CN108291361A - 用于地毯涂层组合物的粘合剂 - Google Patents
用于地毯涂层组合物的粘合剂 Download PDFInfo
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- CN108291361A CN108291361A CN201680067463.7A CN201680067463A CN108291361A CN 108291361 A CN108291361 A CN 108291361A CN 201680067463 A CN201680067463 A CN 201680067463A CN 108291361 A CN108291361 A CN 108291361A
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- Prior art keywords
- carpet
- polyethyleneimine
- coating composition
- dry
- vinyl
- Prior art date
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- 239000008199 coating composition Substances 0.000 title claims abstract description 52
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Abstract
本发明的目标是乙酸乙烯酯‑乙烯共聚物的水分散体和至少一种聚乙烯亚胺在用于生产地毯的地毯涂层组合物中作为粘合剂的用途。
Description
本发明涉及用于地毯涂层组合物的粘合剂、由其可获得的地毯涂层组合物和用此类地毯涂层组合物涂覆的地毯。
典型的市售地毯,作为例如连续压片产品或拼块地毯(carpet tile),是通过从以例如毛圈(loop)形式机械地插入织造或铺设的主背衬中的簇绒(tuft)形成地毯绒头(pile)而制造的。在簇绒地毯中,片状主背衬保持毛圈,但较松散,因此用含粘合剂的配制物(地毯涂层组合物)处理毛圈以使未完成的地毯稳定。所述含粘合剂的配制物以起泡或未起泡的形式被预涂覆至主背衬的背面上,并且除了作为粘合剂的含水聚合物分散体之外,通常进一步包含填料,如例如白垩,以及任选地另外的辅助剂,如增稠剂、分散助剂或起泡助剂。
为了改善它们的尺寸稳定性,由此获得的地毯产品可设有另外的辅助背衬。辅助背衬(secondary backing)通常包括由制造纤维或者天然纤维如黄麻制成的织造织物,所述制造纤维例如为聚丙烯、聚酰胺或聚酯。通过再次施加粘合剂将辅助背衬附着至如此预涂覆(as-precoated)的地毯上,所述粘合剂的配制物可与地毯预涂覆的涂层组合物的配制物类似。同样,在该第二涂层中,配制成泡沫或呈未起泡状态的前述含水聚合物分散体可与填料和另外的辅助剂(如增稠剂、分散助剂或起泡助剂)一起施加以形成辅助涂层。
乙酸乙烯酯-乙烯共聚物,无论是对于纯保护胶体稳定化,对于纯乳化剂稳定化,还是对于混合稳定化来说,都越来越多地用作地毯涂层组合物中的粘合剂。这些共聚物具有不同的玻璃化转变温度和因此在共聚物中不同的乙烯分数,以其在完全完成的地毯中的良好机械性质而值得关注。不仅簇绒拔出力,而且耐分层性,均可在干测试条件下与基于苯乙烯-丁二烯共聚物分散体的标准粘合剂相当地配制。然而,储水后的机械测试,作为地毯暴露于清洁和水分的模型测试,经常显示出比基于苯乙烯-丁二烯胶乳的地毯涂层组合物更低的值。
性能曲线中的坍塌度的起因可能在于涂层的孔隙率、所得孔径分布、粘合剂的亲水性、填料分布本身以及粘合剂相对于地毯构造的组分(辅助背衬上的绒头和涂层)的粘聚性和粘着性。在来源于地毯涂层组合物的泡沫应用的高孔隙率和宽孔径分布的情况下,涂层材料的毛细吸水性也很高,并且涂层的相关减弱导致粘聚降低,并因此导致机械载荷下的过早断裂或撕裂。可通过熟练地选择配制物组分和应用参数来降低或优化毛细吸水性。这不会改变储水下的粘着损失。较低的粘着特别表现为在测量抗分层性时机械强度的损失。
在US 6,359,076 B1中,利用辅助背衬涂层组合物获得具有改善的湿强度的地毯,所述辅助背衬涂层组合物基于具有OH-官能共聚单体单元的乙酸乙烯酯-乙烯共聚物的水分散体,所述OH-官能共聚单体单元与来自多官能氮丙啶、多官能异氰酸酯和多官能环氧化物的组的交联剂组合。
WO 2014/031579 A2提出了通过使用辅助背衬涂层组合物来改善地毯的湿强度,所述辅助背衬涂层组合物基于乙酸乙烯酯-乙烯共聚物分散体并且用乙烯-丙烯酸共聚物改性,任选地添加交联剂。
WO 2014/052143 A1描述了含水乙酸乙烯酯-乙烯共聚物分散体,所述分散体在辅助背衬涂层组合物中使用其处理的地毯的湿强度得以改善。这是通过使用部分水解的聚乙烯醇和完全水解的聚乙烯醇(在每种情况下具有高赫普勒(Hoeppler)粘度)的混合物使共聚物分散体稳定来实现的。
从US 4,126,415中已知聚乙烯亚胺适于为地毯提供抗静电涂饰剂。为此目的,使地毯纤维经受电火花放电,然后用聚乙烯亚胺盐的水溶液喷雾,并随后干燥。WO 2014/070818 A1公开了双组分底漆组合物,所述组合物在一种组分A)中包含乙酸乙烯酯-乙烯共聚物、丙烯酸酯增粘剂和聚乙烯亚胺并且在第二组分B)中包含环氧树脂。
所解决的问题在于提供一种基于含水乙酸乙烯酯-乙烯共聚物分散体的地毯涂层材料组合物,当其用于生产地毯时,使地毯在储水后的机械强度得以改善,而不需要官能共聚单体的共聚或特种稳定剂体系。
本发明提供乙酸乙烯酯-乙烯共聚物的水分散体和至少一种聚乙烯亚胺在用于生产地毯的地毯涂层组合物中作为粘合剂的用途。
适合的聚乙烯亚胺是具有重复结构单元-CH2-CH2-NH-且具有优选500至1 000000g/mol、更优选10 000至1 000 000g/mol的重均分子量(通过GPC确定)的聚合物。这种聚乙烯亚胺可例如以商品名LupasolR从BASF SE商购。在每种情况下基于乙酸乙烯酯-乙烯共聚物(干/干)的干重,聚乙烯亚胺以0.1wt%至10wt%、优选0.5wt%至5wt%的量包含在地毯涂层组合物中。
乙酸乙烯酯-乙烯共聚物是通过在水性介质中自由基引发60wt%至98wt%乙酸乙烯酯和2wt%至30wt%乙烯,优选75wt%至95wt%乙酸乙烯酯和5wt%至25wt%乙烯的乳液聚合而获得的,在每种情况下基于单体的总重量。进一步可能的是,任选地使至多10wt%、优选0.1wt%至10wt%另外的共聚单体共聚,在每种情况下基于单体的总重量。在每种情况下共聚单体的以wt%计的各项加起来为100wt%。
适合的另外的共聚单体是来自以下组的那些:在羧酸基团中具有3至12个碳原子的乙烯酯,如丙酸乙烯酯、月桂酸乙烯酯,具有8至11个碳原子的α-支链羧酸的乙烯酯,如VeoVaREH、VeoVaR9或VeoVaR10(Resolution的商品名称)。还适合的是具有1至15个碳原子的无支链醇或支链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-乙基己基酯、丙烯酸降冰片基酯。乙烯基卤化物如氯乙烯也是适合的。
其它适合的另外的共聚单体是烯键式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;烯键式不饱和羧酰胺和腈,优选丙烯酰胺和丙烯腈;富马酸和马来酸的单酯和二酯,如二乙酯和二异丙基酯,以及还有马来酸酐、烯键式不饱和磺酸和/或其盐,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,如多烯键式不饱和共聚单体,如例如己二酸二乙烯酯、马来酸二烯丙酯、甲基丙烯酸烯丙酯或氰尿酸三烯丙酯,或后交联共聚单体,如例如丙烯酰氨基乙醇酸(AGA)、甲基丙烯酰氨基乙醇酸甲酯(MAGME)、N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺(NMMA)、N-羟甲基烯丙基氨基甲酸酯,N-羟甲基丙烯酰胺或N-羟甲基甲基丙烯酰胺和N-羟甲基烯丙基氨基甲酸酯的烷基醚(如异丁氧基醚)或酯。还适合的是具有羟基或羧基的单体,如例如甲基丙烯酸羟烷基酯和丙烯酸羟烷基酯,如丙烯酸或甲基丙烯酸的羟乙基酯、羟丙基酯或羟丁基酯,以及还有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。
其它适合的另外的共聚单体是具有环氧官能团的共聚单体,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。适合的另外共聚单体的另外实例是具有硅官能团的共聚单体,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,其优选具有在每种情况下具有1至2个碳原子的烷基和/或烷氧基,如例如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。
特别优选不使另外的共聚单体共聚。
进行单体选择,使得乙酸乙烯酯-乙烯共聚物通常具有-20至+20℃的玻璃化转变温度Tg。聚合物的玻璃化转变温度Tg可通过DSC(差示扫描量热法,DIN EN ISO 11357-1/2)以已知方式确定。Tg还可预先使用Fox方程式近似地计算。根据Fox T.G.,Bull.Am.PhysicsSoc.1,3,第123页(1956),1/Tg=x1/Tg1+x2/Tg2+...+xn/Tgn,其中xn是单体n的质量分数(wt%/100),且Tgn是单体n的均聚物的玻璃化转变温度(开)。在Polymer Handbook第2版,J.Wiley&Sons,New York(1975)中列出了均聚物的Tg值。
乙酸乙烯酯-乙烯共聚物以已知方式制备,优选通过在自由基引发的水中乳液聚合来制备。聚合温度为40℃至120℃,优选60℃至90℃。在使气态共聚单体如乙烯共聚的情况下,优选在通常在5巴至120巴的压力下处理。可使用常规用于乳液聚合的引发剂如氢过氧化物或叔丁基氢过氧化物,或使用具有还原剂如(异)抗坏血酸或羟基甲亚磺酸钠(Brüggolite FF)的氧化还原引发剂组合引发聚合。在聚合期间可使用具有调节作用的物质以控制分子量。
所述乙酸乙烯酯-乙烯共聚物在保护胶体存在下或在乳化剂存在下、或在保护胶体和乳化剂的组合存在下聚合。
用于稳定聚合批料的常规保护胶体包括例如部分或完全水解的聚乙烯醇;聚乙烯吡咯烷酮;聚乙烯醇缩醛;呈水溶性形式的多糖,如淀粉、纤维素或其衍生物,如羧甲基衍生物、甲基衍生物、羟乙基衍生物或羟丙基衍生物;蛋白质,如酪蛋白或酪蛋白酸盐、大豆蛋白质、明胶;木素磺酸盐;合成聚合物,如聚(甲基)丙烯酸、(甲基)丙烯酸酯与羧基官能共聚单体单元的共聚物、聚(甲基)丙烯酰胺、聚乙烯磺酸和其水溶性共聚物;三聚氰胺-甲醛磺酸盐、萘-甲醛磺酸盐、苯乙烯-马来酸共聚物和乙烯基醚-马来酸共聚物。
优选纤维素或其衍生物,或部分水解的聚乙烯醇,其具有80mol%至95mol%的水解度和在4%水溶液中1至40mPas、尤其是3至30mPas的赫普勒粘度(赫普勒法,在20℃,DIN53015)。特别优选部分水解的低分子量聚乙烯醇,各自具有优选80mol%至95mol%、更优选85mol%至90mol%且最优选87mol%至89mol%的水解度,以及在每种情况下优选1至5mPas且更优选2至4mPas的赫普勒粘度(根据DIN 53015,赫普勒法,在20℃,在4%水溶液中所确定)。
任选地还可使用与部分水解的低分子量聚乙烯醇混合的具有优选80mol%至95mol%的水解度和在4%水溶液中优选>5至40mPas、更优选8至40mPas的赫普勒粘度(DIN53015赫普勒法,在20℃)的部分水解的高分子量聚乙烯醇。任选地还可使用与部分水解的低分子量聚乙烯醇混合的具有优选96mol%至100mol%、尤其是98mol%至100mol%的水解度和在4%水溶液中优选10至56mPas的赫普勒粘度(DIN 53015赫普勒法,在20℃)的完全水解的高分子量聚乙烯醇。这里部分水解的高分子量聚乙烯醇和/或完全水解的高分子量聚乙烯醇各自以0.1wt%至4wt%的量采用,全部基于共聚单体的总重量。
还优选具有80mol%至99.9mol%、优选85mol%至95mol%的水解度和在4%水溶液中1至30mPas的赫普勒粘度(根据DIN 53015在20℃下所确定)的改性聚乙烯醇(下文也称为X-PVOH)。其实例是带有官能团如乙酰乙酰基的聚乙烯醇。还优选所谓的E-PVOH聚乙烯醇,其含有乙烯单元并且例如以商品名已知。E-PVOH是乙酸乙烯酯和乙烯的部分或优选完全水解的共聚物。优选的E-PVOH具有0.1mol%至12mol%、优选1mol%至7mol%、更优选2mol%至6mol%且尤其是2mol%至4mol%的乙烯含量。质量平均聚合度在500至5000范围内,优选在2000至4500范围内且更优选在3000至4000范围内。水解度通常大于92mol%,优选在94.5mol%至99.9mol%范围内且更优选在98.1mol%至99.5mol%范围内。
保护胶体可商购并且可使用本领域技术人员已知的方法获得。还可使用所述保护胶体的混合物。聚合优选在总共2wt%至10wt%、更优选总共5wt%至10wt%的保护胶体存在下进行,全部基于共聚单体的总重量。
优选用于稳定分散体的非离子型乳化剂。还可使用离子型、优选阴离子型乳化剂。还可使用非离子型乳化剂与阴离子型乳化剂的组合。基于共聚单体的总重量,乳化剂的量通常在0.1wt%至5.0wt%范围内。
适合的非离子型乳化剂包括例如酰基乙氧基化物、烷基乙氧基化物、油基乙氧基化物和烷基芳基乙氧基化物。这些产品可例如以GenapolR或LutensolR商购。它们包括乙氧基化的单烷基酚、二烷基酚和三烷基酚,优选具有3至50个氧化乙烯单元的乙氧基化度和C4至C12烷基部分;以及还有乙氧基化脂肪醇,优选具有3至80个氧化乙烯单元的乙氧基化度和C8至C36烷基部分。适合的非离子型乳化剂进一步包括具有3至30个氧化乙烯单元的乙氧基化度的C13-C15羰基合成醇乙氧基化物、具有11至80个氧化乙烯单元的乙氧基化度的C16-C18脂肪醇乙氧基化物、具有3至11个氧化乙烯单元的乙氧基化度的C10羰基合成醇乙氧基化物、具有3至20个氧化乙烯单元的乙氧基化度的C13羰基合成醇乙氧基化物、具有20个氧化乙烯基团的聚氧乙烯山梨糖醇酐单油酸酯、具有10wt%的最低氧化乙烯含量的氧化乙烯和氧化丙烯的共聚物、具有4至20个氧化乙烯单元的乙氧基化度的油醇的聚聚氧化乙烯醚,以及还有具有4至20个氧化乙烯单元的乙氧基化度的壬基酚的聚氧化乙烯醚。
特别优选乙氧基化度为3至30个氧化乙烯单元的C12-C14脂肪醇乙氧基化物。
适合的阴离子型乳化剂的实例包括具有12至20个碳原子的直链脂族羧酸的钠盐、钾盐和铵盐;羟基十八烷磺酸钠;具有12至20个碳原子的羟基脂肪酸钠盐、钾盐和铵盐以及其磺化和/或乙酰化产物;烷基硫酸酯的钠盐、钾盐和铵盐,包括如三乙醇胺盐,以及各自具有10至20个碳原子的烷基磺酸盐和具有12至20个碳原子的烷基芳基磺酸盐的钠盐、钾盐和铵盐;在烷基部分具有8至18个碳原子的二甲基二烷基氯化铵和其磺化产物;与具有4至16个碳原子的脂族饱和一元醇的磺基琥珀酸酯的钠盐、钾盐和铵盐,和与具有10至12个碳原子的一元脂族醇的聚乙二醇醚的磺基琥珀酸4-酯的钠盐、钾盐和铵盐,尤其是它们的二钠盐;与聚乙二醇壬基苯基醚的磺基琥珀酸4-酯的钠盐、钾盐和铵盐,尤其是其二钠盐;双环己基磺基琥珀酸酯的钠盐、钾盐和铵盐,尤其是其钠盐;木素磺酸以及还有其钙盐、镁盐、钠盐和铵盐;树脂酸以及还有氢化和脱氢树脂酸以及还有它们的碱金属盐。
对于在聚合条件下为液体的单体,聚合通常在每种情况下进行至≥95wt%、优选高达95wt%至99wt%的转化率。
由此可获得的乙酸乙烯酯-乙烯共聚物的水分散体各自具有30wt%至75wt%、优选50wt%至65wt%的固体含量。乙酸乙烯酯-乙烯共聚物的适合的水分散体也可商购;例如,来自Wacker Chemie AG的VinnapasR分散体。
本发明进一步提供地毯涂层组合物,所述地毯涂层组合物包含乙酸乙烯酯-乙烯共聚物的水分散体、和基于乙酸乙烯酯-乙烯共聚物(干/干)的干重0.1wt%至10wt%的至少一种聚乙烯亚胺、和基于乙酸乙烯酯-乙烯共聚物(干/干)的干重100wt%至1400wt%的填料、水、任选存在的一种或多种添加剂以及任选存在的一种或多种辅助剂。
地毯涂层组合物的固体含量优选在72wt%至83wt%范围内,且更优选在75wt%至80wt%范围内,全部基于地毯涂层组合物的总重量。在混合填料后并且不存在添加剂或辅助剂的情况下,地毯涂层组合物具有优选≤7000mPas、更优选≤3000mPas的布氏粘度(如使用布氏RV测量仪器,使用转子4,以20rpm,在25℃下所测量)。
适合的填料包括例如高岭土、滑石、萤石、飞灰、三水合铝,优选白垩。
添加剂的实例是增稠剂,如聚丙烯酸酯或纤维素醚或起泡助剂。优选将起泡助剂混合用于泡沫应用。增稠剂可经混合以建立地毯涂层组合物的目标粘度。为此所需的增稠剂的量通常在0.1wt%至6wt%范围内且优选在1wt%至3wt%范围内,全部基于乙酸乙烯酯-乙烯共聚物(干/干)的重量。优选用于建立2000至10 000mPas的布氏粘度(使用布氏RV测量仪器,使用转子4,以20rpm,在25℃下测量)的该方法。然而,本发明的程序使得可以避免增稠剂。
常规辅助剂包括例如分散剂、润湿剂、颜料、疏水剂或杀生物剂,如甲醛贮库型(depot)化合物、异噻唑啉酮、酚或季铵化合物。为了优化配制物粘度,还可使用有机酸如柠檬酸。地毯涂层组合物优选不含塑化剂或成膜助剂。
地毯涂层组合物含有100至1400重量份的填料对100重量份的乙酸乙烯酯-乙烯共聚物(干/干)。这也被称为100%至1400%的填充水平。配制物中填料的量可根据期望的涂层性质而变化。填料级分(填充水平)越高,机械性质越低。
预涂层优选利用具有300%至1400%的填充水平的地毯涂层组合物。对于用于住宅应用的预涂层,填充水平特别优选在600%至1000%范围内,而对于商业应用如办公室、酒店或船舶,填充水平优选300%至600%。
辅助涂层优选利用地毯涂层组合物的填充水平对于住宅应用为275%至600%,而对于商业应用如办公室、酒店或船舶,填充水平为200%至275%。
在用于生产地毯涂层组合物的可能程序中,将乙酸乙烯酯-乙烯共聚物的水分散体和聚乙烯亚胺级分混合,然后搅拌加入填料。还可通过甚至在乙酸乙烯酯和乙烯的聚合之前、或期间或之后,将聚乙烯亚胺级分添加至聚合混合物中来进行。
任何添加剂和辅助剂通常均可在任何阶段,优选在混合填料之前,混合至地毯涂层组合物中。本领域技术人员熟悉的已建立的地毯涂层组合物生产设备适于生产地毯涂层组合物。
本发明进一步提供在预涂层和/或辅助涂层中涂覆有本发明的一种或多种地毯涂层组合物的地毯。
地毯涂层组合物可有利地使用现有工艺用于制造地毯的现有装置中。
地毯涂层组合物适于地毯(例如连续压片产品或拼块地毯)的加固。
地毯涂层组合物用于制造簇绒地毯、织造地毯或针刺毡地毯(needlefeltcarpet)。
以下实施例用于进一步阐明本发明:
方法:
玻璃化转变温度Tg的的确定:
聚合物的玻璃化转变温度Tg是通过DSC(差示扫描量热法,DIN EN ISO 11357-1/2),使用来自Mettler-Toledo的DSC 1差示扫描量热计在开口坩埚中以10K/min的加热速率确定的。将玻璃化转变温度视为第二加热曲线中点处的温度(中点=梯段高度的一半)。
布氏粘度的确定:
在调节至所报告的温度后,通过使用所报告的特定转子,以所报告的每分钟转数,根据EN ISO 2555,使用布氏RV粘度计确定聚合物水分散体的布氏粘度。以mPas报告粘度。
粒度Dw的确定:
根据ISO 13320使用BeckmannLS测量仪器确定平均粒子直径Dw。
含水乙酸乙烯酯-乙烯共聚物分散体的制备
分散体A(A):
首先向氮吹扫的572升压力反应器中装入以下组分:
125.2kg 去离子水,
56.0kg 具有88mol%的平均水解度和4mPas的赫普勒粘度(如根据DIN 53015在20℃下,在4%水溶液中所确定)的20wt%的聚乙烯醇水溶液,
26.1kg 平均乙氧基化度为30mol EO单元的脂肪醇乙氧基化物的25wt%水溶液,
241.7kg 乙酸乙烯酯,
0.48kg 1.0wt%硫酸铁铵水溶液。
使用250mL甲酸(98wt%)将初始装料调节至pH 4.0。
在搅动(以240rpm搅拌)下,将初始装料加热至35℃,并注入乙烯直至30巴的压力。在达到35℃的温度和30巴的压力后,引发剂进料-由3.5wt%的过氧化氢水溶液和10wt%的异抗坏血酸钠水溶液组成-各自以700g/h开始。一旦反应已开始(引发剂进给开始后10分钟),如从反应器内部温度的增加显而易见的,放出的反应热便将反应器内部温度提升至85℃。同时,在反应已开始后10分钟,以35.1kg/h开始乙酸乙烯酯进料(进料时间120min,70.2kg)。在达到80℃的反应器内部温度后,将乙烯再注入至高达58巴的目标压力,直至已增加52.8kg的乙烯总量。
在完成乙酸乙烯酯进料后,引发剂进料各自以2000g/h继续进一步持续30分钟,在此期间压力降至20巴。随后将该批料冷却至70℃并转移至“无压力”(低压)反应器中,并且在其中在700毫巴(绝对)的压力下,通过混合2.6kg叔丁基氢过氧化物溶液(10wt%,于水中)和2.6kg异抗坏血酸钠溶液(10wt%,于水中)进行后聚合。
固体含量:63wt%
布氏粘度:1300mPas(转子2,20rpm,23℃)
粒度:Dw 1.0μm,(Coulter LS)
玻璃化转变温度:7.0℃(DSC)
保护胶体:3.1wt%,基于共聚单体
乳化剂:1.8wt%,基于共聚单体
分散体B(B):
首先向氮吹扫的590L压力反应器中装入以下组分:
134.9kg 去离子水,
75.9kg 具有88mol%的平均水解度和4mPas的赫普勒粘度(如根据DIN 53015在20℃下,在4%水溶液中所确定)的20wt%的聚乙烯醇水溶液,
12.5kg 具有88mol%的平均水解度和23-26mPas的赫普勒粘度(如根据DIN53015在20℃下,在4%水溶液中所确定)的10wt%的聚乙烯醇水溶液,
224kg 乙酸乙烯酯,
0.48kg 1.0wt%硫酸铁铵水溶液。
用250mL甲酸(98wt%)将初始装料调节至pH值4.0。
在搅动(以240rpm搅拌)下,将初始装料加热至55℃,并注入乙烯直至20巴的压力。在达到55℃的温度和20巴的压力后,引发剂进料-由3wt%的叔丁基氢过氧化物水溶液和5wt%的抗坏血酸水溶液组成-各自以700g/h开始。一旦反应已开始,如反应器内部温度的增加所明确指示的,放出的反应热便使反应器内部温度升高至90℃并使压力升高至48巴。引发剂进料均降低至350g/h,以控制反应热。
在反应已开始45分钟后,开始乙酸乙烯酯进料和聚乙烯醇进料。将乙酸乙烯酯以40kg/h的速率经90分钟(=60kg乙酸乙烯酯)添加至反应器中,而以14kg/h的速率经120分钟(=28.0kg含水聚乙烯醇溶液)添加聚乙烯醇-由具有88mol%的平均水解度和4mPas的赫普勒粘度(如根据DIN 53015在20℃下,在4%水溶液中所确定)的10wt%聚乙烯醇水溶液。在聚合期间以44巴的目标压力再注入乙烯,直至已注入34kg的总乙烯量。
在完成进料后,引发剂进料各自以1300g/h继续进一步持续30分钟,在此期间压力降至20巴。随后将该批料冷却至65℃并转移至“无压力”(低压)反应器中,并且在其中在700毫巴(绝对)的压力下,通过混合1kg叔丁基氢过氧化物溶液(10wt%,于水中)和2kg抗坏血酸溶液(5wt%,于水中)进行后聚合。
固体含量:58wt%
布氏粘度:1800mPas(转子2,20rpm,23℃)
粒径:Dw 1.0μm,(Coulter LS)
玻璃化转变温度:15.0℃(DSC)
保护胶体:6.2wt%,基于共聚单体
分散体C(C):
采用类似于用于制备分散体B的程序,不同之处在于在初始装料中仅包含一种聚乙烯醇,具体为94.0kg具有88mol%的平均水解度和4mPas的赫普勒粘度(如根据DIN 53015在20℃下,在4%水溶液中所确定)的20wt%的聚乙烯醇水溶液,并且不加入聚乙烯醇,并且选择乙酸乙烯酯和乙烯的量以获得具有77wt%乙酸乙烯酯和23wt%乙烯的共聚物。
固体含量:52.5wt%
布氏粘度:210mPas(转子1,20rpm,23℃)
粒径:Dw 1.0μm,(Coulter LS)
玻璃化转变温度:-7.0℃(DSC)
保护胶体:6.4wt%,基于共聚单体
地毯涂层组合物的制备:
配制物1(F1):
分散体A至C用于基于以下通式制备地毯涂层组合物:
100重量份的特定分散体(干聚合物),
X重量份的聚乙烯亚胺,如实施例中所报告的类型和量,
450重量份的白垩(Carbocia 80、Carbocia)(填料),
0.5重量份的起泡助剂(月桂基硫酸钠)。
以重量份数计的各项基于特定地毯涂层组合物的干重。
添加一定量的额外的水以获得具有81.5wt%的固体含量的地毯涂层组合物。
通过首先装入水和特定的分散体以及特定的聚乙烯亚胺并在搅动下混合填料和此后的起泡助剂来制备地毯涂层组合物。
地毯涂层组合物具有81.5wt%的固体含量和450wt%的填充水平。
然后通过混合增稠剂(来自Matco的Matco TR 10丙烯酸酯增稠剂)建立6500mPas的最终粘度(使用布氏RV测量仪器,使用转子4,以20rpm,在25℃下测量)。
配制物2(F2):
与F1一样,但用800重量份的白垩(Carbocia 80,Carbocia)。添加一定量的额外的水,产生具有81.5wt%的固体含量的地毯涂层组合物。
通过混合增稠剂(来自Matco的Matco TR 10丙烯酸酯增稠剂)建立6500mPas的最终粘度(使用布氏RV测量仪器,使用转子4,以20rpm,在25℃下测量)。
配制物3(F3):
与F1一样,但使用250重量份的白垩(Carbocia 80,Carbocia)。添加一定量的额外的水,产生具有81.5wt%的固体含量的地毯涂层组合物。
通过混合增稠剂(来自Matco的Matco TR 10丙烯酸酯增稠剂)建立6500mPas的最终粘度(使用布氏RV测量仪器,使用转子4,以20rpm,在25℃下测量)。
地毯PA和PP的生产:
使用厨房器具将上述特定的地毯涂层组合物(配制物1至3)起泡3分钟以获得950至1015g/l的泡沫密度。
地毯PA:
用148g特定起泡地毯涂层组合物均匀预涂覆来自Edel的38cm×33cm大小的Helsinki 151坯布毛圈簇头簇绒地毯(100%聚酰胺(下文称为PA);550g/m2簇头重量)。
此后将60g起泡地毯涂层组合物F1至F3施加并均匀铺展作为辅助涂层。然后将纺织背衬(Action Back聚丙烯编织物)置于顶部,并且在没有压力的情况下用1.6kg辊处理两次。在烘箱中在130℃下干燥20分钟。
地毯PP:
用148g特定起泡地毯涂层组合物均匀预涂覆来自Edel的38cm×33cm大小的Puma182坯布毛圈簇头簇绒地毯(100%聚丙烯(下文称为PP);550g/m2簇头重量)。
此后将60g起泡地毯涂层组合物F1至F3施加并均匀铺展作为辅助涂层。然后将纺织背衬(Action Back聚丙烯编织物)置于顶部,并且在没有压力的情况下用1.6kg辊处理两次。在烘箱中在130℃下干燥20分钟。
用于测试地毯的方法:
簇绒拔出力的测量:
根据ISO 4919使用Zwick测试仪在23℃和50%相对湿度下进行簇绒拉拔出力的测试。将特定的地毯夹在测量装置底部上的顶部部分中,并将针拧入地毯毛圈中。在十个不同的地毯毛圈上确定将毛圈拉出地毯所需的力。测量结果的平均值报告为干簇绒拔出力。
为了确定湿簇绒拔出力,将为确定干簇绒拔出力而制备的样品在水中放置10min,并且在进一步测试之前,将表面轻拭干燥并由此去除多余的水。
干簇绒拔出力和湿簇绒拔出力是由预涂层提供的簇绒粘合的质量和地毯表面的磨损性质的量度。因此它们应当尽可能高。
抗分层性的测量:
根据DIN EN ISO 11857使用Zwick测试仪在23℃和50%相对湿度下确定抗分层性。通过在机器方向上从特定地毯上切割5cm宽和20cm长的条带并用手在窄边上经20cm的长度分层来制备三个样品。将每个初始分层的样品夹紧至Zwick测试仪中,并以300mm/min的速率从地毯分离辅助背衬。根据DIN EN ISO 11857,从每个样品在可容许的测量范围内的峰值平均值来确定五个样品的总平均值。实际上,出于评价的目的,特定测量曲线的前25%被标记并忽略。图示轨迹的下一个50%被划分成5个相等的区段,并且从这些区段中的每一个确定特定的峰值。峰值被用于计算平均值,而平均值进而被用于计算总平均值。以牛顿[N]报告抗分层性。
为了确定抗湿分层性,将为确定抗干分层性而制备的样品在水中再放置10min,并且在进一步测试之前,将表面轻拭干燥并由此去除多余的水。
实施例1:
在实施例1中,将具有分散体A作为粘合剂的配制物F1另外与0.5%(1.A)、1%(1.B)、3%(1.C)和5%(1.D)(在每种情况下都基于乙酸乙烯酯-乙烯共聚物的干重)的聚乙烯亚胺(LUPASOL FG,BASF,平均分子量800g/mol)混合。测试地毯PA。表1汇总了测试结果。
实施例2:
与实施例1一样,但使用聚乙烯亚胺LUPASOL G20(LUPASOL G20,BASF,平均分子量1300g/mol)。表1汇总了测试结果。
实施例3:
与实施例1一样,但使用聚乙烯亚胺LUPASOL HF(LUPASOL HF,BASF,平均分子量25000g/mol)。表1汇总了测试结果。
实施例4:
与实施例1一样,但使用基于所用乙酸乙烯酯-乙烯共聚物干重的聚乙烯亚胺LUPASOL P(LUPASOL P,BASF,平均分子量750 000g/mol)。表1汇总了测试结果。
比较实施例:
与实施例1一样,但不添加任何聚乙烯亚胺。表1汇总了测试结果。
表1:
关于具有配制物F1和分散体A的地毯PA上的实施例1至4。
(*=改性配制物的抗湿分层性与未改性参照物的抗湿分层性的比率,百分比)
从测试结果明显看出,对于具有混合稳定化的分散体A,尤其是具有相对高分子量的聚乙烯亚胺的分散体A,簇绒拔出和抗分层性的湿性质显著改善。
实施例5至7:
在实施例5至7中,在每种情况下对聚酰胺地毯PA或聚丙烯地毯PP进行测试,并且在每种情况下,
在实施例5.A、5.B、5.C和5.D中,对具有分散体A的配制物F1,添加聚乙烯亚胺或不添加聚乙烯亚胺,
在实施例6.A、6.B、6.C和6.D中,对具有分散体B的配制物F1,添加聚乙烯亚胺或不添加聚乙烯亚胺,
在实施例7.A、7.B、7.C和7.D中,对具有分散体C的配制物F1,添加聚乙烯亚胺或不添加聚乙烯亚胺。
在这些情况中的每一种下,添加1wt%聚亚胺LupasolP(Lupasol P,BASF,平均分子量750 000g/mol),在每种情况下基于乙酸乙烯酯-乙烯共聚物的干重。
机械测试结果可参见表2。
汇总于表2中的结果证实特别是在湿储存之后机械性质改善的效果。特别显著的是在分散体C的情况下抗分层性和簇绒拔出力的增加。作为纯聚乙烯醇稳定的乙酸乙烯酯-乙烯共聚物分散体的分散体B,也显示在抗分层性(湿)方面的显著改善。对于部分稳定的分散体A,主要在簇绒拔出测量中可获得改善。
表2:
地毯PA和PP上的具有分散体A(实施例5.A-5.D)、分散体B(实施例6.A-6.D)和分散体C(实施例7.A-7.D)的配制物F1中MW 750 000g/mol的1wt%聚乙烯亚胺(Lupasol P)。
*对于各自的地毯PA或PP,改性配制物的抗湿分层性或湿簇绒拔出力与未改性参照物的抗湿分层性或湿簇绒拔出力的比率,百分比。
实施例8和9:
在实施例8和实施例9中,对于每种情况下的预涂层,使用配制物2,其具有分散体B和1wt%(在每种情况下基于乙酸乙烯酯-乙烯共聚物的干重)的聚乙烯亚胺(LupasolP,BASF,平均分子量750 000g/mol)。
对于辅助涂层,使用配制物3,其具有分散体C和1wt%(在每种情况下基于乙酸乙烯酯-乙烯共聚物的干重)的聚乙烯亚胺(LupasolP,BASF,平均分子量750 000g/mol)。
用于地毯PA和PP的施加形式是,湿/干-预涂层的初步干燥和辅助涂层的后续施加-或湿/湿-无在辅助涂层的后续施加之前对预涂层的初步干燥。
机械测试结果汇总于表3中。
表3:
地毯PA和PP上预涂层中具有分散体B(F2)的配制物F2中的1wt%聚乙烯亚胺和辅助涂层(F3)中具有分散体C的配制物F3中的1wt%聚乙烯亚胺。施加模式被区分为湿/干和湿/湿。
*对于各自的地毯PA或PP,改性配制物的抗湿分层性或湿簇绒拔出力与未改性参照物的抗湿分层性或湿簇绒拔出力的比率,百分比。
从实施例8和9的结果明显看出,对于地毯变体PP和PA两者,对于湿/干和湿/湿两种施加模式,在添加聚乙烯亚胺的情况下,在抗湿分层性方面都实现了显著改善。在此,特别是在对于预涂层初步干燥的临界施加模式(湿/干)的情况下,实现了在湿储存后抗分层性和簇绒拔出量最高达500%的显著增加。
从根本上说,可通过添加聚乙烯亚胺实现湿性质的改善,对于PA地毯以及对于PP地毯两者均如此。
Claims (9)
1.乙酸乙烯酯-乙烯共聚物的水分散体和至少一种聚乙烯亚胺在用于生产地毯的地毯涂层组合物中作为粘合剂的用途。
2.根据权利要求1所述的用途,其特征在于,所述乙酸乙烯酯-乙烯共聚物是通过60wt%至98wt%乙酸乙烯酯和2wt%至30wt%乙烯在水性介质中自由基引发的乳液聚合获得的,在每种情况下所述百分比基于共聚单体的总重量,在每种情况下以wt%计的各项加起来为100wt%。
3.根据权利要求1或2所述的用途,其特征在于,所述乙酸乙烯酯-乙烯共聚物的乳液聚合在保护胶体存在下或在乳化剂存在下、或在保护胶体和乳化剂的组合存在下发生。
4.根据权利要求1至3之一所述的用途,其特征在于,所述聚乙烯亚胺具有500g/mol至1000 000g/mol的重均分子量。
5.根据权利要求1至3之一所述的用途,其特征在于,所述聚乙烯亚胺具有10 000g/mol至1 000 000g/mol的重均分子量。
6.根据权利要求1至5之一所述的用途,其特征在于,基于所述乙酸乙烯酯-乙烯共聚物的干重,所述聚乙烯亚胺以0.1wt%至10wt%的量包含在所述地毯涂层组合物中。
7.一种地毯涂层组合物,其包含乙酸乙烯酯-乙烯共聚物的水分散体、和基于所述乙酸乙烯酯-乙烯共聚物的干重0.1wt%至10wt%(干/干)的至少一种聚乙烯亚胺、和基于所述乙酸乙烯酯-乙烯共聚物的干重100wt%至1400wt%(干/干)的填料、水、任选存在的一种或多种添加剂以及任选存在的一种或多种辅助剂。
8.根据权利要求7所述的地毯涂层组合物,其通过混合所述乙酸乙烯酯-乙烯共聚物的水分散体和所述聚乙烯亚胺级分,然后在搅拌下掺入所述填料来获得,或通过在乙酸乙烯酯和乙烯的聚合之前或期间或之后,将所述聚乙烯亚胺添加至用于制备所述水分散体的聚合混合物中来获得。
9.一种地毯,其在所述预涂层和/或辅助涂层中涂覆有根据权利要求7或8所述的一种或多种地毯涂层组合物。
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CN201680067463.7A Pending CN108291361A (zh) | 2015-11-24 | 2016-11-09 | 用于地毯涂层组合物的粘合剂 |
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US (1) | US11220783B2 (zh) |
EP (1) | EP3380664B1 (zh) |
CN (1) | CN108291361A (zh) |
DE (1) | DE102015223233A1 (zh) |
TR (1) | TR201909764T4 (zh) |
WO (1) | WO2017089127A1 (zh) |
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CN108367549A (zh) * | 2015-12-15 | 2018-08-03 | 肖氏工业集团公司 | 地毯涂层、具有改进的湿脱层强度的地毯以及其制造方法 |
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DE69201426T2 (de) * | 1991-09-24 | 1995-06-22 | Air Prod & Chem | Wässriges Hochleistungskontaktklebmittel enthaltend Mikrohohlkugeln. |
EP1008689A2 (en) * | 1998-12-09 | 2000-06-14 | National Starch and Chemical Investment Holding Corporation | Carpet back coating composition having increased wet strength |
CN1752342A (zh) * | 2004-09-22 | 2006-03-29 | 三星Total株式会社 | 用于减少新家综合症的壁纸 |
CN104684937A (zh) * | 2012-09-27 | 2015-06-03 | 瓦克化学公司 | 地毯涂层组合物 |
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JPS5321244A (en) * | 1976-08-10 | 1978-02-27 | Kuraray Co Ltd | Construction sheet material having tenacity |
US4126415A (en) | 1977-10-12 | 1978-11-21 | Allied Chemical Corporation | Antistatic carpet |
JPS592474B2 (ja) * | 1979-12-19 | 1984-01-18 | 電気化学工業株式会社 | 接着剤組成物 |
US20060292952A1 (en) * | 2005-06-23 | 2006-12-28 | Building Materials Investment Corporation | Fiber mat and process for making same |
BE1020391A3 (de) * | 2010-04-30 | 2013-09-03 | Shaw Ind Group Inc | Vinylfreies elastisches bodenbelagsprodukt und verfahren zu dessen herstellung. |
WO2014031579A2 (en) | 2012-08-21 | 2014-02-27 | Celanese International Corporation | Carpet coating compositions of vinyl acetate having improved wet and/or dry strength |
US20140127499A1 (en) | 2012-11-02 | 2014-05-08 | Ashland Licensing And Intellectual Property Llc | Two Part Primer Composition |
-
2015
- 2015-11-24 DE DE102015223233.6A patent/DE102015223233A1/de not_active Withdrawn
-
2016
- 2016-11-09 WO PCT/EP2016/077030 patent/WO2017089127A1/de active Application Filing
- 2016-11-09 CN CN201680067463.7A patent/CN108291361A/zh active Pending
- 2016-11-09 US US15/776,302 patent/US11220783B2/en active Active
- 2016-11-09 TR TR2019/09764T patent/TR201909764T4/tr unknown
- 2016-11-09 EP EP16798426.9A patent/EP3380664B1/de active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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DE69201426T2 (de) * | 1991-09-24 | 1995-06-22 | Air Prod & Chem | Wässriges Hochleistungskontaktklebmittel enthaltend Mikrohohlkugeln. |
EP1008689A2 (en) * | 1998-12-09 | 2000-06-14 | National Starch and Chemical Investment Holding Corporation | Carpet back coating composition having increased wet strength |
CN1752342A (zh) * | 2004-09-22 | 2006-03-29 | 三星Total株式会社 | 用于减少新家综合症的壁纸 |
CN104684937A (zh) * | 2012-09-27 | 2015-06-03 | 瓦克化学公司 | 地毯涂层组合物 |
Also Published As
Publication number | Publication date |
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TR201909764T4 (tr) | 2019-07-22 |
DE102015223233A1 (de) | 2017-05-24 |
WO2017089127A1 (de) | 2017-06-01 |
EP3380664B1 (de) | 2019-04-24 |
US20180327966A1 (en) | 2018-11-15 |
US11220783B2 (en) | 2022-01-11 |
EP3380664A1 (de) | 2018-10-03 |
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