚磺酸钠(Brüggolit)和(异)抗坏血酸。优选使用羟基甲烷亚磺酸钠和亚硫酸钠。基于总的单体，还原剂的量优选在0.015至3wt％的范围内。所列举的氧化剂，特别是过氧二硫酸的盐，也可单独作为热引发剂使用。
聚合在基于总的共聚单体为2至10wt％的一种或多种部分水解的和低分子量的聚乙烯醇的存在下进行，所述部分水解的和低分子量的聚乙烯醇具有水解度为80至95mol％以及在4％水性溶液的粘度为1至5mPas(在20℃I下，DIN 53015方法，)。优选使用均基于总的共聚单体为6至10wt％，更优选6至8wt％的一种或多种部分水解的和低分子量的聚乙烯醇。部分水解的和低分子量的聚乙烯醇的水解度优选在85至90mol％的范围内，更优选在87至89mol％的范围内。部分水解的和低分子量的聚乙烯醇在4％水性溶液中的粘度优选在2至4-5mPas的范围内(在20℃下DIN 53015方法)。所述聚乙烯醇是可商购的，并且它们可通过本领域技术人员已知的方法获得。
可选地，还可以使用部分水解的和高分子量的聚乙烯醇与部分水解的和低分子量的聚乙烯醇的混合物，该部分水解的高分子量的聚乙烯醇具有的水解度优选为80至95mol％以及在4％水性溶液中的粘度优选为8至40mPas(DIN 53015法，在20℃)。可选地，还可以的是完全水解的高分子量聚乙烯醇与部分水解的和低分子量的聚乙烯醇混合使用，该完全水解的高分子量聚乙烯醇具有的水解度优选为98至100mol％并且在4％水性溶液中的粘度优选为10至56mPas(DIN 53015法，在20℃)。所述部分水解的和高分子量的聚乙烯醇和/或所述完全水解的高分子量聚乙烯醇可以混合使用，均基于总的共聚单体，优选各自以0至2wt％的量使用。
可选地，在聚合中可以额外使用少量乳化剂，例如基于总的共聚单体为0.1至2.0wt％。优选地，在聚合期间不使用乳化剂，并且后续不混入任何乳化剂。
在聚合之前，聚乙烯醇部分被完全包括在初始进料(initial charge)中、或者在聚合过程中全部加入、或者部分被包括在初始进料中且部分加入。聚乙烯醇部分也可以部分地在聚合之前或期间混入，并且随后在聚合完成之后混入余量，需满足的条件是(subject to the provisio)在聚合之前或期间混入的比例基于总的共聚单体为至少2wt％，优选至少5wt％。
所述聚合可以间歇方法、半间歇方法或连续方法进行。所述的单体在起始时可全部装入、全部加入，或起始时可以部分装入，其余量在聚合开始后加入。添加进料可以是分开的(空间和时间)，或者可以在预乳化之后添加所有或部分待添加的组分。
聚合通常进行到单体(在聚合条件下为液体)的转化率≥95wt％，优选最高95至99wt％的转化率。随后将聚合混合物降至0.1至5.0巴绝对压力下，优选0.1至1.0巴绝对压力。
由此获得的水性乙酸乙烯酯-乙烯共聚物分散体的固体含量为30至75wt％，优选为50至65wt％。
本发明还提供用于固结地毯(例如，连续片材产品或方块地毯)的地毯涂层组合物，其包含根据本发明所述的聚乙烯醇稳定的水性乙酸乙烯酯-乙烯共聚物分散体和基于所述乙酸乙烯酯-乙烯共聚物为100至1400wt％的填料(固体/固体)。地毯涂层组合物的固体含量均基于地毯涂层组合物的总重量优选在72至83wt％的范围内，更优选在75至80wt％的范围内。值得注意的是，在混合增稠剂之前，该地毯涂层组合物的Brookfield RV粘度≤3000mPas(使用Brookfield RV测量仪器，使用转子4，20rpm，在25℃下测量)。
地毯涂层组合物含有填料以及水性乙酸乙烯酯-乙烯共聚物分散体。合适的填料是本领域技术人员已知的，实例是白垩、高岭土、滑石、萤石、飞灰、三水合铝。优选将白垩用作填料。地毯涂层组合物还可以含有增稠剂，如聚丙烯酸酯或纤维素醚。发泡助剂(Foamingauxiliary)可以混合用于泡沫应用。常规的添加剂还包括分散剂、润湿剂、颜料或杀生物剂。
地毯涂层组合物相对于每100重量份乙酸乙烯酯-乙烯共聚物含有100至1400重量份的填料(干/干)。这也称为填充水平为100％至1400％。制剂中填料的量可根据所需的涂层性质而变化。填料部分(填充水平)越高，机械特性越低。
预涂层优选使用具有300至1400％填充水平的制剂。对于住宅应用的预涂层，填充水平优选在600至1000％的范围内，对于商业应用(办公室、酒店、船舶)，填充水平优选为300至600％。
对于住宅应用，次级涂层优选使用具有275至600％填充水平的制剂，而对于商业应用(办公室、酒店、船舶)，优选200至275％的填充水平的制剂。
在用于生产地毯涂层组合物的可能程序中，首先将乙酸乙烯酯-乙烯共聚物分散体与水和分散剂一起加入，并将填料搅入。使用本发明的聚乙烯醇稳定的水性乙酸乙烯酯-乙烯共聚物分散体用于乙酸乙烯酯-乙烯共聚物分散体，提供了Brookfield RV粘度≤3000mPas(使用Brookfield RV测量仪器，使用转子4，20rpm，在25℃下测量)的组合物。随后，为了建立目标粘度，可以混合增稠剂。基于乙酸乙烯酯-乙烯共聚物分散体，0.1至3wt％的量通常足以用于该增稠剂。优选使用增稠剂来建立2000至10000mPas的Brookfield RV粘度(使用Brookfield RV测量仪器，使用转4，20rpm，在25℃下测量)。
本发明进一步提供涂布有本发明的地毯涂层组合物的地毯，其在预涂层和/或次级涂层中包含乙酸乙烯酯-乙烯共聚物分散体。
地毯涂层组合物可以用于制造簇绒地毯、纺织地毯或针刺毡地毯，对于这些地毯，可以在用于地毯制造的现有设备中，使用现有方法来利用涂层组合物。
具体实施方式
下面的实施例说明了本发明：
实施例1：(根据本发明)(高填料相容性的水性乙酸乙烯酯-乙烯共聚物分散体的制备)
首先，向压力反应器(容量：570升)中装填130kg 10wt％的水性聚乙烯醇溶液，该聚乙烯醇具有在4wt％溶液中的粘度为4mPas且水解度为88mol％。初始的填料另外包括224kg的乙酸乙烯酯和101.5kg的去离子水。使反应器达到21巴的压力和55℃的温度(对应于18.5kg的乙烯量)，并且开始以750g/h分别装入叔丁基过氧化氢(3wt％，在水中)和抗坏血酸(5wt％的，在水中)引发剂进料以使聚合开始。在反应开始时，从温度升高可以看出，通过放出的聚合热将反应温度升至90℃并将压力升至44巴。将引发剂进料各自减少至350g/h。反应开始后45分钟开始进一步进料：40kg/h的乙酸乙烯酯进料90分钟时长(对应于60kg的乙酸乙烯酯)和30kg/h的10wt％的水性聚乙烯醇溶液，进料120分钟时长相当于60kg的量)，该水性聚乙烯醇溶液具有在4wt％的溶液中的4mPas的粘度，以及水解度为88mol％。在44巴的目标压力下补充乙烯直到总乙烯量为34kg。
在单体进料完成时，将引发剂进料各自增加至1300g/h持续30分钟，在此期间压力降至20巴(时间点1)。随后，将批料冷却至65℃，并转移至大气压(低压)反应器中，并通过混入1kg叔丁基过氧化氢溶液(10wt％，在水中)和2kg抗坏血酸溶液(5wt％，在水中)，在700毫巴绝对压力下进行后聚合。
获得的分散体的固体含量为59wt％，粘度为1800mPas(Brookfield，20，23℃)，玻璃化转变温度Tg为15.0℃。该共聚物含有89wt％的乙酸乙烯酯单体单元和11wt％的乙烯单体单元。基于共聚单体，聚乙烯醇含量为6wt％。
实施例2：(根据本发明)(类似于实施例1，不同之处在于，在聚合过程中仅使用3wt％的聚乙烯醇，其余的3wt％在聚合之后混入到聚合物分散体中)
重复实施例1，不同之处在于起始时仅装填65kg聚乙烯醇溶液而不是130kg，并且仅加入30kg聚乙烯醇溶液而不是60kg。在聚合完成时，随后向乙酸乙烯酯-乙烯共聚物分散体中混入95kg聚乙烯醇溶液。
比较例3：(非根据本发明)(仅使用2.4wt％低粘度的部分水解的聚乙烯醇和1.8wt％高粘度的部分水解的聚乙烯醇进行稳定化)
乙酸乙烯酯-乙烯共聚物分散体包含85wt％乙酸乙烯酯单元和15wt％乙烯单元，以及2.4wt％的具有粘度为4mPas且水解度为88mol％的聚乙烯醇和1.8wt％的具有粘度为26mPas且水解度为88mol％的聚乙烯醇的混合物，wt％均基于总的共聚单体。
比较例4：(非根据本发明)(仅使用3.2wt％低粘度的部分水解的聚乙烯醇和1.8wt％非离子乳化剂进行稳定化)
乙酸乙烯酯-乙烯共聚物分散体包含85wt％乙酸乙烯酯单元和15wt％乙烯单元，以及3.2wt％的具有粘度为5mPas且水解度为88mol％的聚乙烯醇和1.8wt％的脂肪醇乙氧基化物乳化剂的混合物，wt％均基于总的共聚单体。
比较实施例5：(非根据本发明)(乳化剂稳定的乙酸乙烯酯-乙烯共聚物分散体)
乙酸乙烯酯-乙烯共聚物分散体包含85wt％乙酸乙烯酯单元和10wt％乙烯单元、1wt％丙烯酸、2wt％甲基丙烯酸缩水甘油酯(GMA)以及2wt％脂肪醇乙氧基化物和1wt％阴离子磺基琥珀酸盐和烷基苯磺酸盐乳化剂的混合物，所述wt％均以总的共聚单体为基础。
地毯涂层组合物的制备：
将实施例1和2以及比较实施例3至5的分散体各自用于制备以下制剂：
具有1000％填充水平和78.5wt％的固体含量的预涂层：
100重量份干燥的根据实施例1至2和比较实施例3至5的乙酸乙烯酯-乙烯共聚物分散体，
1000重量份干燥的白垩(Carbocia 80,Carbocia)，
2.0重量份干燥的分散剂(Sokalan CP 10,BASF)，
0.6重量份干燥的发泡助剂(月桂基硫酸钠,Disponil SDS,BASF)，
约200重量份水以建立78.5wt％的固体含量。
具有400wt％填充水平和79.5wt％固体含量的次级涂层：
100重量份干燥的根据实施例1至2和比较实施例3至5的乙酸乙烯酯-乙烯共聚物分散体，
400重量份干燥的白垩(Carbocia 80,Carbocia)，
0.8重量份干燥的分散剂(Sokalan CP 10,BASF)，
0.5重量份干燥的发泡助剂(月桂基硫酸钠,Disponil SDS,BASF)，
约30重量份水以建立79.5wt％的固体含量。
水和VAE共聚物分散体，以及分散剂各自在初始时装填。随后在搅拌下混入填料，然后加入发泡助剂。
然后测量各制剂的Brookfield粘度(使用Brookfield RV测量仪器，使用转子4，20rpm，在25℃下测量)。
然后使用增稠剂(Matco TR 10丙烯酸酯增稠剂，Matco)或通过水的混合物，建立最终粘度6000至7000mPas(使用Brookfield RV测量仪器，使用转子4，20rpm，在25℃下测量)。
在混合增稠剂之前的Brookfield RV粘度是填料相容性的量度。所测量的值列于表1中。
表1：在增稠剂混合之前的Brookfield粘度，单位mPas(RV/20Rpm)
在表中可以清楚的看到，本发明的聚乙烯醇稳定的乙酸乙烯酯-乙烯共聚物分散体(实施例1和2)可用于生产，在混入增稠剂之前，具有<3000m Pas粘度且固体含量分别为78.5％和79.5％的预涂层和次级涂层。
不可能的是比较实施例3的聚乙烯醇稳定的分散体，其并非根据本发明。
并不是根据本发明所述的乳化剂-共稳定分散体(比较实施例4)或仅乳化剂-稳定的分散体(比较实施例5)各自产生在混合增稠剂之前粘度<3000mPas的预涂层。
测试地毯的簇绒拔出力和耐分层性(delamination resistance)：
地毯涂层组合物的制备：
对于预涂层和次级涂层，通过在实验室规模上使用具有450％填充水平的一种制剂来评价机械特性(实验室基准测试)。
实际上，在工业实践中采用的是较高的预涂层填充水平和较低的添加量(add-ons)，但是在本实验室基准测试中获得的簇绒结合强度和分层强度值的确允许所使用的聚合物分散体之间的相对比较。
实施例1和2以及比较实施例3至5的分散体各自被用于生产具有以下配方的以下制剂：
具有450wt％填充水平和81.5wt％的固体含量的实验室基准制剂：
100重量份干燥的根据实施例1至2和比较实施例3至5的乙酸乙烯酯-乙烯共聚物分散体，
450重量份干燥的白垩(Carbocia 80,Carbocia)，
0.8重量份干燥的分散剂(Sokalan CP 10,BASF)，
0.5重量份干燥的发泡助剂(月桂基硫酸钠,Disponil SDS,BASF)，
约20重量份水以建立81.5wt％的固体含量。
首先装填水和VAE共聚物分散体和分散剂。随后在搅拌下将填料混入，然后加入发泡助剂。
然后，使用增稠剂(Matco TR 10丙烯酸酯增稠剂,Matco)以建立6000至7000mPas最终粘度(使用Brookfield RV测量仪器，使用转子4，20rpm，在25℃下测量)。在比较实施例3中，通过使用水稀释来建立粘度，未使用丙烯酸酯增稠剂。
实验室地毯样品的生产：
在实验室中，使用厨房器具将用于预涂层和次级涂层的制剂起泡(通常约3分钟)以产生具有密度为950至1015g/L的泡沫。在每种情况下，用148g发泡制剂均匀地预涂布来自Edel的尺寸为38cm×33cm的Helsinki式原坯圈式(greige loop)方块簇绒地毯(100％聚酰胺；550g/m2纱线重量(pile weight))。
随后在每种情况下施用60g起泡制剂作为次级涂层。将织物底布(Action Bac聚丙烯编织物)放在顶部，用1.6kg重辊在无压力下处理两次，并在烘箱中在130℃干燥20分钟。
在比较实施例3中，由于较低的固体含量而成比例地施用更多的制剂，以便在干燥后获得相同的添加量(add-on)。
尽管次级涂层的添加量对应于工业上常规的量，但是预涂层的添加量高出两倍以上，以在实验室中使制剂在地毯上均匀分布。
簇绒拔出力的测量：
簇绒拔出力的测试根据ISO 4919标准使用Zwick测试仪在23℃和50％相对湿度下进行。将实验室地毯样品各自夹在测量装置的基部的顶部部件，并将针穿入地毯毛圈。在10个不同的地毯毛圈上确定将毛圈拉出地毯所需的力，并且将测量结果的平均值报告为簇绒拔出力。
以牛顿[N]为单位的簇绒拔出力是由预涂层提供的绒促联结(tuft bind)和地毯表面的耐磨性质的量度。结果列于表2中。
耐分层性的测定：
耐分层性根据DIN EN ISO 11857使用Zwick测试仪在23℃和50％相对湿度下测定。将每个实验室地毯样本的三个样品在机器方向上切成5cm宽和20cm长，并在窄边上用手在5cm的长度上分层。将初始分层的样品夹在Zwick测试器中，并以300mm/min的速率将第二底布与地毯分离。
确定峰的平均值，忽略峰的前25％和最后的25％，并报告总平均值作为以牛顿[N]为单位的耐分层性。结果列于表2中。
表2：
| 分散体 | 簇绒拔出力[N] | 耐分层性[N] |
| 实施例1 | 42.5 | 55.2 |
| 实施例2 | 38.9 | 38.3 |
| 比较实施例3 | 43.1 | 52.0 |
| 比较实施例4 | 38.0 | 33.8 |
| 比较实施例5 | 38.6 | 30.2 |
结果总结和说明：
仅聚乙烯醇稳定的乙酸乙烯酯-乙烯分散体(比较实施例3)通常表现出较高的机械强度，特别是较高的耐分层性(见表2)，但填料相容性不充分(参见表1)。
实施例1的聚乙烯醇稳定的乙酸乙烯酯-乙烯共聚物分散体不仅表现出高机械特性，特别是高耐分层性(表2)，而且还表现出良好的填料相容性(表1)。
随后的PVOH的混合(实施例2)同样提供了较高的填料相容性和良好的机械特性。
另外的乳化剂稳定的分散体(比较实施例4)或仅乳化剂稳定的分散体(比较实施例5)虽然表现出良好的填料相容性(表1)，但表现出差的机械特性，特别是较低的干强度(表2)。
Claims (9)
1.一种用于固结地毯的地毯涂层组合物，其包含水性乙酸乙烯酯-乙烯共聚物分散体并且包含基于100wt％的乙酸乙烯酯-乙烯共聚物的100至1400wt％的固体/固体的填料，所述分散体是通过乙酸乙烯酯和乙烯以及可选的另外的烯属不饱和共聚单体在水性介质中的自由基引发的乳液聚合获得的，其特征在于，
所述分散体包含一种稳定体系，基于总的共聚单体，所述稳定体系包含5至10wt％的一种或多种部分水解的且具有低分子量的聚乙烯醇，该部分水解的且具有低分子量的聚乙烯醇具有为80至95mol％的水解度，和在4％水性溶液中根据DIN 53015方法，在20℃测得的为1至5mPa·s的粘度。
2.根据权利要求1所述的用于固结地毯的地毯涂层组合物，其特征在于，由65至99wt％的乙酸乙烯酯和由1至30wt％的乙烯，以及可选的至多10wt％的另外的共聚单体进行共聚。
3.根据权利要求1或2所述的用于固结地毯的地毯涂层组合物，其特征在于，基于总的共聚单体，部分水解的且具有高分子量的聚乙烯醇以0至2wt％的量与所述部分水解的且具有低分子量的聚乙烯醇混合使用，所述部分水解的且具有高分子量的聚乙烯醇具有80至95mol％的水解度，以及在4％水性溶液中根据DIN 53015法，在20℃测得的8至40mPa·s的粘度。
4.根据权利要求1或2所述的用于固结地毯的地毯涂层组合物，其特征在于，基于总的共聚单体，完全水解的且具有高分子量的聚乙烯醇以0至2wt％的量与所述部分水解的且具有低分子量的聚乙烯醇混合使用，所述完全水解的且具有高分子量的聚乙烯醇具有98至100mol％的水解度，以及在4％水性溶液中根据DIN 53015法，在20℃测得的10至56mPa·s的粘度。
5.根据权利要求1或2所述的用于固结地毯的地毯涂层组合物，其特征在于，在所述乳液聚合期间不使用乳化剂，后续也不混合任何乳化剂。
6.根据权利要求1或2所述的用于固结地毯的地毯涂层组合物，其特征在于，所述聚乙烯醇部分在聚合之前完全包括在初始进料中、或在聚合过程中全部加入、或部分包括在初始进料中且部分加入，或者所述聚乙烯醇部分在聚合之前或期间被部分地混入，并且随后余量在聚合完成之后混入，需满足的条件是在后者情况中，在聚合之前或期间混入的比例是基于总的共聚单体的至少2wt％。
7.根据权利要求6所述的用于固结地毯的地毯涂层组合物，其中所述比例是至少5wt％。
8.根据权利要求1或2所述的用于固结地毯的地毯涂层组合物，基于所述地毯涂层组合物的总重量，具有72至83wt％的固体含量。
9.一种在预涂层和/或次级涂层中涂布了根据权利要求1或2或3或4或5或6或7或8所述的地毯涂层组合物的地毯。
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| EP2644769A1 (en) * | 2010-05-03 | 2013-10-02 | Celanese International Corporation | Carpets with Surfactant-Stabilised Emulsion Polymer Coating Binder |
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- 2015-07-01 EP EP15735899.5A patent/EP3171737B1/de active Active
- 2015-07-01 CN CN201580039135.1A patent/CN106536663B/zh active Active
- 2015-07-01 WO PCT/EP2015/064962 patent/WO2016012209A1/de active Application Filing
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| EP1174447A1 (de) * | 2000-07-21 | 2002-01-23 | Wacker Polymer Systems GmbH & Co. KG | Verfahren zur Herstellung von zweiphasigen Polymerisaten in Form deren wässrigen Polymerdispersionen und in Wasser redispergierbaren Polymerpulver |
| CN1358778A (zh) * | 2000-12-14 | 2002-07-17 | 瓦克聚合系统两合公司 | 挥发性成分减少的聚合物的制备方法 |
| EP2644769A1 (en) * | 2010-05-03 | 2013-10-02 | Celanese International Corporation | Carpets with Surfactant-Stabilised Emulsion Polymer Coating Binder |
| CN103119215A (zh) * | 2010-08-12 | 2013-05-22 | 塞拉尼斯乳液有限公司 | 具有由乙烯酯/乙烯共聚物分散体形成的涂布层的可洗地毯产品 |
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| US11866576B2 (en) | 2019-03-27 | 2024-01-09 | Wacker Chemie Ag | Formaldehyde-free binder composition |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2016012209A1 (de) | 2016-01-28 |
| US20170253759A1 (en) | 2017-09-07 |
| EP3171737A1 (de) | 2017-05-31 |
| US10457827B2 (en) | 2019-10-29 |
| DE102014214472A1 (de) | 2016-01-28 |
| EP3171737B1 (de) | 2019-10-02 |
| CN106536663A (zh) | 2017-03-22 |
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