CN101180181B - 制备防水层叠体的方法 - Google Patents

制备防水层叠体的方法 Download PDF

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CN101180181B
CN101180181B CN2006800181231A CN200680018123A CN101180181B CN 101180181 B CN101180181 B CN 101180181B CN 2006800181231 A CN2006800181231 A CN 2006800181231A CN 200680018123 A CN200680018123 A CN 200680018123A CN 101180181 B CN101180181 B CN 101180181B
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M·B·赫尔梅柯
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Abstract

本发明涉及制备防水层叠体的方法，包括将热熔性湿固化粘合剂施加在主基材上和使所述主基材与在层叠之前已经用防水材料处理过的次级基材粘结。所述粘合剂组合物包含由多元醇组分和多聚异氰酸酯组分形成的热熔性湿固化聚氨酯预聚物。所述多元醇组分包含数均分子量约500～约8,000的第一聚醚多元醇；熔点小于约40℃的第一聚酯多元醇或分子量约200～约1,000的第二聚醚多元醇，和熔点为约40℃～约120℃的结晶聚酯多元醇。

Description

制备防水层叠体的方法
技术领域
本发明涉及用热熔性湿固化聚氨酯粘合剂组合物制备防水(waterrepellent)层叠体的方法。
背景技术
防水层叠体被用于制备多种防水服装。防水层叠体通常包含具有夹在两个基材之间的粘合剂的主基材和次级基材。所述主基材是将粘合剂首先被施加于其两个表面之一上的基材。所述次级基材是与所述主基材的带有粘合剂的表面粘结以形成层叠体的基材。为了赋予防水层叠体防水性，存在不同的处理和层叠所述基材的方法。可以在防水处理之前将所述主基材和次级基材层叠。或者，可以在层叠之前用防水材料处理所述次级基材，但是仅在其暴露表面上处理，即将暴露于环境(例如潮湿环境)的表面。其粘结表面(即将与所述主基材的带有粘合剂的表面粘结的表面)保持未处理。作为替代，在与带有粘合剂的主基材层叠之前，可以用防水材料对所述次级基材的暴露表面和其粘结表面这两者进行处理。然而，当用纺织工业中现有的热熔性湿固化聚氨酯粘合剂使得次级基材的经处理的粘结表面与主基材的带有粘合剂的表面粘结时，由此形成的防水层叠体迄今显示出最小粘附力。
发明概述
一方面，本发明的特征在于制备防水层叠体的方法。所述层叠体包含具有第一表面和第二表面的主基材，和具有粘结表面和暴露表面的次级基材。所述次级基材的粘结表面和暴露表面已经用防水材料处理过。所述方法包括a)将热熔性湿固化聚氨酯粘合剂组合物施加在所述主基材的第一表面上以形成带有粘合剂的表面；和b)使所述主基材的带有粘合剂的表面与所述次级基材的粘结表面接触以形成层叠体。所述粘合剂组合物包含重均分子量不大于约20,000g/mol的热熔性湿固化聚氨酯预聚物。该预聚物是多元醇组分和多聚异氰酸酯组分的反应产物。所述多元醇组分包含由选自环氧乙烷、环氧丙烷、1，2-环氧丁烷、1，4-环氧丁烷或其混合物的至少一种单体形成的第一聚醚多元醇；熔点小于约40℃的第一聚酯多元醇；和熔点为约40℃～约120℃的结晶聚酯多元醇。
在一种实施方案中，所述粘合剂组合物进一步包含数均分子量为约500g/mol～约6,000g/mol的无定形聚酯多元醇。
另一方面，本发明的特征在于制备防水层叠体的方法，所述层叠体具有：具有第一表面和第二表面的主基材和具有粘结表面和暴露表面的次级基材。所述次级基材的粘结表面和暴露表面已经用防水材料处理过。所述方法包括a)将热熔性湿固化聚氨酯粘合剂组合物施加在所述主基材的第一表面上以形成带有粘合剂的表面；和b)使所述主基材的带有粘合剂的表面与所述次级基材的粘结表面接触以形成层叠体。所述粘合剂组合物包含重均分子量不大于约20,000g/mol的热熔性可湿固化的聚氨酯预聚物。该预聚物是多元醇组分和多聚异氰酸酯组分的反应产物。所述多元醇组分包含由选自环氧乙烷、环氧丙烷、1，2-环氧丁烷、1，4-环氧丁烷或其混合物的至少一种单体形成的第一聚醚多元醇；数均分子量为约200g/mol～约1,000g/mol的第二聚醚多元醇，和熔点为约40℃～约120℃的结晶聚酯多元醇。
另一方面，本发明的特征在于由本发明的方法制成的防水层叠体。
本发明的层叠体显示出良好的可洗性(或耐洗性、或耐水解性)。消费者环境中的良好可洗性定义为能够经受大于约20个标准洗涤周期(washcycle)。当所述组合物被用于衣服上如户外服装或运动服装时，良好的可洗性是重要的。
在一种实施方案中，所述防水层叠体包含作为所述主基材的热塑性膜和作为所述次级基材的持久防水(DWR)织物。该层叠体显示出柔软的手感、可洗性和耐干洗性。
在另一实施方案中，防水层叠体包含作为所述主基材的透气热塑性膜和作为所述次级基材的持久防水(DWR)织物。该层叠体显示出柔软的手感、可洗性、耐干洗性和透气性。
本发明的防水层叠体可以例如用于制备防水服装，如防雨服饰(protective rain gear)、体育和运动服装服饰(athletic and sportswearapparel gear)、军队制服、工业防护服、医用服装(medical garment)、帐篷、户外睡袋、露营装备等。
发明详述
一方面，本发明的特征在于防水层叠体，其包含至少两个基材-具有夹在所述两个基材之间的热熔性湿固化聚氨酯粘合剂组合物的主基材和次级基材。所述主基材具有将粘合剂首先施加在其上的带有粘合剂的表面。所述次级基材具有暴露表面和粘结表面，该粘结表面与所述主基材的带有粘合剂的表面粘结以形成层叠体。所述主基材可以由任何适宜的材料制成，如根据最终用途可以是湿气可透过或可以不是湿气可透过的热塑性膜，或者同样根据最终用途可以用防水剂处理过或未处理过的织物。所述热塑性膜的实例包括例如聚四氟乙烯(PTFE)、热塑性聚氨酯树脂(TPU)、聚酯、聚丙烯等。作为主基材的织物的实例包括例如机织织物或无纺织物、棉制品、聚酯、聚酰胺(尼龙)等。所述次级基材可以由任何适宜的材料制成，如机织织物或无纺织物、棉制品、聚酯、聚酰胺(尼龙)等。在层叠之前已经用防水材料处理过所述次级基材的暴露表面和其粘结表面这两者。所述暴露表面是暴露于环境(如潮湿环境)的表面，而所述粘结表面在形成层叠体时与所述主基材的带有粘合剂的表面接触。
根据本发明，“防水(water repellent)”可与术语“不透水(waterproof)”或“耐水(water resistant)”互换。
“环氧丙烷和环氧乙烷的共聚物”和“环氧丁烷和环氧乙烷的共聚物”是指聚合物链上的端基主要是环氧乙烷基团的那些聚合物。
另一方面，本发明的特征在于用热熔性湿固化聚氨酯粘合剂组合物制备防水层叠体的方法。所述粘合剂组合物包含热熔性异氰酸酯封端的聚氨酯预聚物，其暴露于周围湿分时是可湿固化的。
所述聚氨酯预聚物具有不大于约20,000g/mol、或者不大于约15,000g/mol、或者不大于约13,000g/mol、或者不小于约5,000g/mol、或者不小于8,000g/mol的重均分子量。
所述预聚物包含多元醇组分和多聚异氰酸酯组分的反应产物。在一种实施方案中，所述多元醇组分包含第一聚醚多元醇、第一聚酯多元醇和结晶聚酯多元醇。在另一实施方案中，该多元醇组分进一步包含无定形聚酯多元醇。在另一实施方案中，所述多元醇组分包含第一聚醚多元醇、第二聚醚多元醇和结晶聚酯多元醇。
有用的第一聚醚多元醇包括由选自环氧乙烷、环氧丙烷、1，2-环氧丁烷、1，4-环氧丁烷和其混合物的一种或多种单体形成的聚合物。该第一聚醚多元醇的数均分子量是约500～约8,000g/mol。在一种实施方案中，该第一聚醚多元醇包含数均分子量是约500～约4,000g/mol的环氧丙烷的均聚物。在另一实施方案中，该第一聚醚多元醇包含数均分子量是约500～约4,000g/mol的环氧丙烷和环氧乙烷的共聚物。在其它实施方案中，该第一聚醚多元醇包含环氧丙烷的均聚物、或环氧丁烷的均聚物、或环氧丙烷和环氧乙烷的共聚物、或环氧丁烷和环氧乙烷的共聚物、或其混合物。这些共聚物可以具有无规或嵌段构造和约1,000～约6,000g/mol的数均分子量。第一聚醚多元醇的存在量基于所述粘合剂组合物的总重量是约10wt％～约60wt％、或约20wt％～约50wt％。
有用的第二聚醚多元醇包括例如数均分子量不大于约1,000g/mol、或不小于约200g/mol的那些烷撑二醇。有用的烷撑二醇包括具有3个或更多碳原子的那些如丙二醇或丁二醇。市售第二聚醚多元醇的实例包括来自Dow Chemical Company的Voranol 220-260，或来自Arch Chemicals，Inc.的Poly-G 20-265。第二聚醚多元醇的存在量基于所述粘合剂组合物的总重量是不小于约5wt％、或不小于约10wt％、或不大于约30wt％、或不大于约20wt％。
第一和第二聚醚多元醇都是可从制造商获得的，如Huntsman Corp.(Houston，TX)；Texaco Chemical Co.(Bellaire，TX)；BASF Corp.(Charlotte，NC)；Arch Chemicals，Inc.(Stamford，CT)；Mazer Chemicals(Gurnee，IL)；Ashland Chemical Co.，Drew Division(Boonton，NJ)；Dow Chemical Co.(Midland，MI)；Witco Corp.(Houston，TX)；和Bayer Corp.(Pittsburgh，PA)。
有用的第一聚酯多元醇包括熔点小于约40℃的那些、和数均分子量约500～约6,000g/mol的那些。市售第一聚酯多元醇的实例包括来自BayerCorp.(Pittsburgh，PA)的Desmophen S 107-55，和来自Degussa Corp.(Piscataway，NJ)的Dynacoll 7250。第一聚酯多元醇的存在量基于所述粘合剂组合物的总重量是约5wt％～约50wt％、或约10wt％～约40wt％。
有用的结晶聚酯多元醇包括熔点约40℃～约120℃、玻璃化转变温度(Tg)不大于约0℃的那些。
所述结晶聚酯多元醇的实例包括己二醇或丁二醇与包括己二酸、十二烷二酸、癸二酸、对苯二甲酸或其混合物的酸的反应产物。在一些实施方案中，所述酸是癸二酸或己二酸。在一些实施方案中，所述结晶聚酯多元醇不含醚键，因为醚键可能降低该聚酯多元醇的结晶性。市售结晶聚酯多元醇的实例包括来自Degussa Corp.的Dynacoll
Figure 2006800181231_0
7360、7371、7380和7381。所述结晶多元醇的存在量基于所述粘合剂组合物的总重量是约l0wt％～约40wt％、或约15wt％～约30wt％。
有用的无定形聚酯多元醇包括数均分子量约500-约6,000g/mol的那些。市售无定形聚酯多元醇的实例包括来自Stepan Company(Northfield，IL)的Stepanpol PN-110。无定形聚酯多元醇的存在量基于所述粘合剂组合物的总重量是约5wt％～约20wt％。
所述多聚异氰酸酯组分包含具有两个或更多个异氰酸酯(-NCO)基团的多官能异氰酸酯化合物。那些多聚异氰酸酯化合物可以是脂族、芳族或其混合物。所述多聚异氰酸酯化合物还可以包含其它取代基，该取代基不会显著不利地影响所述预聚物的性能如异氰酸酯封端预聚物的粘度、或粘合层的粘结性能、或预聚物形成期间-NCO基团的反应性。有用的芳族多聚异氰酸酯的实例包括二苯基甲烷二异氰酸酯化合物类(MDI)，包括其异构体、碳二亚胺改性的MDI、二苯基甲烷4，4’-二异氰酸酯、二苯基甲烷-2，2’-二异氰酸酯、二苯基甲烷-2，4’-二异氰酸酯、和其他低聚亚甲基异氰酸酯；包括其异构体的甲苯二异氰酸酯化合物(TDI)；四甲基二甲苯二异氰酸酯(TMXDI)、萘二异氰酸酯的异构体、三苯基甲烷三异氰酸酯的异构体，和其混合物。有用的脂族多聚异氰酸酯的实例包括例如异佛尔酮二异氰酸酯、氢化的芳族二异氰酸酯、脂族多聚异氰酸酯和环脂族多聚异氰酸酯。其他有用的多聚异氰酸酯化合物在US 4,775,719、US 4,808,255和US 4,820,368中有述，其通过引用并入本文。市售多聚异氰酸酯化合物的实例包括可购自Dow Chemical Co.(Midland，MI)的Isonate
Figure 2006800181231_1
125M，它是纯的二苯基甲烷二异氰酸酯(MDI)。
在不会不利地影响其他物理性能如原始强度(green strength)或热稳定性的情况下，在所述预聚物的制备中可以任选地采用催化剂以提高固化速度。优选的催化剂包括醚和吗啉官能团，最优选2，2-二吗啉基乙基醚(2，2-dimorpholinoethyl ether)和二(2，6-二甲基吗啉基乙基)醚。市售催化剂的实例包括可购自Huntsman Corp.(Houston，TX)的JeffcatTM DMDEE(4，4’-(氧二-2，1-乙烷二基)双-吗啉)。所述催化剂的存在量基于所述粘合剂组合物的总重量是约0.01wt％-约2wt％。
任选地，还可以将稳定剂或抗氧化剂加入到所述粘合剂组合物中以保护该组合物免受由例如热、光或原料中的残留催化剂诱导的降解。市售抗氧化剂的实例包括可购自Ciba-Geigy(Hawthorne，NY)的Irganox
Figure 2006800181231_2
565、1010和1076，其都是受阻酚类抗氧化剂，以及来自Great Lakes Chemicals(West Lafayette，IN)的Anox
Figure 2006800181231_3
20，它也是受阻酚类抗氧化剂。充当自由基清除剂的这些抗氧化剂可以单独使用或与其他抗氧化剂组合使用，如亚磷酸酯类抗氧化剂，例如可购自Ciba-Geigy的Irgafos
Figure 2006800181231_4
168。其他抗氧化剂包括可购自Cytec Industries(Stamford，CT)的Cyanox
Figure 2006800181231_5
LTDP，硫醚抗氧化剂；以及可购自Albemarle(Baton Rouge，LA)的Ethanox
Figure 2006800181231_6
330，受阻酚类抗氧化剂。如果存在的话，所述抗氧化剂的量基于所述粘合剂组合物的总重量是至多约2wt％。
所述粘合剂组合物可以包含填料如滑石、粘土、二氧化硅及其经过处理的形式、炭黑和云母。市售填料的实例包括来自Luzenac America，Inc.(Englewood，Colo)的Mistron VaporTM滑石。
其他任选的成分包括紫外线(UV)清除剂或吸收剂、增添颜色的颜料、荧光剂、除味剂、粘合促进剂(即硅烷)、表面活性剂、消泡剂等等。通常，这些成分以基于所述粘合剂组合物的总重量通常小于约5wt％、或小于约2wt％的量少量加入。
可以通过使所述多元醇组分与所述多聚异氰酸酯组分在约40℃～约200℃的升高的温度下反应而制备所述粘合剂组合物。可以首先将所述多元醇组分引入反应容器中，加热至反应温度并干燥以除去被该多元醇吸收的环境湿分。然后将所述多聚异氰酸酯组分加入到该反应器中。在约0.75∶1.0～约0.15∶1.0的OH∶NCO比率下进行所述多元醇组分与多聚异氰酸酯组分之间的反应，从而获得在最终粘合剂中基于所述粘合剂组合物的总重量约1wt％～约5wt％的异氰酸酯含量。然后将所得粘合剂组合物装在合适的防潮容器中。
可以在施加后采用多种途径使所述粘合剂组合物固化。所述固化反应在具有可获得的活性氢原子的化合物与所述聚氨酯预聚物的NCO基团之间发生。多种具有游离活性氢的反应性化合物是本领域中已知的，包括水、硫化氢、多元醇、氨和其他活性化合物。可以依靠周围湿分进行这些固化反应，或者可以将所述活性化合物添加至所述粘合层处的组合物。当所述组合物与水反应时，形成脲基以提供聚氨酯脲聚合物。
所述粘合剂组合物具有90℃下小于约12,000cPs的粘度。在一些实施方案中，该粘合剂组合物具有90℃下约2,000cps～约8,000cps的粘度。在另外的实施方案中，该粘合剂组合物具有90℃下约3,000～约6,000cPs的粘度。施加温度因此可以是低的，约70℃～约110℃(158
Figure 2006800181231_7
～约230
Figure 2006800181231_8
)，或约80℃～约100℃(约175
Figure 2006800181231_9
～约212
Figure 2006800181231_10
)，或约80℃～约95℃(约175
Figure 2006800181231_11
～约200
Figure 2006800181231_12
)。
所得粘合剂组合物一般具有优异的原始强度，其指的是固化之前的粘合强度。所得组合物可以具有范围大概约30秒或更少至约30分钟的固化速率。该固化时间只涉及无粘性膜(tack free film)的形成。
施加方法可以包括槽膜涂布、辊涂、照相凹版式涂布、移膜涂饰、模型涂布(pattern coating)、丝网印刷、喷涂和长丝纺丝(filamentapplication)、挤出等。施加温度可以在约70℃-约110℃之间变化。基材对高温的敏感度可以决定可适用的施加温度。可以变化诸如所述组合物的粘度和固化速率等的物理特性以适应上述施加条件。
通过以下的非限制性实施例进一步说明本发明。除非另作说明，所有的份数、百分比、比率、量都是以重量计。
实施例
测试方法
熔体粘度
用27#转子在DV-1型Brookfield Thermosel粘度计上确定热熔性湿固化聚氨酯粘合剂组合物的熔体粘度。
分子量
通过凝胶渗透色谱(GPC)分子量分析测定热熔性湿固化聚氨酯预聚物的分子量。
粘附力
根据以下方法测试次级织物对主织物的粘附力。
将3”×6”的主织物放在工作台面上并在该片的一宽端上用带扎约1”。在施加温度下用金属涂敷器施加熔体形式的粘合剂。一旦施加所述粘合剂，就将在其两表面上已经用防水材料处理过的次级织物放在所述粘合剂层的上面。将隔离纸放在粘合的层叠体的上面以保护它。用辊对整个粘合的层叠体施加压力。此后，在环境温度和约50％相对湿度下保持该粘合的层叠体约7天以使所述粘合剂固化。为了测试粘附力，手动剥离该粘合的层叠体，并观察次级织物上的粘附力和以1至5进行评价等级。等级越高，粘附力越强。
实施例1-3和比较例1-2
通过使表I中的成分反应制成实施例1-3和比较例1-2中的各个热熔性湿固化聚氨酯粘合剂组合物。
根据所述粘附力测试方法测试所得的粘合剂组合物并在表II中列出结果。
表I
    成分     成分说明   实施例1 实施例2 实施例3 比较例1 比较例2
 Poly-G 20-112 第一聚醚多元醇   31.6 22.8
 Poly-G 20-265 第二聚醚多元醇     19
 Poly-G 55-56 第一聚醚多元醇     20     12
 Acclaim 4220N 第一聚醚多元醇     20
 DesmophenS-107-55 第一聚酯多元醇     20   22.8
 DesmophenS-105-36 结晶聚酯多元醇   34.2
 DesmophenS-105-22 结晶聚酯多元醇     15     5
 DesmophenS-1028-55 第一聚酯多元醇     30.5
 Dynacoll 7210 第一聚酯多元醇     44
  Dynacoll7361   结晶聚酯多元醇     15     16
  Dynacoll7340   结晶聚酯多元醇     10
  DynacollX7371   结晶聚酯多元醇     10
  StepanpolPN-110   无定形聚酯多元醇     10     20
  StepanpolPHN-56   无定形聚酯多元醇     12
  Pearlbond 503   热塑性聚氨酯     4
  BNX 1010   抗氧化剂     0.46     0.46
  Unitex OB   UV稳定剂     0.01     0.01     0.01     0.01
  Jeffcat DMDEE   催化剂     0.03     0.03     0.03
  Irganox 1010   抗氧化剂     0.29
  Isonate 125M   异氰酸酯     22.9     20.17     24.5     13.7     21.5
  Mistron Vapor   滑石     1     0.99
  预聚物的重均分子量     10,600     12,700     11,800     25,000
表II粘附力
DWR*层叠体#1  DWR层叠体#2   DWR层叠体#3
  实施例1     4     4     4
  实施例2     4     4     4
  实施例3     4     4     4
  比较例1     0     0     0
  比较例2     0     0     1
*DWR：持久防水

Claims (10)

1.一种制备防水层叠体的方法，所述层叠体包含具有第一表面和第二表面的主基材和具有粘结表面和暴露表面的次级基材，所述次级基材的所述粘结表面和暴露表面已经用防水材料处理过，所述方法包括：
a)将热熔性湿固化聚氨酯粘合剂组合物施加在所述主基材的所述第一表面上以形成带有粘合剂的表面；和
b)使所述主基材的所述带有粘合剂的表面与所述次级基材的所述粘结表面粘结以形成层叠体，
其中所述粘合剂组合物在90℃的粘度小于12000cps并且包含重均分子量不大于20,000g/mol的热熔性湿固化聚氨酯预聚物，所述预聚物是多元醇组分和多聚异氰酸酯组分的反应产物，所述多元醇组分包含由选自环氧乙烷、环氧丙烷、1，2-环氧丁烷、1，4-环氧丁烷或其混合物的至少一种单体形成的第一聚醚多元醇；熔点小于40℃的第一聚酯多元醇；和熔点为40℃～120℃，玻璃化转变温度Tg不大于0℃的结晶聚酯多元醇。
2.权利要求1的方法，其中所述多元醇组分进一步包含数均分子量500g/mol～6,000g/mol的无定形聚酯多元醇。
3.权利要求1或2的方法，其中所述第一聚醚多元醇是环氧丙烷的均聚物或者环氧丙烷和环氧乙烷的共聚物；所述第一聚醚多元醇具有500g/mol～4,000g/mol的数均分子量。
4.权利要求1或2的方法，其中所述多聚异氰酸酯组分是二苯基甲烷-4，4’-二异氰酸酯。
5.权利要求1或2的方法，其中所述粘合剂组合物具有90℃下2,000cps～8,000cps的粘度。
6.权利要求1或2的方法，其中所述主基材是选自聚四氟乙烯(PTFE)、热塑性聚氨酯树脂(TPU)、聚酯或聚丙烯的热塑性膜。
7.权利要求1或2的方法，其中所述次级基材包含机织织物或无纺织物、棉制品、聚酯或聚酰胺。
8.权利要求1或2的方法，其中所述层叠体显示出耐洗性。
9.由权利要求1-8中任一项的方法制成的层叠体。
10.包含权利要求9的层叠体的服装。
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