CN1070924A - 亲水性处理吸收泡沫材料的方法 - Google Patents
亲水性处理吸收泡沫材料的方法 Download PDFInfo
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Abstract
将通常的疏水性泡沫塑料,例如聚氨酯泡沫塑料
和油包水乳状液聚合的泡沫塑料通过用简单的表面
活性剂和亲水试剂盐进行处理使之成为亲水性的。
这种含表面活性剂的泡沫塑料用一种,例如氯化钙的
溶液进行处理,然后进行干燥,在含有表面活性剂的
内泡沫表面留下大体均匀分布的水合的或可水合的
氯化钙残余物。在使用中,表面活性剂和氯化钙水合
物的结合为泡沫塑料提供了亲水表面。其它可水合
的钙或镁盐也可以使用。所得的亲水泡沫塑料适用
于吸收部件,包括婴儿尿布,妇女卫生纸,绷带,等
等。
Description
本发明涉及一种将通常的疏水聚合物泡沫塑料转换为亲水泡沫塑料的方法。经过这样“亲水性”处理的泡沫适合用于各种有吸收力的部件中,如婴儿尿布,大小便失禁的成年人的外套,妇女卫生纸,绷带,等等,这些泡沫塑料尤其适用于吸收各种人体水性流体。
在商品化实践中已熟知大量能有效吸收水分的泡沫材料,或普通“海绵”。尤其是这类泡沫为开孔结构并含有各种纤维素或聚合物材料。例如,各种聚氨酯及类似材料已长期被用来制备合成泡沫塑料。如现有技术已知,泡沫材料的功能是当其表面实质上亲水时就能最有效地吸收水性液体。然而,许多合成泡沫是通过能产生聚合物泡沫的有机单体聚合而制备的,这些泡沫的性质实质上是疏水的。因此人们已付出相当大的关注以寻求能将疏水合成泡沫塑料变成亲水性的方法。
例如,已知某些类型的泡沫,它们是用某些特定选择的单体制备的,这些单体本身至少赋予所形成的聚合泡沫一定程度的亲水特性。于是这类单体在聚合过程中就掺入到泡沫网状结构的基本结构中。遗憾的是,单体中存在的亲水取代基不能称心合意地改进所得泡沫的基本特性。因此,当所得的泡沫可能具有所希望的亲水特性时,它可能失去某些其它所希望的结构性能或性能特性。此外,这种特指的亲水单体比用于制取泡沫的标准单体贵,因此其使用就增加了泡沫的整个成本。
在其它方法中,将某些泡沫进行处理以在其聚合物结构中提供阴离子取代基(例如羧酸盐或磺酸盐)部分。这种阴离子取代基对泡沫表面的亲水性处理是有效的,但遗憾的是,使用它们会导致泡沫相当坚硬且缺少弹性。这种泡沫当用于与人体皮肤紧密接触时,如用于婴儿尿布和妇女卫生纸时是极不舒适的。
在某些情况下,在泡沫基体中掺入少量表面活性剂可使合成疏水性泡沫表现亲水性。尽管这可使泡沫变得亲水而且对于某些用途极为有用,然而会有表面活性剂的泡沫不总是适用于长期与皮肤接触,因为表面活性剂可引起皮肤刺激。另外,某些表面活性剂,例如水溶性表面活性剂会从泡沫中放出并溶于被泡沫吸收的流体中。这将明显改变流体的表面张力并显著影响泡沫固着其的强度。
制造用于流体吸收的卫生制品(尤其是可随意使用的婴儿尿布和妇女卫生纸)的亲水性泡沫要求该泡沫不仅具有优良的流体处理性能,还要使其在长期与人体皮肤紧密贴紧的穿着使用中对穿戴者舒适和安全。另外对于设计用在尿布和月经纸中的泡沫的性能也是重要的,即当某些表面活性剂,例如水溶性表面活性剂,被用于亲水的吸收泡沫时,可能会发生人体流体(如尿和月经)的流动性实质是不受亲水试剂的影响。因此,使吸收泡沫安全、有效、经济的亲水化方式实质上对制造这种产品是重要的。本发明提供了一种安全有效的泡沫亲水性处理方法以满足上述要求。
Lindquist的美国专利3563243(1971年2月16日颁发)涉及到把氧化烯取代的聚氨酯泡沫塑料用于婴儿尿布。也可参见1990年9月21日公开的日本专利未决申请02-239863(Kao)。
Jones等人的美国专利4612334(1986年9月16日颁发)和Haq等人的美国专利4606958(1986年8月19日颁发)都涉及了某些带有羧基和其它阴离子基的泡沫。
Unilever的欧洲专利申请299762(1989年1月18日公布)涉及了在制造高内相乳剂泡沫时使用氯化钙。
Kelly等人的美国专利4985467(1991年1月15日颁发)揭示了一种亲水性聚氨酯泡沫,它含有超吸收能力的材料。该专利也列举了涉及吸收泡沫和/或其它吸收材料的以下参考文献:美国专利4104435;4717738;4725629;4076663;4454268;4337181;4133784;3669103;4464428;4394930;3900030;4239043;4731391和日本55-168104(1982);57-92032(1982);还有美国专利3021290;3171820;3175025;4359558和4521544。
Barby等人的美国专利4797310(1989年1月10日颁发);Edwards等人的美国专利4788225(1988年11月29日颁发);和Barby等人的美国专利4522953(1985年6月11日颁发)都涉及了多孔聚合物材料(泡沫),其中一些材料的特定表面活性剂以及某些材料可能是亲水的。
本发明涉及了一种使实质上疏水聚合物泡沫塑料变成适于吸收亲水性液体的方法。在该方法的第一步,将某种类型的表面活性剂和由水这样的溶剂与某种类型的亲水试剂盐形成的溶液一起掺入聚合物泡沫材料中去,该聚合物泡沫材料在没有加入的或没有残留的亲水试剂时实质上是疏水的。在该方法的第二步,将此经处理的聚合物泡沫材料干燥除去溶剂,并因此留下掺在泡沫材料内的大体均匀分布的,具有一定亲水量的表面活性剂和亲水试剂盐。所用表面活性剂是一种大体上水不溶性物质,且是柔和的对皮肤相对无刺激。在本方法中主要使用的特殊亲水性试剂盐是毒性可接受的,水合的或可水合的钙和镁盐例如氯化钙和氯化镁。
本发明也指示了一些亲水性处理的聚合物发泡材料,它们本身就适于吸收亲水性液体。这种泡沫塑料具有以上提及的大体均匀分布的掺入的表面活性剂和亲水性试剂盐,所含亲水量至少为泡沫重量的0.05%。这种泡沫塑料进一步含有不多于泡沫重量大约50%的游离子水。
图1是本发明的一种典型亲水吸收泡沫塑料的间隙的显微照片。
图2是一婴儿尿布结构的部件分解图,其中有一双层吸收芯结构,并且使用了一亲水吸收泡沫塑料作为其一个元件。
本发明的亲水性处理方法涉及聚合物泡沫材料的处理,该材料适于将液体吸收到其泡沫结构中。聚合物泡沫塑料通常可以称为这样一种结构,当将一种相对无单体的气体或相对无单体的液体作为气泡分散在可聚合的含单体液体中,接着将可聚合单体在包住气泡的含单体液体中聚合,就形成这种结构。所得的聚合的分散体可以是泡沫聚集体的多孔固化结构形式,这些泡孔的界面或壁含有固态聚合材料。泡孔本身含有相对无单体的气体或相对无单体的液体,其在聚合前已在液体分散体中形成“气泡”。
如后面更详细所述,优选用在本发明中的聚合物泡沫材料是由特殊类型油包水乳状液聚合而制备的那些泡沫材料。这种乳状液是由相当少量的可聚合含单体油相和相当大量相对无单体水相形成的。相对无单体的非连续内水相因此形成由连续的可聚合含单体油相包围的分散的“气泡”。接着在连续油相中的单体聚合形成微孔泡沫结构。在聚合时形成的留在泡沫结构中的水性液体可通过加压和/或干燥泡沫而除去。
用在本发明中的特别优选的聚合物泡沫材料是由油包水乳状液(在该乳状液油相中含有某些可聚合的单体,如苯乙烯,烷基(甲)丙烯酸酯和/或二乙烯基苯)聚合制成的那些材料。这种类型最优选的聚合物泡沫材料是由Desmarais,Stone,Thompson,Young,LaVon,和Dyer同时申请的美国专利申请,序号_(P&G Case 4451),中所叙述的那些材料,该申请的名称为“用于含水体液的具有吸收能力的泡沫材料和含有这种材料的具有吸收能力的制品”,该申请在此引作参考。这种特别优选的泡沫材料通常具有的微孔体积从约12至100ml/g以及毛细空吸比表面积从约0.5-5.0m2/g。这些泡沫塑料可用油包水乳状液制备,其中水对油的重量比范围从约12∶1至100∶1,优选20∶1至70∶1。
另一种用于本发明的普通类型聚合物泡沫材料含有聚氨酯。聚氨酯泡沫塑料是由多异氰酸酯如二异氰酸酯与含羟基材料如聚醚多醇在有水和催化剂存在下经反应而制成的那些泡沫材料。当聚合物形成时,水与异氰酸酯基反应产生交联,并形成二氧化碳,产生发泡。三氟甲烷或其它挥发性材料也可用作发泡剂。
聚合物泡沫塑料(包括此处优选的由油包水乳状液聚合制备的泡沫塑料)在性质上可以是相对闭孔的或相对开孔的,这取决于泡孔壁或界面,即孔窗是否和/或多少被聚合物材料填充或卷起。用于本发明方法中的聚合物泡沫材料是相对开孔的泡沫材料,其中泡沫塑料的各个泡孔大部分没有被泡壁的聚合物材料彼此完全分隔开。因此在这种大体开孔的泡沫结构中的泡孔具有内微孔开口或“窗口”,它们都足够大以便于流体在泡沫结构内从一个泡孔移到另一个泡孔。
在此处所用的大体开孔型结构中,泡沫塑料通常具有网状特征,各个泡孔由许多相互联结的,三维尺寸分支的边限定。形成开孔泡沫结构分支边的聚合物材料股可以被称作“支柱”。具有代表性的支柱型结构的开孔泡沫塑料已例示于图1中的显微照片。作为本发明的目的,在泡沫结构中若至少80%的泡孔与至少一个相邻泡孔是流体联通的,该泡沫材料就是“开孔”的。
形成泡沫塑料的聚合物材料在本发明的方法中用作原材料,它在水性流体中通常是不膨胀的,而且在其聚合物结构中通常大体上没有极性官能基团。这样在这种泡沫的结构形成后,泡沫结构表面就会有这样一种聚合物材料,它在没有任何残留的或加入的表面活性剂或其它亲水试剂时,其性质大体上是疏水的。
聚合物泡沫材料是“疏水的”还是“亲水的”,此程度可通过此泡沫塑料与一种吸收测试液体接触时所呈现的“粘合张力”从而参考确定。粘合张力由下式确定
AT=γcosθ
其中AT是粘合张力,单位为达因/厘米;
γ是由泡沫材料吸收的测试液体的表面张力,单位为达因/厘米;
θ是泡沫聚合物材料与一矢量之间的接触角,此矢量在测试液体与泡沫聚合物表面的接触点与测试液体相切,单位:度。
对于任何给出的泡沫材料,可用一种方法通过实验确定此泡沫呈现的粘合张力,在该方法中测量一种亲水测试液体,例如合成尿对于一种已知尺寸和毛细空吸比表面积的泡沫样品的重量摄取量。此方法在后面的“测试方法”部分还要详述。
对于本发明来说,一种特定的泡沫材料如果在大体上没有任何加入的或残留的表面活性剂或其它亲水试剂情况下,它呈现的粘合张力少于大约15达因/厘米(通过毛细空吸摄取的具有表面张力为65±5达因/厘米的合成尿而测定),就认为此材料大体上是疏水的。反过来,当用这种相同的合成尿的毛细空吸摄取测定时,聚合物泡沫材料呈现粘合张力为15达因/厘米或更大,优选20达因/厘米或更大,则认为它是相对亲水的。
在本方法的第一步,把大体是疏水的聚合物泡沫进行处理,结果是在泡沫材料中掺入某种类型的表面活性剂和一种含有特殊类型亲水试剂(将它溶于一种合适的溶剂)的溶液。掺入到泡沫材料中的表面活性剂可以包括任何实质上水不溶性的,柔和的,相对无刺激的表面活性剂化合物,该化合物有助于增强与之接触并可能在上面沉积的聚合物表面的湿润性:这种表面活性剂可以包括,例如,脱水山梨糖醇脂肪酸酯,聚甘油脂肪酸酯和聚氧乙烯(POE)脂肪酸和脂。这些类型的表面活性剂的例子包括TRIODAN
20(它是一种市场上可买到的聚甘油醚,由Grindsted销售)和EMSORB
2502
(它是一种脱水山梨糖醇倍半油酸酯,由Henkel销售)。
特别优选的脱水山梨糖醇脂肪酸酯是例如脱水山梨糖醇单月桂酸酯(SPAN
20),脱水山梨糖醇-油酸酯(SPAN
80)和脱水山梨糖醇三油酸酯(SPAN
85)与脱水山梨糖醇-油酸酯(SPAN
80)的混合物。一种这样特别优选的表面活性剂混合物含有脱水山梨糖醇-油酸酯和脱水山梨糖醇三油酸酯以重量比大于或等于大约3∶1,更优选大于大约4∶1的混合物。
另一种特别优选的脱水山梨糖醇脂肪酸酯表示为脱水山梨糖醇单月桂酸酯(SPAN
20)。脱水山梨糖醇单月桂酸酯事实上在给予有吸收能力的泡沫塑料亲水特性方面是如此有利以致它用作一种亲水试剂已成为一个单独的主题,最近已由DesMarais和Stone向美国申请专利,序列号为_(P&G 案件号4455),该申请在此处引作参考。此脱水山梨糖醇单月桂酸酯因此在本发明范围内是极为优选的用作掺入泡沫塑料中的表面活性剂材料。
上述类型的表面活性剂材料可以任何合适的方式掺入到泡沫材料中去,只要这些方式能导致表面活性剂泡沫材料的聚合物表面接触就行。特别优选的是,这可以促使将表面活性剂材料用作加工中的一个组份(该加工在此处用于制备泡沫材料)。此处优选的泡沫塑料是通过油包水乳状液的聚合制备的,可以将大体上水不溶性的表面活性剂材料作为乳化剂加到此乳状液的含油相单体上。在此方式中,表面活性剂材料执行双重角色,既稳定了要聚合的乳液又作为残留的亲水试剂,它接触并最好涂覆在这之后形成的泡沫结构的聚合物表面。表面活性剂材料可被加到可聚合的含单体油相中,其数值为油相中可聚合的单体材料重量的大约0.5%至20%。
另一方面,本发明所用的表面活性剂材料可以掺入或再掺入到泡沫材料中,该材料在制备时就不含表面活性剂或残留的表面活性剂已被除去。这种表面活性剂的掺入或再掺入可通过用适当的表面活性剂溶液或悬浮液处理此泡沫材料而进行。因此,此处所用的水不溶性表面活性剂可被溶解或分散到一适合的溶剂或载体(例如异丙醇)中然后把所得的溶液或悬浮液与要被处理的泡沫材料相接触。在此方法中,表面活性剂材料被掺入到泡沫结构的孔隙中。
本发明所用表面活性剂在泡沫材料中的通常加入量,与亲水性试剂盐组份结合,能赋予这样处理后的泡沫材料以适当的亲水特性。此表面活性剂的掺入量范围常为聚合的泡沫材料重量的约0.5%至20%,更优选聚合物泡沫材料重量的约1%至16%。
如所指出的,本发明方法的第一步还包括在泡沫材料中掺入某种类型的亲水试剂盐溶液。这种亲水试剂盐溶液的基本组份是选自毒理学可接受的,水合的或可水合的钙和镁盐这样的亲水试剂盐。
此处所用亲水试剂盐的非限制性例子包括水合的或可水合的材料,例如四水合酒石酸钙,六水合硫代硫酸钙,六水合氯化钙,四水合氯化钙,四水合柠檬酸钙,三水合溴化钙,六水合溴化钙,二水合硫酸钙,八水合磷酸镁,五水合酒石酸镁,六水合氯化镁,五水合柠檬酸镁,八水合碘酸镁,七水合硫酸镁,和四水合水杨酸镁。优选的亲水试剂包括收湿或容易潮解的盐,例如氯化钙,溴化钙,氯化镁和碘化镁。也可以使用这些盐的混合物。
用于本发明的钙和镁盐当然应当是毒理学所接受的。毒理学可接受的盐是这样的盐,在亲水泡沫塑料使用或制造或以后的处理过程中,如果偶然摄取或吸入可能遇到的一定量的这样的盐对人类或动物仅有微小的或没有危险。因此,例如水合砷酸镁可能会为泡沫塑料提供很好的适宜亲水性。但是这种盐如被摄取或吸入是有毒的,因此它不包含在本发明的范围之内。
通常把上文所述的亲水化剂盐溶于适宜的溶剂中形成一种溶液,把该溶液依据此方法混入要处理的聚合物泡沫材料中。水是优选的用来制备这种处理溶液的溶剂,但挥发性醇或水/醇溶剂也可被使用。亲水化剂可以任何合宜的浓度混入溶液中。一般所用的溶液含有该溶液重量大约1%至10%的亲水化剂。但更高浓度,甚至饱和的溶液也可使用。当氯化钙被用作亲水化剂时,其在水溶液中的通常浓度为大约1%至5%(重量)。
可用任何适宜的工艺将含有亲水化剂盐的溶液与表面活性剂混入大体上疏水聚合物泡沫材料的结构中,这将导致该溶液在泡沫材料内填充明显数量的泡孔。最优选的是,将此实际应用亲水化剂溶液在制备泡沫结构的工艺中完成。因此,例如,可把适宜的钙和/或镁盐加入到油包水乳状液的水相之中(该乳状液用于制取聚合物泡沫塑料)。当这种乳状液随后进行聚合时,环绕残留的水相材料(具有所希望的溶解的亲水化剂盐),形成泡沫塑料的固体微孔结构。
另一方面,对于在泡沫塑料制备过程中没有使用任何亲水化剂溶液而制成的泡沫塑料,可在其形成后,用一种适宜的亲水化剂盐溶液重复接触并洗涤而对其进行处理,使溶液混入泡沫材料中。作为已形成的大体上是疏水的泡沫材料的这种处理可能是困难的,不管怎样,因为亲水化剂溶液常常是水成的,因此它可能不易被疏水泡沫吸收。在这种情况下,可能需要施加压力或通过反复洗涤和/或对泡沫挤压步骤迫使亲水化剂溶液进入泡沫结构中。也可能需要,例如在相当大泡孔(>90μ)疏水泡沫塑料如聚氨酯的情况下,对亲水化剂使用一种醇或水/醇溶剂以满意地实现在泡沫结构内亲水化剂盐的均匀分布。
当然,也可以结合上述技术进行应用,将亲水化剂盐溶液混入要被处理的泡沫结构中。这样,例如就可将一部分最后所要求的亲水化剂盐混入制备泡沫塑料中所用的流程液体中。这样一种泡沫塑料形成后,在随后的后成型处理(例如洗涤)带有亲水化剂溶液的泡沫的过程中可以掺入附加的或替换的亲水化剂盐。
在本方法的第二加工步骤,使带有混入的表面活性剂和混入的亲水化剂盐溶液的聚合物泡沫材料经历干燥程序以便从亲水化剂盐溶液中除去溶剂。干燥可采用空气,加热或微波处理或其它惯用方法进行,只要这些方法能从泡沫结构中除去溶剂,又不过量除去亲水化剂盐本身就行。
根据本发明有可能从泡沫中完全除去曾用来把亲水化剂盐传送到泡沫中的溶剂。通过干燥步骤而完全除去溶剂将会在泡沫表面留下沉积的亲水化剂盐细颗粒。根据下文的讨论可以知道,以这种方法处理的泡沫可以被称作“过干燥”,因为在干燥时,亲水化剂盐失去了其水合水。因此生成的泡沫看来好像是疏水的。然而在出现相对湿度高于大约40%的情况下,这种被完全干燥的泡沫的亲水表面将得以再生。最好不要把泡沫材料干燥到这种状态。更确切些地说,最好将干燥条件进行调整,使得亲水化剂盐保留其水合水,这样,所得泡沫就成为亲水的。常常将溶剂用此方法从被处理的泡沫结构中除去,这样在泡沫中残留的溶剂,例如,游离的水的含量就不高于(干燥)泡沫重量的大约50%,优选不高于(干燥)泡沫重量的大约10%。
可以知道,通过直接方法而引入到整个泡沫网状物和泡沫网状结构表面的亲水化剂盐的量可根据所要求的亲水化程度以及根据所选亲水化剂盐的效力而变化。例如用完全容易潮解的亲水化剂盐,仅需较小的比例就可得到令人满意的结果。而对于形成较低水合物的盐材料,就要稍微多用一些亲水化剂盐。总的来说,本发明的目的就是在泡沫结构之中和其上引入一定亲水化量的表面活性剂和钙和/或镁盐。为了本发明的这一目的,此亲水化量可以这样确定,即当这些盐完全被水合时,表面活性剂和钙和/或镁盐的数量使某种泡沫呈现至少大约15达因/厘米的粘合张力,优选至少大约20达因/厘米的粘合张力,这可以用具有65±5达因/厘米表面张力的合成尿在37℃通过毛细空吸吸收加以确定。
一般干燥的泡沫材料含有至少大约0.05%重量的表面活性剂加上亲水化剂盐。当使用氯化钙这样的材料时,此泡沫材料常会有约0.1%至7%重量的亲水化剂盐(以泡沫材料的重量为基准)。可以使用更高的含量,但是应当知道,过量的亲水化剂盐通常并不能提供任何有用的效果,而且可能由于干燥的亲水化剂盐过载而引起所得泡沫材料脱落粉末颗粒。
可以知道,对于能有效赋予被处理的泡沫材料亲水特性的表面活性剂和亲水化剂盐,表面活性剂和亲水化剂盐都必须大体均匀分布在泡沫的内部结构中。如果表面活性剂和/或亲水化剂盐仅在泡沫内分散的非连续区域沉积,这就可能发生例如,假若表面活性剂或亲水化剂盐溶液在由聚合物支撑形成的泡沫结构中形成珠或滴,则由此方法提供的整个泡沫材料的亲水效应就可能不能实现。
根据本方法对聚合物泡沫材料的处理可使这种泡沫材料变得适于吸收亲水性液体。虽然不受理论的限制,然而看来好像这里所用的表面活性剂和特殊的亲水化剂盐并不与泡沫聚合物材料化学反应。更确切些说,看来好像这里的亲水化剂盐的功能只是简单地在泡沫表面提供均匀分布的水合水分子。如上所述,此处用亲水化剂盐处理的泡沫可通过从泡沫中的盐除去水合水被“过干燥”。这种过干燥泡沫于是显现为疏水性。然而可把这种泡沫放置在高湿度环境中相当短的时间间隔,于是泡沫的亲水特性可被显著地再生。
在此泡沫被使用的环境中,特别是卫生衬垫,婴儿尿布,等等,靠近人体或与皮肤接触的湿度几乎为100%。根据本方法用水合的或可水合的亲水化剂盐处理的泡沫在有水存在时保持(或已再生)了其亲水特性。这样,在使用中,或因为空气中的湿度或因为紧贴皮肤所提供的湿度都可使可水合的盐完全水合或再水合。在这种情况下,就提供了用于吸收水或人体流体的适宜的亲水性泡沫。不管是什么机理,此处的水合或可水合亲水化剂盐与表面活性剂组份一起按所希望的方式发生作用,并使这种亲水性泡沫没有上述其它方法亲水化疏水泡沫时所提及的某些缺点。
本发明的亲水泡沫材料尤其适用作为吸收含水体液的吸收制品例如婴儿尿布,失禁衬垫,月经产品等等。这种经处理的吸收泡沫的亲水特性可允许这种材料快速接受人体流体如尿和月经至其泡沫结构中。亲水化泡沫材料常常对水性流体例如人体流体呈现所希望的流体传送,例如虹吸性质,因此已吸收的流体可在材料内从吸收泡沫的一个区域移动到另一个区域。
聚合物泡沫材料虹吸,尤其是垂直虹吸水性流体的速度事实上被用作隔离试验以测定使某一给定的聚合物泡沫材料变得亲水性的程度。垂直虹吸速率可以这样确定,即用一给定尺寸的泡沫测试带虹吸一种彩色测试流体例如合成尿至一给定的垂直高度(例如泡沫虹吸流体5cm),测定其所用的时间。这样一种确定垂直虹吸速率的方法在后面的“测试方法”部分还要详述。
甚至一种更简单的隔离试验就可用来测定已被处理的泡沫样品的相对亲水性,该试验包括测量泡沫样品的浸透时间。在此试验中,将泡沫样品落入一烧杯水性测试流体中,例如合成尿,记录下样品浸透所需的时间。所观察到的样品浸透时间越短,则其亲水性越高。一般虹吸时间试验在后面的“测试方法”部分还要详述。
测试方法
在叙述本发明时,描述了吸收泡沫材料的某些特性。在此加以记录的这些特性可用以下的测试流体和测试方法加以确定。
Ⅰ)制备测试流体和泡沫样品
A)测试流体-合成尿
在此试验中所述的几种测量中包括使用合成尿或乙醇这样的测试流体。在下文所述的测试中所用的合成尿是由市场上可买到的合成尿配制的,这种合成尿是由Jayco Pharmaceuticals(Mechanicsburg,PA,17055)生产制造的。此Jayco生产的合成尿包含Kcl,0.2%;Na2SO4,0.2%;NH4H2PO4,0.085%;(NH4)2HPO4,0.015%;CaCl2*2H2O,0.025%;和MgCl2*6H2O,0.05%(重量%)。该合成尿样品是根据标签说明书用蒸馏水配制的。为有助于溶解,把Jayco盐混合物慢慢地加到水中。如果需要除去任何微粒可将样品过滤。任何未用的合成尿一周后都要废弃。为了改进流体的能见度,每升合成尿溶液中可加入5滴蓝色食品颜料。所用的Jayco合成尿其表面张力为65±5达因/厘米。
B)泡沫样品的制备
以下的粘合张力和垂直虹吸速率测试包括制备和测试特别规定尺寸的泡沫样品。这些所需尺寸的泡沫样品应使用锋利的往复式刀锯从大块泡沫上切割下来。使用这种或同等类型的泡沫切割装置可用来大体消除泡沫样品边沿裂缝,这些裂缝对于后面述及的进行测试程序中的某种测量有不利影响。
样品尺寸规格也包括泡沫样品的厚度尺寸。对于本发明来说,厚度的测量应当使泡沫样品处于0.05psi(350Pa)的限制压力下进行。
Ⅱ)粘合张力的确定
由亲水性泡沫样品通过毛细空吸而吸入测试流体而呈现的粘合张力是测试流体的表面张力γ乘以测试流体与泡沫样品的内表面相接触所呈现的接触角θ的余弦乘积。粘合张力可以通过试验确定,即用两种相同的泡沫测试样品使用不同的测试流体而呈现的毛细空吸平衡摄取量进行确定。在这种程序的第一步,泡沫样品的比表面积用乙醇作为测试流体加以确定。如此确定的比表面积在测量第二种测试流体,合成尿的毛细空吸摄取量从而通过实验确定粘合张力时被用作一个系数。
A)比表面积的测量
此处本发明所用泡沫吸收的毛细空吸比表面积可根据已知低表面张力的一种测试液体的平衡摄取量进行确定。在这种情况下,使用无水乙醇(闪点是10℃)。
为实施此测试,将一在22℃±2℃校准平衡的适宜尺寸(例如25cm长×2cm宽×0.8cm厚)泡沫样品条垂直放置并用一实验室千斤顶将其一端在一乙醇储器中浸入1-2mm。可允许乙醇虹吸至泡沫条的平衡高度,该高度应低于样品长度。然后在乙醇样条仍与储器接触时对其称重从而测定全部乙醇摄取量。在此程序过程中应将样品隔离以防乙醇蒸发。
该泡沫样品的比表积可通过下式进行计算:
Sc= (MeGLn)/(Mnγe)
这里Sc=毛细空吸比表面积,单位cm2/g;Me=乙醇(EtOH)的液体摄入量,单位克;G=重力常数(为980cm/sec2);Ln=样品总长度,单位cm;Mn=干燥泡沫样品的质量,单位克;和γe=乙醇(EtOH)的表面张力(为22.3达因/厘米)。
B)粘合张力的确定
如上所述用毛细空吸摄入程序确定泡沫样品的比表面积,然后在相同泡沫的其它样品上以与乙醇程序相同的方式重复,只是将JAYCO合成尿用作测试流体且测试在37℃进行。合成尿的接触角可根据下式从已知的比表面积和合成尿摄入数据进行计算:
cosθu= (MuGLn)/(MNγuSc)
这里θu=Jayco合成尿的接触角,度;Mu=Jayco合成尿的液体摄量,克;G=重力常数(为980cm/sec2);MN=干燥泡沫样品的质量,克;ru=JAYCO尿的表面张力(为~65达因/厘米)Sc=泡沫样品的比表面积,cm2/g,如乙醇摄入量程序所确定;和LN=泡沫样品长度,厘米。
当有表面活性剂存在时(例如在泡沫样品表面上和/或前面提出的测试液体中残留的乳化剂)前面提出的液体的特性可由粘合张力(AT)方程加以限定:
AT= (MTGLN)/(MNSc)
其中MT是由泡沫样品吸收的测试液体的质量,G.LN,MN和SC如前面所限定。[参见Hodgson和Berg,J.Coll,Int.Sci,121(1),1988 PP22-31]
在确定任何给定测试液体的粘合张力时,在任何点随时间的推移都没有作出表面张力的假定值,因此对于虹吸过程中样品表面上表面活性剂的浓度和/或前面所提液体中表面活性剂的浓度可能发生变化是不重要的。所观察到的粘合张力实验值(γ·cosθ)作为最大粘合张力的百分比特别有用,最大粘合张力就是该测试液体的表面张力(例如使用JAYCO合成尿其最大粘合张力应为[65±5][COS 0°=65±5达因/厘米)。
Ⅲ垂直虹吸速率的确定
垂直虹吸速率是干燥泡沫从储器垂直虹吸流体能力的测度。对于前面所述的流体虹吸通过5cm垂直长度的泡沫束所需的时间被测定指定为垂直虹吸速率,对于泡沫塑料来说,平衡垂直虹吸高度至少大于5cm。
用蓝色食品颜料染色的Jayco合成尿被用于以下方法以确定垂直虹吸速率。在此测试程序中,使材料在22℃平衡,并在相同的温度进行测试。
1)样品制备
ⅰ)如在前面粘合张力测试中所述,准备一束泡沫塑料大致为25cm×2cm×0.8cm。
ⅱ)将一流体储器放置在一台实验室千斤顶的顶上并将泡沫样品的一端夹住,于是它就垂直悬于流体储器的上方。
ⅲ)下一步将一把尺子夹在泡沫样品上,结果尺子的底端(ocm)就在泡沫样品底端之上大约1-2mm。
ⅳ)将流体储器用染色的合成尿溶液充至大约全部的3/4。
2)垂直虹吸速率
ⅰ)用实验室千斤顶将储器升高至泡沫样品的底端。流体一接触泡沫样品的底端就开始计时。
ⅱ)立即升高储器直至液体接触到尺子底端为止。可能需要调整实验室千斤顶使样品保持被浸入1-2mm,而且应将样品保护起来防止蒸发。
ⅲ)记录前述流体达到5cm所用的时间。为进行比较也记录下流体测试达到2cm和10cm的时间,如果泡沫样品具有虹吸特性,则测试流体将虹吸至此。
Ⅳ浸透时间的确定
从一较大块的泡沫上切下几块圆柱状泡沫样品,1.125吋(2.86cm)直径,厚度适宜(如0.8cm)。以这样一种方式(即平圆柱面与烧杯中的测试流体相接触)把圆柱形样品从2-3吋5-7.6cm)的高度落入-250ml烧杯中,烧杯中含有大约100ml Jayco的合成尿。只要泡沫样品的底部一与测试流体接触就开始将秒表计时。观察样品直至测试流体虹吸至样品的顶表面。当泡沫样品的顶面大体湿透时,停表,记录下浸透时间。
测试流体的温度可明显影响浸透时间,尤其对本发明优选的油包水为基础的泡沫更是这样。这样对于所有要进行对比测试的样品在特殊的浸透时间屏蔽实践中应使测试流体保持相同的温度。频繁地使用大约70-80°F(21-27℃)的测试流体“冷”温度和大约110-120°F(43-49℃)的测试流体“热”温度。
实施例
亲水化吸收泡沫材料的制备,这种亲水化泡沫材料的特性以及这些亲水性吸收泡沫在用完即可丢弃的婴儿尿布中的应用都在以下的例子中加以举例说明。
例1
用此例说明在半中试装置规模制备亲水化泡沫吸收体。
乳状液的制备
将320g氯化钙和48g过硫酸钾溶于32升蒸馏水中。这就提供了用于形成高内相乳液的水相。
在含有苯乙烯(900克)二乙烯基苯(1260克)和2-乙基己基丙烯酸酯(3840克)的单体混合物中加入脱水山梨糖醇-油酸酯(960克,如SPAN
80)和脱水山梨糖醇三油酸酯(240克,如SPAN
85)。混合后,它含有用于形成高内相乳液的油相。
在55℃至65℃的温度范围分别将油相和水相流加入一动态混合室中。用一销钉转子装置彻底混合动态混合室中的混合的液流。在此操作规模,一合适的销钉转子包含一长约为22cm直径约1.9cm的圆柱轴,此轴安装着两行17个和两行16个的圆柱形销,每个销的直径为0.5cm,从轴的中心轴线径向向外延伸1.6cm的长度。这四行销钉环绕转子轴的圆周呈90°角度配置。互相垂直的各行沿着轴的长度是不重合的,这样从轴的中心线延伸出的同一径向平面内就没有互相垂直的销。销钉转子被安装在一圆柱形套筒内,该套筒形成动态混合室,转子上的销与圆柱形套筒壁有0.8mm的间隙,转子以每分钟800转的速度运行。
在动态混合室的下游接着再安装一台静态混合器(14吋长,1/2吋外径,0.43吋内径)以帮助提供某种背压。这可以帮助动态混合室保持完整地含有圆柱套筒及其销钉转子。这也有助于保证油和水相的恰当的完全的混合。
具有水对油相必要比率的一种乳液是被逐渐接近达到的。首先,调节流动速率将3重量份水相和1重量份油相(油相流动速率为0.75g/sec,0.1磅/分)加入带有销钉转子的动态混合室内。提高水对油相的比率,经几分钟后,直至进入动态混合室的水油相之比达到29份水相对1份油相的比率且流入速率为23ml/sec为止。用肉眼观察,此阶段的乳状液从静态混合器小孔以可搅动的乳状液和“凝结”的稠度流动至使人联想起的含奶油酸奶的稠度。
乳液聚合
在这一点,从静态混合器出来的乳状液随时可以固化。将乳状液加入通常为长方形的模具中,该模具由聚乙烯制成,尺寸为38cm长;25cm宽和22cm深。把乳状液注入至此模具中,直至每个模具含有大约20,000ml要固化的乳状液为止。
把盛有乳状液的模具放在60℃的固化炉中进行固化大约16小时。固化后,所得固体聚合泡沫材料含有高达98%的水,其触感是软的和彻底湿透的。
泡沫的洗涤和亲水化
将湿的已固化泡沫材料从固化模中取出经受进一步的加工。泡沫中的残留水相通过对泡沫材料或泡沫材料的薄片施以足够的压力进行压榨,挤出至少90%原来保留的残留水相材料。
然后将泡沫样品在含有氯化钙作为亲水化剂盐的60℃水中洗涤20秒钟。此亲水化溶液含有1%(重量)的氯化钙。
用在第一次洗涤中的氯化钙溶液用压力再次压榨,然后用氯化钙溶液在60℃对泡沫进行第二次洗涤处理。此第二次洗涤的意图是在泡沫中留下乳化剂/表面活性剂的残余物(16%重量)和氯化钙,因而使内泡沫表面变得相对亲水。
泡沫脱水
两次亲水化的泡沫然后被再次挤压从泡沫的多孔结构内压榨出过量的亲水化溶液。然后把泡沫材料在一烘箱中于60℃干燥12小时使其干燥。干燥后将泡沫材料切成适于后面所述的垂直虹吸速率测试的样品块。
例Ⅱ
用与前述例1大概相同的方式制备另一种聚合物泡沫材料。在此例中,乳状液的制备,聚合、洗涤、亲水化和干燥工序均像例1那样进行只是将10%的CaCl2溶液(3200g CaCl2)用作水相。
例Ⅲ
在此例中,用根据例Ⅰ和Ⅱ的一般工序而制备的聚合物泡沫材料测试其垂直虹吸合成尿的倾向。对比的泡沫材料(其经受不同的洗涤工序从而除去或置换CaCl2亲水化剂盐)也进行测试。
所有制备的泡沫样品均按前面“测试方法”部分中所述的方式测试其垂直虹吸速率和浸透时间。对泡沫样品的说明,对泡沫洗涤处理溶液的说明以及由这些泡沫样品所呈现的垂直虹吸速率和浸透时间均列于表Ⅰ。
表Ⅰ
垂直虹吸速率
泡沫类型 例1 例1 例1 例1
对下列高度 (CaCl2) (仅是H2O)a (FeSO4.7H2O)b (CuCl2)c
的虹吸时间
(分:秒)
2厘米 0:28 4:44 >60:00 12:37
5厘米 1:56 8:33 -- >60:00
10厘米 12:43 >60:00 -- --
在22°的浸 29 159 >360 >360
透时间(秒)
泡沫类型 例Ⅱ 例Ⅱ 例Ⅱ
对下列高度的虹 (CaCl2) (仅是H2O)x (MgCl2)y
吸时间(分:秒)
2厘米 0:48 -- 0:15
5厘米 2:42 10:10 1:17
10厘米 9:23 21:36 8:39
在22°的浸 6 308 4
透时间(秒)
a-例1的泡沫用60℃,不含加入盐的自来水洗涤
b-例1的泡沫用60℃,含2%FeSO4.7H2O的自来水洗涤
c-例1的泡沫用60℃,含1%CuCl2的自来水洗涤
x-例Ⅱ的泡沫用60℃,不含加入盐的自来水洗涤
y-例Ⅱ的泡沫用60℃,含1%MgCl2的自来水洗涤
表Ⅲ的数据显示用CaCl2和MgCl2处理例Ⅰ和Ⅱ的泡沫材料从而提供所希望的高垂直虹吸速率和所希望的短浸透时间。另一方面,仅用水处理或用其它水合的或可水合的盐处理而要使泡沫变得亲水效率极低,这已由如此处理过的泡沫所呈现的相当低的垂直虹吸速率和相当长的浸透时间而得以证明。
例Ⅳ
制备例Ⅱ的泡沫并分别用10%的下列盐的水溶液进行亲水化处理;CaCl2-MgCl2(1∶1重量,混合物);MgSO4;和MgI2。
例Ⅴ
按常规方式用甲苯二异氰酸酯和聚醚多醇制备一种聚氨酯泡沫塑料。将此泡沫在10% CaCl2溶液和异丙醇中的脱水山梨糖醇-油酸/脱水山梨糖醇三油酸中反复浸湿和挤压。用人工压力将过量的溶液榨出。可允许对泡沫进行空气干燥,由此借助于保留在泡沫中的残留表面活性剂和CaCl2使泡沫亲水化。
例Ⅵ
用图2的放大展开分解图所示的结构和部件制备一种使用可吸收泡沫(已按本发明进行了亲水化处理)的易处理婴儿尿布。这种尿布含有一热粘合的聚丙烯上片70,一抗流体渗透的聚乙烯基片71,和放置在顶片和基片之间的双层有吸收力的芯层。此双层有吸收力的芯层包括一改进的水漏形流体储藏/再分配层72,含有例1型亲水化吸收泡沫的向下设置改进水漏形的流体接收/分配层73。上片含有两个大体平行的带弹性阻挡层支架套箍长条74。两个长方形弹性腰带元件75被固定在尿布基片上。将两个腰壳形元件76(由聚乙烯构制)也被固定在聚乙烯基片的每一端。两个平行的支架弹性条77也被固定在基片上,一片聚乙烯78被附着在基片外侧,该面为两个y型件79的专用系紧表面,该y型件可用于将尿布环绕穿戴者系紧。
尿布芯层的接收/分布层含有92%/8%硬化的,加粘的,蜷曲的纤维素纤维和一般的非硬化纤维素纤维的湿铺混合物。此硬化的,加粘的,蜷曲的纤维素纤维是由南方针叶材牛皮纸浆(Foley fluff)制取的,该纸浆已用戊二醛交联到以干燥纤维纤维素葡糖酐基准计大约2.5摩尔百分率。该纤维按照Dean,Moore,Owens和Schggen的美国专利4822453中所述的“干燥交联方法”进行交联,该专利于1989年4月18日颁布,在此引入作为参考。
这些已固化的纤维与具有以下表Ⅱ中所述特性的纤维是相似的。
表Ⅱ
硬化的,加粘的,蜷曲的纤维素(STCC)纤维
类型=南方针叶材牛皮纸浆用戊二醛交联到以干燥纤维纤维素葡糖酐基准计1.41摩尔百分率
干燥的加粘支数=6.8结点/毫米
潮湿的加粘支数=5.1结点/毫米
Isopropol醇保留值=24%
水保留值=37%
蜷曲系数=0.63
用来与STCC纤维混合的一般非硬化纤维素纤维也是用Foleyfluff制取的。将这些非硬化纤维素纤维精制为大约200CSF(加拿大标准打浆度)。
接收/分配层具有的平均干燥密度约为0.07g/cm3,用合成尿浸透的平均密度(以干燥重量为基准)约0.08g/cm3,平均基准重量约0.03g/cm2。在尿布芯层中使用大约9.2克流体接收/分配层。接收/分配层的表面积约为46.8吋2(302厘米2)。其厚度约为0.44厘米。
尿布芯层的流体储藏/再分配层含有一改进的水漏形、前述例1类型的亲水化吸收泡沫部件。用于形成此储藏/再分配层的泡沫大约12克,其表面积大约659吋2(425厘米2),厚度大约0.325吋(0.826厘米)。
具有这种特殊芯层构件的尿布呈现出芯层的特别希望的和有效的应用,它容纳排出的尿,因此当婴儿按一般方式穿戴它时,它提供特别低的渗漏发生率。
例Ⅶ
一种适用于月经期间的轻型妇女衬裤衬垫,它含有根据例Ⅱ的亲水化泡沫衬垫(表面积117cm2;厚度1.5mm),把所说的衬垫插入根据Ahr等人的美国专利4463045(1984年7月31日颁布)的多孔形成膜顶片和含有0.03mm厚聚乙烯薄膜的基片之间。
例Ⅷ
一种根据例Ⅶ制备的月经带,但使用根据例Ⅰ的4mm厚亲水化泡沫衬垫和一多孔非光滑薄膜形成的顶片。此月经带具有Van Tilburg的美国专利4687478(1987年8月18日颁布)中所述的结构。
例Ⅸ
本例叙述本发明范围内另一种类型表面活性剂/CaCl2-亲水化HIPE泡沫材料的制备。
乳状液的制备
将36.32kg氯化钙和568g过硫酸钾溶解在378升水中。这就提供了用在一连续方法中形成可聚合高内相乳液(HIPE)的水相流。
在含有苯乙烯(1600g),二乙烯基苯55%技术级(1600g),和2-乙基己基丙烯酸酯(4800g)的单体混合物中加入脱水山梨糖醇单月桂酸酯(960克如SPAN
20)。混合后可允许将此混合物材料静置过夜。抽出上层清液并用作连续生产工艺形成可聚合的HIPE乳液的油相。(大约75克粘性残余物被废弃。)
将各单独的油相(温度为22℃)流和水相(温度为48-50℃)流加入一动态混合装置中。将混合的料流在动态混合装置中用一销钉转子实行彻底混合。在此种操作规模,合适的销钉转子包括一根长约21.6cm直径约为1.9cm的圆柱形轴。此轴如例1所述,安装着4列销钉,2列有16个销,2列有17个销,每个销钉的直径为0.5cm且从轴的中心线向外延伸1.6cm的长度。将销钉转子安装在一个圆柱形套筒内形成动态混合装置,销钉与圆筒形套筒壁的间隙是0.8mm。
在动态混合装置的下游安装一台螺旋形静态混合器以便为动态混合器提供背压并提供改进的并入最终形成的乳液中的组分。此静态混合器长14吋(35.6cm)外径为0.5吋(1.3cm)。此动态混合器是通过切掉2.4吋(6.1cm)而改进的TAH Industries Model 070-821。
在所建立的联合混合装置中充入油相和水相(以2份水对1份油的比率)。当充料完成时使动态混合器排气让空气逸出。充料时的流速为1.127g/sec油相和2.19cm3/sec水相。
所组装的装置一开始充料,就开始在动态混合器中用转子以1800RPM搅拌。然后在130秒的时间平稳地将水相流动速率提高到35.56cm3/sec的速率。由动态和静态混合器建立的背压在此点是7.5PSI(51.75KPa)。然后在60秒的时间期间将转子速度平稳降至1200RPM。背压落至4.5PSI(31.05KPa)。在这一点,转子速度立刻提高到1800RPM。这之后该系统的背压保持恒定在4.5PSI(31.05KPa)。
乳液的聚合
从静态混合器这一点流出的所形成的乳液被收集到Rubbermaid系统冷冻食品储存箱(Economy Cold Food Storage Boxes),型号3500。这些箱子是用食品级聚乙烯构制的,其公称尺寸为18″×26″×9″(45.7cm×66cm×22.9cm)。这些箱子的实际内部尺寸为15″×23″×9″(38.1cm×58.4cm×22.9cm)这些箱子用一种溶液的薄膜进行预处理,该溶液含有20%溶于等重量的二甲苯和异丙醇混合溶剂中的SPAN
20溶液。可容许这种溶剂混合物蒸发只留下SPAN
20。每个箱子中收集47升乳液。
含有乳液的箱子被放置在维持65℃的场所18小时,以便在箱中进行乳液的聚合而形成聚合物泡沫材料。
泡沫洗涤,亲水化的脱水
完全固化后,将湿的已固化的泡沫材料从固化箱中取出。泡沫此时含有聚合材料重量的30-40倍(30-40X)的残留水相,此水相含有溶解的乳化剂,电解质和引发剂。把此泡沫材料用锋利的往复式锯片切成0.350吋(0.89cm)厚的薄片。这些薄片然后用一连串的3辊隙辊组进行压缩,这些夹辊把残留的泡沫水相含量逐渐降低为已聚合材料重量的大约6倍(6X)。此时再用1% CaCl2溶液在60℃使薄片再饱和,使薄片在辊隙中受压榨,至水相含量约为10X,用1%CaCl2溶液在60℃再饱和,然后在辊隙中再压榨至水相含量约为10X。
现在把含有10X基本上是1%CaCl2溶液的泡沫薄片通过最后配备有真空狭缝的辊隙。这最后的压轧将CaCl2溶液含量降至聚合物重量的5倍(5X)。在最后压轧后,泡沫保持被压缩到大约0.080吋(0.2cm)的厚度。然后将泡沫在设定为大约60℃的空气循环炉中干燥大约3小时。这种干燥使水分含量减少至聚合物材料重量的大约5-7%。此时泡沫薄片的厚度为大约0.075吋(0.19cm)而且是非常褶皱的。此泡沫还含有大约5%重量(以无水的为基准)残留的作为亲水化剂的水合氯化钙以及11%重量残留的脱水山梨糖醇单月桂酸脂(SML)。在被压缩状态,泡沫的密度约为0.17g/cm3。当泡沫在JAYCO合成尿中扩充其自由吸收容量时(26.5ml/g),此膨胀的泡沫具有约为2.24m2/g的毛细空吸比表面积,大约29.5cc/g的孔体积和大约15微米的平均泡孔尺寸。
按照例Ⅸ制备的SML/CaCl2亲水泡沫薄片显示了本发明的一个“薄至湿透”的优选例,因为这些亲水化泡沫薄片是压缩形式的泡沫材料,当其与人体水性流体接触时就会膨胀。一经膨胀,泡沫材料就可用于吸收曾引起泡沫膨胀的人体流体。这种优选的被压缩泡沫是由非水解的聚合物材料形成的那些泡沫,它们所具有的毛细空吸比表面积从大约0.5至5.0m2/g,它们含有大约0.5%至20%的残留乳化剂,并且它们含有泡沫材料重量(以无水的为基准)大约0.1%至7%毒物学可接受的,收湿的,水合盐,此盐优选氯化钙或氯化镁作为亲水化剂盐。
当这种亲水化泡沫材料以其被压缩的状态,储存于72°F(22℃)和50%相对湿度的环境条件时,它将含有聚合物材料重量大约4%至15%的残留水含量。此水含量包括与收湿的水合的盐缔合的水合水以及吸收在泡沫之内的游离水。这种被压缩的亲水化泡沫材料还将具有干燥基准密度,其范围从大约0.08至0.3g/cm3。
这种优选的薄至湿透SML/CaCl2亲水化泡沫材料在其膨胀状态具有从大约12至100ml/g的孔体积,该材料并呈现耐压弯曲性,这样当泡沫在37℃用表面张力为65±5达因/厘米的合成尿饱和至其无吸收容量时,压缩其结构使之变形(从大约5%至95%)15分钟后就产生5.1KPa的限定压力。这些优选的薄至湿透亲水化泡沫材料在其膨胀状态,泡孔的平均尺寸范围从大约5至30微米。已膨胀的亲水化泡沫材料当在此合成尿中饱和至无吸收容量时,其干燥基准密度约为其在被压缩状态的干燥基准密度的9%至28%。
例Ⅹ
用“测试方法”部分中所述的浸透时间方法对按例Ⅸ制备的泡沫材料测试其亲水特性。使这种泡沫材料也经历各种处理工序从其中除去加入的或残留的亲水化剂并有选择地再加入某些材料以测试它们给与泡沫材料亲水特性的有效度。
泡沫材料,处理剂和浸透时间的测试结果均列在下面的表Ⅲ中。
表III
CaCl2重量% | SML重量% | 在JAYCO合成尿中的浸透时间 | |
冷的(~21-27℃ | 热的(~43-49℃) |
例9型泡沫
如所制备的水洗的-膨胀的泡沫-压缩的泡沫-CaCl2再处理的(由H2O) | 3.7%-0--0-3.6 | 11%11%11%11% | 70秒>20分300秒180秒 | 3秒4秒2秒3秒 |
IPA2洗的-CaCl2再处理的(由IPA)-SML再处理的(由IPA)-SMO/STO3再处理的(由IPA) | -0-~5%-0--0- | -0--0-11%19% | ***无限期漂浮***漂浮数小时 漂浮>15分钟~5秒 ~1秒~300秒 ~180秒 |
2IPA=异丙醇
将表Ⅰ(例Ⅲ)和表Ⅲ的数据一起加以研究显示出在例Ⅰ、Ⅱ和Ⅸ型的泡沫样品中掺入CaCl2和表面活性剂的混合物可对泡沫提供亲水特性,此特性一般优于完全不掺亲水化剂或只掺CaCl2或表面活性剂的泡沫亲水特性。
例Ⅺ
制备与例Ⅳ所述结构大体相似的一种尿布,所用流体储藏/再分配层为例Ⅸ所述类型的薄至湿透压缩的、SML/CaCl2亲水化的吸收泡沫片材。在此尿布中,含有硬化的,加粘的,蜷取的纤维素纤维的流体接收/分配层的用量为大约13克。薄至湿透的、SML/CaCl2亲水化的流体储藏/再分配层的用量也是大约13克。
具有这种特殊结构的尿布呈现出利用具有吸收能力的芯层容纳排放的尿特别称心和有效,并因此在婴儿以正常方式穿着时提供特别低的泄漏发生率。
Claims (6)
1、一种使大体疏水聚合物泡沫材料变得适于吸收亲水性液体的方法,该方法的特征在于它包括
A)当泡沫材料大体上没有加入的或残留的亲水试剂时,该泡沫材料大体上是疏水的,将一种实质上水溶性的,柔和的,相对无刺激的表面活性剂(最好选自脱水山梨糖醇脂肪酸酯,聚甘油脂肪酸酯和聚氧乙烯脂肪酸和酯)和一种亲水试剂盐溶液(该溶液由最好选自水,异丙醇及其混合物的一种溶剂和一种选自毒理学可接受的,水合的或可水合的钙和镁盐(最好选自卤化钙,卤化镁及其混合物)的溶解的亲水试剂盐形成的)掺入到聚合物的、优选开孔的、最好是聚氨酯泡沫材料中;和
B)随后将所说的聚合物泡沫材料干燥以除去溶剂,干燥程度最好达到使之含有不高于泡沫重量50%的游离水,由此留下掺在所说聚合物泡沫材料之内大体均匀分布的,亲水量优选至少0.05%重量的所说表面活性剂的所说亲水试剂。
2、权利要求1的方法,其特征在于聚合物泡沫材料是油包水乳状液型聚合的泡沫,该材料最好含有选自苯乙烯、烷基(甲)丙烯酸酯,二乙烯基苯和这些单体的混合物的聚合单体。
3、权利要求1至2任一项的方法,特征在于它含有
A)将在水中含有1%至10%,优选1%至5%重量的氯化钙的水溶液掺入到聚合物泡沫材料中,该材料是通过聚合油包水乳状液而制备的,该乳状液含有可聚合的单体以及可聚合单体重量0.5%至20%的表面活性剂,该表面活性剂选自在所说乳状液油相中的脱水山梨糖醇单月桂酸酯和脱水山梨糖醇-油酸酯及脱水山梨糖醇三油酸酯的混合物;和
B)随后将所说的聚合物泡沫材料干燥以除去水,从而留下掺在所说泡沫材料之内至少为所说泡沫材料重量0.05%,优选0.1%至7%的表面活性剂加氯化钙,以及不多于所说泡沫材料重量50%,最好不多于10%的游离水。
4、一种适于吸收亲水性液体的亲水性聚合物泡沫材料,所说的亲水性聚合物泡沫材料的特征在于它含有一种聚合的,优选开孔的,最好是聚氨酯泡沫材料(该材料在大体上没有加入的或残留的亲水试剂时,实质上是疏水的);一种大体均匀分布的,亲水量至少为所说泡沫材料重量0.05%的,结合实质上水不溶的,柔和性,相对无刺激的表面活性剂(该表面活性剂最好选自脱水山梨糖醇脂肪酸酯,聚甘油脂肪酸酯和聚氧乙烯脂肪酸酯),以及掺在所说泡沫材料中的亲水试剂盐[该盐选自毒理学可接受的,水合的或可水合的钙和镁盐(优选选自卤化钙,卤化镁及其混合物)];以及掺在所说泡沫材料之内的不多于所说泡沫材料重量50%的游离水。
5、权利要求4的亲水聚合物泡沫材料,特征在于掺在泡沫材料之内的表面活性剂的量的范围是泡沫材料重量的0.5%至20%,该表面活性剂最好选自脱水山梨糖醇单月桂酸酯和脱水山梨糖醇一油酸酯和脱水山梨糖醇三油酸酯的混合物;掺在泡沫材料之内的亲水试剂盐的量的范围是泡沫材料重量的0.1%至7%,掺在泡沫材料之内的游离水的量包括不高于泡沫材料重量的10%;亲水试剂盐(优选氯化钙)是完全水合的。
6、权利要求4和5中任一项的亲水聚合物泡沫材料,特征在于聚合物泡沫材料是一种油包水乳状液型聚合的泡沫,它最好含有选自苯乙烯,烷基(甲)丙烯酸酯,二乙烯基苯和这些单体的混合物的聚合单体。
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CN104884515A (zh) * | 2012-12-18 | 2015-09-02 | 于尔戈实验室 | 用于向亲水性聚合物泡沫中掺入活性剂的方法 |
CN104884515B (zh) * | 2012-12-18 | 2018-10-23 | 于尔戈实验室 | 用于向亲水性聚合物泡沫中掺入活性剂的方法 |
CN104988548A (zh) * | 2015-07-21 | 2015-10-21 | 苏州荣昌复合材料有限公司 | 增加工程塑料镀层结合力的表面处理剂及应用 |
US11998432B2 (en) | 2016-06-30 | 2024-06-04 | Kimberly-Clark Worldwide, Inc. | Method of manufacturing a foam and fiber composite |
CN113307906A (zh) * | 2021-05-10 | 2021-08-27 | 万华化学集团股份有限公司 | 无需亲水后处理的高内相乳液泡沫材料的制备方法、泡沫材料及其应用 |
CN118374052A (zh) * | 2024-03-29 | 2024-07-23 | 绍兴高希新材料科技有限公司 | 一种在厚度方向上具有亲水性梯度的高内相乳液多孔泡沫材料的制备方法和应用 |
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