CN101248230B - 改善的湿气调节复合材料 - Google Patents

改善的湿气调节复合材料 Download PDF

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CN101248230B
CN101248230B CN2006800306631A CN200680030663A CN101248230B CN 101248230 B CN101248230 B CN 101248230B CN 2006800306631 A CN2006800306631 A CN 2006800306631A CN 200680030663 A CN200680030663 A CN 200680030663A CN 101248230 B CN101248230 B CN 101248230B
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M·赫利希-洛斯
C·海因德尔
S·钱普
M·贝克
M·腾内森
M·法斯特内尔
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Abstract

本发明涉及改善的包含片状基材、水溶性吸湿物质和在吸湿物质的存在下聚合在基材上并可通过包含至少一种烯属不饱和单体i)和基于100重量份单体i)至少6重量份交联剂iii)的单体溶液聚合而得到的吸水性聚合物的湿气调节复合材料，它们的制备方法和它们在湿气调节中的用途。

Description

改善的湿气调节复合材料
本发明涉及改善的湿气调节复合材料，制备它们的方法及其在湿气调节中的用途。 
本发明的其他实施方案可由权利要求、说明书部分和实施例中看出。应当理解不偏离本发明的范围上文提到的和将在下文更特别描述的本发明的主题特征不仅可应用于所指出的具体组合，也可应用于其他组合。 
吸水性聚合物尤其为(共)聚合的亲水性单体的聚合物，一种或多种亲水性单体在适合的接枝基上的接枝(共)聚合物，纤维素或淀粉的交联醚，交联的羧甲基纤维素，部分交联的聚氧化烯或可溶胀于含水流体的天然产物例如瓜耳胶衍生物。这种聚合物作为可吸收水溶液的产物用于生产尿布、棉塞、卫生巾或其他卫生制品，还作为保水剂用于商品蔬菜种植业。 
生产吸水性聚合物的现有技术例如概括于专论“ModernSuperabsorbent Polymer Technology”，F.L.Buchholz and A.T.Graham，Wiley-VCH，1998，第69-117页中。 
WO 01/56625，EP-A-1178149和US-5,962,068描述了生产吸水性复合材料的方法，每种方法中将吸水性聚合物聚合在基材上。 
WO 00/64311公开了吸水性聚合物聚合在基材上的复合材料。复合材料用于座垫中湿气调节。WO 2004/067826A1教导了多层织物，尤其是由缝编在一面上的无纺织物构成的那些，其可例如包含活性组分如吸水性聚合物。 
JP-A 05-105705描述了由基材和吸湿盐组成的不潮解干燥剂，其中吸湿盐借助吸水性聚合物而固定在基材上。 
现有德国专利申请DE 102005015536.7描述了包含至少一种片状基材、至少一种水溶性吸湿物质和至少一种在水溶性吸湿物质的存在下聚合在基材上的吸水性聚合物的湿气调节复合材料。 
现有的湿气调节复合材料常常相对刚性并且其中吸水性聚合物的粒子 相对硬。此刚性可在进一步加工和复合材料的使用中产生困难，并且不利地影响复合材料的悬垂性。另外，其中通常用于避免蒸发相关的不愉悦效应的这种湿气调节复合材料开始与比通常通过蒸发产生的更大量的液体接触，例如当液体溢出用这种复合材料装备的座椅家具或汽车座椅时，可出现不想要的不匀性，花费比湿气调节复合材料的常规干燥更长的时间通过干燥再次消失。 
本发明的目的是提供能可逆地吸收大量水蒸气而与大量液体接触时不形成不想要的不匀性的湿气调节复合材料。 
我们发现该目的通过包含如下组分的湿气调节复合材料实现： 
a)至少一种片状基材， 
b)至少一种水溶性吸湿物质，和 
c)在所述物质b)的存在下聚合在所述基材a)上并可通过包含至少一种烯属不饱和单体i)和基于100重量份单体i)至少6重量份交联剂iii)的单体溶液聚合而得到的至少一种吸水性聚合物， 
其中所述吸湿物质b)与所述聚合物c)之重量比为0.01-1。 
吸湿物质b)与聚合物c)之比优选小于0.8，更优选小于0.6，甚至更优选小于0.5，最优选小于0.4且为至少0.05，更优选至少0.1，甚至更优选至少0.15。 
基材a)不受任何限制。优选的基材为如WO 01/56625在第16页第40行至第20页第27行所述机织织物和/或无纺织物，或如WO 2004/067826所公开的包含机织织物和无纺织物的混合形式。 
适合的基材a)例如为包含合成聚合纤维的机织织物或无纺织物。纤维可由任何可纺的聚合材料制成，其中聚合材料的实例为聚烯烃如聚乙烯或聚丙烯、聚酯如聚对苯二甲酸乙二酯、聚酰胺如尼龙-6或尼龙-6.6、聚丙烯酸酯、改性纤维素如乙酸纤维素。也可使用上述聚合材料的混合物。 
机织织物为由交叉纤维，优选相交成直角的纤维组成的制品。 
无纺织物为包含纤维且其完全性通常归因于纤维的固有紧贴感的无纺制品。无纺织物优选例如通过针刺、相互成圈(nterlooping)或借助水或空气的锐利喷射缠结而机械固结(consolidate)。无纺织物也可粘着或内聚固  结。粘着固结的无纺织物可例如通过纤维与液体粘合剂相互粘着或通过熔融在它的生产期间加入无纺织物中的粘合纤维而得到。内聚固结的无纺织物例如通过起初用适合的化学品溶解纤维并施加压力而得到。 
基材的定量便利地为20-800g/m2，优选50-600g/m2，更优选100-500g/m2。 
吸湿物质b)能吸收水蒸气；即来自空气的水蒸气冷凝在吸湿物质上，导致吸湿物质b)的含水量增加。吸湿物质b)例如为无机盐如氯化钠、硝酸铅、硫酸锌、高氯酸钠、氧化铬或氯化锂，或至少部分结晶的有机化合物如水溶性聚丙烯酸。吸湿无机盐为优选的吸湿物质b)。最优选氯化钠。 
特别有利的吸湿物质b)为在20℃下平衡的饱和水溶液以上相对湿度小于95％，优选小于90％，更优选小于85％，甚至更优选小于80％且为至少40％，优选至少45％，更优选至少50％，甚至更优选至少55％，最优选至少60％的化合物。 
相对湿度为水蒸气压力与水蒸气压力的商乘以100％。 
优选吸湿物质b)在聚合在其上的吸水性聚合物中为支付(disbursed)状态。 
当本发明湿气调节复合材料例如用于座垫时，90％以上的相对湿度感觉不愉悦，这是由于在高大气湿度下有利于汗的形成。然而，40％以下的相对湿度也不利，这是由于这种低相对湿度对于进一步增强座椅舒适毫无用处。 
本发明湿气调节复合材料可通过使施用在基材上并聚合的包含如下组分的单体溶液聚合而得到： 
i)至少一种烯属不饱和单体， 
ii)至少一种水溶性吸湿物质， 
iii)基于100重量份单体i)，至少6重量份交联剂， 
iv)如果合适的话，一种或多种可与i)下提到的单体共聚的烯属和/或烯丙属不饱和单体，和 
v)如果合适的话，一种或多种水溶性聚合物， 
其中所述吸湿物质ii)与所述单体i)的重量比为0.01-1。 
吸湿物质ii)与单体i)的重量比优选至多，尤其是小于0.8，更优选至多，尤其是小于0.6，甚至更优选至多，尤其是小于0.5，最优选至多，尤其是小于0.4且为至少0.05，更优选至少0.1，甚至更优选至少0.15。 
适合的单体i)例如为烯属不饱和羧酸，如丙烯酸、甲基丙烯酸、马来酸、富马酸和衣康酸，或其衍生物，如丙烯酰胺、甲基丙烯酰胺、丙烯酸酯和甲基丙烯酸酯。优选包含酸性基团的单体i)。丙烯酸和甲基丙烯酸为特别优选的单体。最优选丙烯酸。 
单体i)，尤其是丙烯酸包含优选至多0.025重量％的量的氢醌半醚。优选的氢醌半醚为氢醌单甲基醚(MEHQ)和/或生育酚。 
生育酚指如下通式的化合物： 
Figure S2006800306631D00041
其中R1为氢或甲基，R2为氢或甲基，R3为氢或甲基，R4为氢或具有1-20个碳原子的酸基。 
优选的基团R4为乙酰基、抗坏血酸基、琥珀酰基、烟酰基和其他生理上可相容的羧酸。羧酸可以为单羧酸、二羧酸或三羧酸。 
优选其中R1＝R2＝R3＝甲基的α-生育酚，尤其是外消旋α-生育酚。R4 更优选氢或乙酰基，尤其优选RRR-α-生育酚。 
单体溶液的氢醌半醚含量优选不大于130重量ppm，更优选不大于70重量ppm，优选至少10重量ppm，更优选至少30重量ppm，特别优选50重量ppm左右，全部基于丙烯酸，其中丙烯酸盐作为丙烯酸计算。例如，单体溶液可使用具有适合的氢醌半醚含量的丙烯酸制备。 
用于本发明方法的有用吸湿物质ii)已作为吸湿物质b)描述。 
吸水性聚合物为交联状态，即聚合在具有至少两个可自由基共聚入聚合物网络的可聚合基团的化合物(“交联剂”)的存在下进行，使得产生的聚合物当然以共聚形式包含交联剂的相应片断。有用的交联剂iii)例如包括  如EP-A 530 438所述的二甲基丙烯酸乙二醇酯、二丙烯酸二甘醇酯、甲基丙烯酸烯丙酯、三羟甲基丙烷三丙烯酸酯、三烯丙基胺、四烯丙氧基乙烷，如EP-A 547 847、EP-A 559 476、EP-A 632 068、WO93/21237、WO03/104299、WO 03/104300、WO 03/104301和DE-A 10331450所述的二丙烯酸酯和三丙烯酸酯，如DE-A 10331456.3和现有德国专利申请10355401.7所述的不仅包含丙烯酸酯基团还包含其他烯属不饱和基团的混合丙烯酸酯或如DE-A-195 43 368、DE-A-196 46 484、WO90/15830和WO 02/32962所述的交联剂混合物。 
有用的交联剂iii)尤其包括N，N’-亚甲基双丙烯酰胺和N，N’-亚甲基双甲基丙烯酰胺，多元醇的不饱和一元羧酸或多元羧酸的酯如二丙烯酸酯或三丙烯酸酯，例如二丙烯酸丁二醇酯、二甲基丙烯酸丁二醇酯、二丙烯酸乙二醇酯、二甲基丙烯酸乙二醇酯以及三羟甲基丙烷三丙烯酸酯和烯丙基化合物如(甲基)丙烯酸烯丙酯、氰尿酸三烯丙酯、马来酸二烯丙酯、聚烯丙酯、四烯丙氧基乙烷、三烯丙基胺、四烯丙基乙二胺、磷酸的烯丙酯以及乙烯基膦酸衍生物，例如如EP-A 343 427所述。有用的交联剂iii)另外包括季戊四醇二烯丙基醚、季戊四醇三烯丙基醚、季戊四醇四烯丙基醚、聚乙二醇二烯丙基醚、乙二醇二烯丙基醚、甘油二烯丙基醚、甘油三烯丙基醚、基于山梨糖醇的聚烯丙基醚，及其乙氧基化变体。本发明方法可使用聚乙二醇的二(甲基)丙烯酸酯，所用的聚乙二醇分子量为300-1000。 
然而，特别有利的交联剂iii)为3-20重乙氧基化甘油的二丙烯酸酯和三丙烯酸酯，3-20重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯，3-20重乙氧基化三羟甲基乙烷的二丙烯酸酯和三丙烯酸酯，尤其是2-6重乙氧基化甘油或2-6重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯，3重丙氧基化甘油的二丙烯酸酯和三丙烯酸酯，或3重丙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯以及3重混合的乙氧基化或丙氧基化甘油的二丙烯酸酯和三丙烯酸酯，或3重混合的乙氧基化或丙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯，15重乙氧基化甘油的二丙烯酸酯和三丙烯酸酯，15重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯，至少40重乙氧基化甘油的二丙烯酸酯和三丙烯酸酯，至少40重乙氧基化三羟甲基  乙烷的二丙烯酸酯和三丙烯酸酯或至少40重乙氧基化三羟甲基丙烷的二丙烯酸酯和三丙烯酸酯。 
非常特别优选的交联剂iii)为二丙烯酸酯化、二甲基丙烯酸酯化、三丙烯酸酯化或三甲基丙烯酸酯化的多重乙氧基化和/或丙氧基化甘油，例如如WO 03/104 301所述。3-10重乙氧基化甘油的二丙烯酸酯和/或三丙烯酸酯特别有利。非常特别优选1-5重乙氧基化和/或丙氧基化甘油的二丙烯酸酯或三丙烯酸酯。最优选3-5重乙氧基化和/或丙氧基化甘油的三丙烯酸酯。这些的显著之处在于在吸水性聚合物中特别低的残留水平(通常为10重量ppm以下)和用其制备的吸水性聚合物的含水提取物具有与相同温度下的水相比几乎不变的表面张力(通常不小于0.068N/m)。 
根据本发明，交联剂以至少6重量份，优选至少7重量份，更优选至少8重量份，最优选至少9重量份的量包括在单体溶液中，所有基于100重量份单体i)。单体中交联剂含量的上限不太关键，通常使用不大于25重量份，优选不大于20重量份，更优选不大于18重量份的交联剂含量。适合的交联剂含量的实例为基于100重量份单体i)至少10重量份，至少10.5重量份，至少11重量份，至少11.5重量份，至少12重量份，至少12.5重量份，至少13重量份。 
可与单体i)共聚的烯属不饱和单体iv)的实例为丙烯酰胺、甲基丙烯酰胺、巴豆酰胺、甲基丙烯酸二甲基氨基乙酯、丙烯酸二甲基氨基乙酯、丙烯酸二甲基氨基丙酯、丙烯酸二乙基氨基丙酯、丙烯酸二甲基氨基丁酯、甲基丙烯酸二甲基氨基乙酯、甲基丙烯酸二乙基氨基乙酯、丙烯酸二甲基氨基新戊酯和甲基丙烯酸二甲基氨基新戊酯。 
有用的水溶性聚合物v)包括聚乙烯醇、聚乙烯基吡咯烷酮、淀粉、淀粉衍生物、聚乙二醇或聚丙烯酸，优选聚乙烯醇和淀粉。 
吸湿聚合物如可溶聚丙烯酸不仅可用作吸湿物质ii)，也可用作水溶性聚合物v)。 
当将常规接枝聚合催化剂如铁盐加入单体溶液中时，则聚合物将用作聚合的接枝基并且待聚合单体将接枝于聚合物上。当不使用接枝聚合催化剂时，则聚合物将以基本上未改变的状态继续存在于聚合中并充当吸湿物  质。 
优选的单体i)的酸基通常为部分中和状态，它们的中和度优选25-95摩尔％，更优选40-90摩尔％，甚至更优选50-80摩尔％，最优选60-80摩尔％。可使用常规中和剂，优选碱金属氢氧化物、碱金属氧化物、碱金属碳酸盐或碱金属碳酸氢盐及其混合物。也可使用铵盐代替碱金属盐。特别优选钠和钾作为碱金属，但最优选氢氧化钠、碳酸钠或碳酸氢钠及其混合物。通常，中和通过将中和剂作为水溶液、作为熔体或优选作为固体混入而实现。例如含水量明显在50重量％以下的氢氧化钠可作为熔点在23℃之上的蜡状块存在。在这种情况下，可作为块(piece)或熔体在升高的温度下计量加入。 
单体水溶液优选通过喷雾应用于基材上。有用的基材已作为基材a)描述。 
随后，使基材上的单体溶液聚合并将复合材料干燥。聚合优选通过UV辐射和/或热引发。按照常规，对于这种聚合反应，引发剂可用于促进或控制聚合反应的起动；这里，可以以常规方式使用任何已知的引发剂或引发剂体系。 
在本发明优选实施方案中，聚合物c)包含至少一种在聚合之前包括在单体溶液中并保留在聚合物中的增塑剂。其中增塑剂应理解为意指以所用的量降低聚合物c)的玻璃化转变温度的物质。所用增塑剂的量将使聚合物的玻璃化转变温度降低至少2℃，优选至少4℃，更优选至少6℃，最优选至少10℃。例如，以将使聚合物的玻璃化转变温度降低至少20℃或至少30℃的量包括增塑剂。玻璃化转变温度为聚合物的已知性能并可通过ASTM E1356-03“Standard Test Method for Assignment of the GlassTransition Temperatures by Differential Scanning Calorimetry”或同等ISO11357-2标准测量。 
常规增塑剂在室温下为液体，并且也为聚合物的溶剂或分散剂。当聚合物通过单体的UV辐射而制备时，则必须选择对于UV光充分稳定且还不干扰UV引发聚合的增塑剂。优选，增塑剂为亲水性并可以以任何比例与水溶混。适合的增塑剂的实例为醇，多元醇如甘油和山梨糖醇，二醇和  醚二醇如聚亚烷基二醇的单醚和二醚、聚亚烷基二醇的单酯或二酯、聚乙二醇、聚丙二醇、混合聚乙二醇或聚丙二醇、甘醇酸酯、甘油、脱水山梨糖醇酯、柠檬酸酯或酒石酸酯或咪唑啉衍生的两性表面活性剂。优选的增塑剂为多元醇如甘油和山梨糖醇、聚乙二醇及其混合物。特别优选甘油。 
有用的增塑剂另外包括烃和烃混合物如白油，尤其是药用白油或液体石蜡。 
通常以足以实现所需玻璃化转变温度的降低的量包括增塑剂。通常的增塑剂含量基于100重量份单体i)为5-50重量份，优选8-40重量份，尤其是10-30重量份增塑剂。 
本发明复合材料对于湿气调节，尤其是在褥垫和座垫中，例如汽车座椅中非常有用。 
包含本发明复合材料的座垫或褥垫通过将相对大气湿度调整至令人愉悦的水平并防止出汗过度而增强坐或躺的舒适。同时，本发明复合材料能在不使用时期再次最佳释放吸收的湿气且能自身快速再生。由于这种平衡的性能特征，本发明复合材料提供至今未达到的坐或躺的舒适。 
方法 
吸收湿气的测定 
将复合材料在23℃和50％的相对湿度下调整60分钟直至平衡。然后使相对湿度上升至90％，并将复合材料在30℃下保持90分钟(吸收阶段)。其后，将相对湿度降低至40％，并将试样在40℃下保持100分钟(解吸阶段)。 
连续测量由于吸/解吸的重量变化并作为基于g施用物质(吸水性聚合物和/或盐)的重量增加。重量增加的参比点为60分钟平衡后的重量。 
实施例 
实施例1 
在通过UV辐射固化2分钟之前，将定量为70g/m2的聚对苯二甲酸乙二酯无纺织物用单体溶液喷雾。这之后在90℃下在逆流干燥机中干燥5分钟。 
单体溶液包含19599g37.重量％丙烯酸钠水溶液(相当于整个单体溶  液中24.5重量％丙烯酸钠)、435g丙烯酸(8.5重量％)、900g聚乙二醇二丙烯酸酯(平均摩尔质量为400的聚乙二醇的二丙烯酸酯)(3重量％)作为交联剂、66g2-羟基-1-[4-(羟基乙氧基)苯基]-2-甲基-1-丙酮(0.22重量％)作为引发剂、1500g甘油(5重量％)和7500g25重量％氯化钠水溶液(6.25重量％NaCl)。 
单体溶液的量的选择使得具有聚合在其上的吸水性聚合物的聚对苯二甲酸乙二酯无纺织物的负载为160g/m2。 

Claims (10)

1.一种包含如下组分的湿气调节复合材料：
a)至少一种片状基材，
b)至少一种水溶性吸湿物质，和
c)在所述物质b)的存在下聚合在所述基材a)上并可通过包含至少一种烯属不饱和单体i)和基于100重量份单体i)至少6重量份交联剂iii)的单体溶液聚合而得到的至少一种吸水性聚合物，
其中所述吸湿物质b)与所述聚合物c)之重量比为0.01-1，
其中所述吸湿物质b)为氯化钠。
2.根据权利要求1的复合材料，其中所述基材a)为机织织物和/或无纺织物。
3.根据权利要求1或2的复合材料，其中所述聚合物c)包含酸性基团。
4.根据权利要求3的复合材料，其中所述酸性基团至少25摩尔％被中和。
5.一种生产湿气调节复合材料的方法，其包括将包含如下组分的单体溶液施用在片状基材上并聚合：
i)至少一种烯属不饱和单体，
ii)至少一种水溶性吸湿物质，
iii)基于100重量份单体i)，至少6重量份交联剂，
iv)任选，一种或多种可与i)下提到的单体共聚的烯属和/或烯丙属不饱和单体，和
v)任选，一种或多种水溶性聚合物，
其中所述吸湿物质ii)与所述单体i)的重量比为0.01-1，
其中所述吸湿物质ii)为氯化钠。
6.根据权利要求5的方法，其中所述单体i)包含酸性基团。
7.根据权利要求6的方法，其中所述酸性基团至少25摩尔％被中和。
8.根据权利要求5-7中任一项的方法，其中所述基材为机织织物和/或无纺织物。
9.根据权利要求1-4中任一项的复合材料在湿气调节中的用途。
10.包含根据权利要求1-4中任一项的复合材料的座垫或褥垫。
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