CN114929816A - 包含聚电解质复合物的不含碳氟化合物的生物基油水阻隔材料 - Google Patents
包含聚电解质复合物的不含碳氟化合物的生物基油水阻隔材料 Download PDFInfo
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- CN114929816A CN114929816A CN202080072858.2A CN202080072858A CN114929816A CN 114929816 A CN114929816 A CN 114929816A CN 202080072858 A CN202080072858 A CN 202080072858A CN 114929816 A CN114929816 A CN 114929816A
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- D06N2213/00—Others characteristics
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
本发明总体上涉及能够在纤维基材料上形成屏障的包含阴离子和阳离子生物聚合物的聚电解质复合物(PEC)的组合物。还公开了具有抗油抗水的屏障涂层的纤维基材料,其中所述材料具有来自至少两层的屏障,所述屏障由包含阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物(PEC)的至少一种组合物形成。与具有单层所述至少一种组合物的相同材料相比,所述两层得到了耐油性和耐水性的改善。
Description
技术领域
本发明总体上涉及能够在纤维基材料上形成屏障的包含阴离子和阳离子生物聚合物的聚电解质复合物(PEC)的组合物。
背景技术
为了增加如用于纸包装的纸等纤维基材料的耐油性和耐水性(产生油水屏障),通常用不同的聚合物材料涂布这些材料。现今,几乎仅使用来自化石来源的聚合物,如聚乙烯。在一些情况下,塑料也与铝箔结合使用以得到更强的屏障。碳氟化合物在制造抗油抗水的纤维材料方面也是非常有效的化学品,但是由于它们的毒性和生物累积,全世界逐渐禁止氟化化合物。如今,包装工业/造纸工业正寻求新的可持续的解决方案以产生满足无毒、生物基和生物可降解的标准的油水屏障。
随着对生物基材料的认识和需求的增加,对寻找化石基屏障的替代物的兴趣也增加。在食品工业中,特别重要的是找到常规屏障的生物基替代物,因为特别关注包装材料的可回收性。此外,包装工业需要可生物降解的屏障,因为可堆肥性是一次性使用物品的主要挑战。
PEC是在带相反电荷的颗粒之间形成的缔合复合物,如聚合物-聚合物、聚合物-药物和聚合物-药物-聚合物。这些复合物由于带相反电荷的聚离子之间的静电相互作用而形成,从而避免使用化学交联剂。基于来源,聚电解质被分类为天然的、合成的和化学改性的生物聚合物。
WO2015/119891描述了一种生产粗糙涂层的方法,所述粗糙涂层用于例如降低经涂布制品的粘性阻力。该涂层包含至少一种阳离子聚电解质和至少一种阴离子聚电解质的聚电解质复合物。然而,该文献中描述的涂层不被认为是对油水的屏障。
Schnell.C.等"Films from xylan/chitosan complexes:preparation andcharacterization”,Cellulose,2017,vol.24,pp.4393-4403,公开了由包含木聚糖和壳聚糖的阳离子聚电解质复合物形成的屏障。所公开的屏障表现出水蒸气和氧气阻隔性能。然而,有利的是提供对脂肪化合物(例如油)也表现出阻隔性能的屏障组合物。
美国专利8,747,955公开了通过包含来自阴离子和阳离子聚合物(例如合成聚丙烯酸酯和多元酸)的聚电解质复合物的涂层来生产具有脂肪屏障的食品包装的方法。然而,有利的是发现合适的生物基材料,其可以由聚电解质组合物形成类似有用的屏障涂层。
WO 2018/038671描述了来自生物基带相反电荷的聚合物的聚电解质复合物的组合物,其可用作纤维基材料、纺织品、织造和非织造材料的粘合剂,并引起材料强度的改善。
Chi,K&Catchmark,M.“Improved eco-friendly barrier materials based oncrystalline nanocellulose/chitosan/carboxymethyl cellulose polyelectrolytecomplexes”,Food Hydrocolloids,2018,vol.80,pp.195-205,公开了具有单层抗油抗水屏障涂层的纤维基材料。所述屏障由来自阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物的组合物形成。
期望的是,进一步开发源自生物基带电聚合物的PEC组合物以获得可用于获得生物可降解纤维材料的受控屏障的组合物,所述生物可降解纤维材料用于脂肪、油脂或油以及用于水基体系,特别是但不限于用于保护食品的目的。对于本领域技术人员来说,由公知常识显而易见的是,拒水拒油的屏障材料在适用时也可用于防污。还应当进一步理解,使用这些种类的屏障材料实现了氧气阻隔率的增大。
出于许多原因,希望使用淀粉,特别是使用阳离子淀粉来产生对油和水的可持续高效阻隔。如下本发明来源于聚电解质复合物(PEC)可在各种情况下从阳离子和阴离子聚合物带来协同作用的总体知识。
发明内容
本发明的总体目的是使用亲水性生物材料来形成对油性产品和水或水基产品都有用的屏障结构。
本发明的一个目的是提供亲水性生物材料的组合物,其可在纤维基材料上形成若干层,使得所述层可协同作用以改善具有其施加层的材料的油水阻隔能力。
本发明的一个具体目的是提供具有油水屏障的纤维基材料,所述油水屏障来源于来自阳离子和阴离子生物聚合物的可生物降解的聚电解质复合物的组合物,所述组合物仅包含通常被批准用于食品接触的组分和添加剂。
本发明的另一个目的是获得油水屏障,该屏障具有施加屏障的受控粘性,并由此具有对屏障的崩解或溶解具有高抗性,同时仍然控制热封能力。
在一个总的第一方面,本发明涉及具有抗油抗水的屏障涂层的纤维基材料,其中所述材料具有来自至少两层的屏障,所述屏障由包含阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物(PEC)的至少一种组合物形成。与具有单层所述至少一种组合物的相同材料相比,两层的存在具有协同效应,并且可以产生抗油性和抗水性的改善。优选地,当至少一种组合物施加到纤维基材料上时,两层中的每一层的载量(add-on)低于施加单层的所述至少一种组合物的载量(单位为g/m2)。
该方面的术语改进的含义是,对于所述材料,抗油性和抗水性的增加将是显著的并且用标准测试可观察到,如对于油的根据T999 pm-96的KIT测试和对于水的根据ISO536:191(E)的COBB方法。
本申请含义中的纤维基材料通常可包含合成或生物纤维,例如纤维素纤维、聚合物纤维或其混合物,包括在各种类型的纸、纸板、瓦楞纸板、包装用纸、其它特种纸、容器、模制纸浆或其它用途、硬纸板、纺织品以及织造和非织造材料中,包括但不限于气流成网(airlaid)、干法成网(drylaid)、纺粘、水刺(spunlace)、湿法缠结(wetlace)、熔喷和湿法成网(wetlaid)的非织造材料。
在本发明的上下文中,油或油脂屏障具有以下含义:材料对于油、油脂、脂肪或诸如通常用于KIT测试的其它亲脂性试剂或有机溶剂的排斥性或防芯吸性。许多这样的测试是本领域技术人员公知的,例如在应用的造纸技术中,并且对于抗油脂性的非限制性实例是TAPPI T559。
在本发明的一个方面,至少一种组合物的PEC包含阳离子生物聚合物和阴离子生物聚合物,所述阳离子生物聚合物选自阳离子淀粉(CS)和/或壳聚糖,所述阴离子生物聚合物选自木质素碱、木质素磺酸或多糖,特别是羧甲基纤维素钠(CMC)、海藻酸、果胶、角叉菜胶、阿拉伯树胶、半纤维素、黄原胶和纳米晶纤维素(NCC)中的至少一种,其中海藻酸和木质素磺酸优选以其钠盐形式存在。
在本发明的一个方面中,所述材料包括屏障,所述屏障包括由包含CS和CMC的聚电解质复合物(PEC)的两种组合物形成的两个层。两种组合物可以包含0.1至20重量%的CMC和0.1至20重量%的CS,优选0.5至10重量%的CMC和0.5至20重量%的CS。
在本发明的一个方面中,多层屏障的至少一种组合物具有限定的pH并包含选自酸、缓冲系统和碱的pH调节剂。根据该方面,酸是有机或无机酸中的一种或多种。有机酸选自以下中的一种或多种:乙酸、乙酰水杨酸、己二酸、抗坏血酸、天冬氨酸、苯磺酸、樟脑磺酸、柠檬酸、二羟基富马酸、esylic酸、甲酸、乙醇酸、谷氨酸、乙醛酸、盐酸、乳酸、苹果酸、丙二酸、马来酸、扁桃酸、mesylic酸、草酸、对甲苯磺酸、戊酸、邻苯二甲酸、丙酸、丙酮酸、水杨酸、硫酸、酒石酸、三氟甲磺酸、任何氨基酸、乙酰丙酸和琥珀酸。无机酸例如为选自卤化氢中的任一种的无机酸:盐酸(HCl)、氢溴酸(HBr)、氢碘酸(HI)或卤素含氧酸:次氯酸、氯酸、高氯酸、高碘酸以及溴和碘的相应化合物,或硫酸(H2SO4)、氨基磺酸、氟硫酸、硝酸(HNO3)、磷酸(H3PO4)、氟锑酸、氟硼酸、六氟磷酸、铬酸(H2CrO4)或硼酸(H3BO3)中的任一种。优选地,酸以0.01至30重量%的量存在于所述层形成组合物中,优选地,所述酸选自柠檬酸、乳酸、草酸和酒石酸,更优选地,所述酸为5至15重量%的柠檬酸和/或乳酸。所述酸优选产生2至4的pH。
本发明前述方面的pH调节剂可以是缓冲体系,因此至少一种组合物包含0.01至30重量%的酸-碱对,优选能够使pH为2至9的相应酸-碱对,更优选1至15重量%的所述酸-碱对。在一个实施方式中,组合物包含1至10重量%的柠檬酸和1至10重量%的柠檬酸三盐,优选二者为等量的。
作为另选,本发明前述方面的pH调节剂可以是碱,优选地,该碱是碳酸氢钠(NaHCO3),其优选提供8至9的pH。
在本发明的一个方面,两种组合物包含具有相同相对量的CS和CMC的PEC;即CS和CMC以相同的重量百分比存在于两种组合物中。
在本发明的一个方面,多层屏障的至少一种组合物包含增塑剂,优选地,增塑剂是多元醇型增塑剂,更优选地,增塑剂是以1至20重量%的量存在的甘油和/或山梨醇。
在本发明的一个方面,多层屏障的至少一种组合物包含选自以下的添加剂:碳酸锆铵;防腐剂;消泡剂;发泡剂;润湿剂;聚结剂;催化剂;表面活性剂;乳化剂;交联剂;湿强度添加剂,例如表氯醇;流变改性剂;填料;非离子聚合物;染料和颜料。
在本发明的一个方面,所述材料具有来自至少两个施用层的屏障,所述至少两个施用层的根据T 999 pm-96测量的KIT值为5以上,根据ISO 536:191(E)测量的COBB60值为50以下。
在本发明的一个方面,该材料具有屏障,其中第一层由具有第一pH值的组合物制成,第二层由具有第二pH值的组合物制成,优选地,第二层由具有比提供第一层的组合物更低的pH值的组合物制成。在一个实施方式中,用于第一层的组合物包含以上概述的缓冲系统,并且用于第二层的组合物包含以上概述的酸。在另一具体的实施方式中,第一层由pH值为3至6的组合物制成,其包含5至20重量%的CS、1至5重量%的CMC和缓冲系统,所述缓冲系统包含选自柠檬酸和柠檬酸的相应羧酸盐以及乳酸和乳酸的相应羧酸盐的酸-碱对,并且所述第二层由pH值为2至3的组合物制成,其包含5至20重量%的CS、1至5重量%的CMC以及选自柠檬酸和乳酸的酸。第一层和第二层例如由具有相同相对量(以重量计)的CS和CMC的两种组合物制成。在该实施方式的一个实例中,第一层形成组合物包含5至15重量%的柠檬酸和柠檬酸三盐,第二层形成组合物包含5至15重量%的柠檬酸。优选地,根据该实施方式,所述第一层是屏障的内层,所述第二层是屏障的外层。
在本发明的一个方面,至少一种组合物的PEC的电荷比≤1。电荷比表示由阳离子和阴离子生物聚合物形成的PEC的总电荷,并且在本说明书的示例部分中进一步定义。
在本发明的其它方面,至少一种组合物的PEC的电荷比为约1或大于1。本领域技术人员可以选择阳离子和离子生物聚合物之间的关系以获得PEC的接近中性的净电荷或阴离子电荷。例如,阴离子生物聚合物CMC的浓度可以相对于阳离子生物聚合物增加,如CS所示例的。可行的是,选择具有不同电荷密度的不同品牌的阳离子生物聚合物以控制所得PEC的电荷比。本发明的以下详述和示例部分为本领域技术人员提供了控制本发明PEC组合物电荷密度的进一步指导。
在本发明的一个方面,该材料具有屏障,所述屏障包含由至少一种包含阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物(PEC)的组合物形成的至少一个层,以及至少一个包含氨基官能硅氧烷的层,或包含疏水剂如蜡的层。用于形成包含氨基官能硅氧烷的层的合适组合物是WO2018/048342(在此引入作为参考)中公开的乳化组合物,可任选向其中加入常规的层形成添加剂。合适的用于包含疏水材料的层的包含氨基官能硅氧烷、可水解的烷基硅烷和水的酸性乳液组合物可见于WO2018/038670(在此引入作为参考)。这样的组合物包含电荷比≤1的来自阳离子和阴离子生物聚合物的PEC和一种或多种选自油、蜡和其它脂质或疏水剂的脂肪化合物。在该方面的一个实施方式中,该材料包含屏障,其具有如上任何地方概述的两层和包含现在描述的氨基官能硅氧烷的附加层,或者包含疏水剂的层。
根据另一方面,本发明涉及施用于纤维基材料的水性聚电解质(PEC)组合物,其用于获得抗油抗水的屏障涂层,其中所述组合物包含:(a)0.1至20重量%的CMC和0.1至20重量%的CS,优选0.5至10重量%的CMC和0.5至20重量%的CS,条件是PEC的电荷比≤1;(b)1至20重量%的增塑剂,优选山梨醇;和(c)1至15重量%的选自酸、缓冲系统和碱的pH调节剂。
在一个实施方式中,所述组合物包含5至20重量%的CS、1至5重量%的CMC和1至15重量%的缓冲系统,所述缓冲系统由酸-碱对组成,其优选为源自有机酸的相应酸-碱对,更优选地,所述缓冲系统选自柠檬酸/柠檬酸的相应羧酸盐以及乳酸/乳酸的相应羧酸盐。优选地,组合物的pH为3至6。还优选地,组合物包含等量(以重量计)的柠檬酸和柠檬酸三盐。
在另一个实施方式中,所述组合物包含5至20重量%的CS、1至5重量%的CMC和有机酸或无机酸,从而提供pH为1至3的组合物,优选所述酸以0.01至30重量%的量存在,更优选地,所述酸选自柠檬酸、乳酸、草酸和酒石酸,更优选地,所述酸为5至15重量%的柠檬酸和/或乳酸。
在另一个实施方式中,所述组合物包含5至20重量%的CS、1至5重量%的CMC和碱,从而提供pH为8至9的组合物,优选地,所述碱为碳酸氢钠(NaHCO3)。
如此实施的组合物可以进一步包含选自以下的添加剂:碳酸锆铵;防腐剂;消泡剂;发泡剂;润湿剂;聚结剂;催化剂;表面活性剂;乳化剂;交联剂;流变改进剂;填料;非离子聚合物;染料和颜料。
本发明的另一方面涉及具有至少两种组合物的试剂盒,其包含:(a)0.1至20重量%的CMC和0.1至20重量%的CS,优选0.5至10重量%的CMC和5至20重量%的CS,条件是PEC的电荷比≤1;(b)1至20重量%的增塑剂,优选山梨糖醇;和(c)1至15重量%的选自酸、缓冲系统和碱的pH调节剂。该试剂盒可用于在纤维基材料上形成屏障并获得抗油抗水的屏障涂层,所述试剂盒包括:包含具有缓冲系统的第一组合物的第一隔室,和具有pH低于第一组合物的包含酸的第二组合物的第二隔室。该第一组合物可以包含5至20重量%的CS、1至5重量%的CMC以及1至15重量%1至15重量%的缓冲系统,所述缓冲系统由酸-碱对组成,其优选为源自有机酸的相应酸-碱对,更优选地,所述缓冲系统选自柠檬酸和柠檬酸的相应羧酸盐以及乳酸和乳酸的相应羧酸盐,并且甚至更优选地,该组合物包含等量(以重量计)的柠檬酸和柠檬酸三价盐,并且具有3至6的pH。第二组合物可以包含5至20重量%的CS、1至5重量%的CMC、以及有机或无机酸,从而提供pH为1至3的组合物,优选地,所述酸以0.01至30重量%的量存在,优选地,所述酸选自柠檬酸、乳酸、草酸和酒石酸,更优选地,所述酸为5至15重量%的柠檬酸和/或乳酸。
如此描述的具有至少两种本发明的组合物的试剂盒通常被组装成在整个运输和储存过程中保持组合物分离并支持组合物的方便的工业应用,以制造具有改进的屏障的本发明材料。为此,将组合物分别储存在试剂盒的不同隔室中,所述隔室可以是本领域技术人员可获得的常规或合适的单独容器。该试剂盒还可以包括用户手册,以便支持在说明书的以下部分中概述的应用或制造方法。
在又一方面,本发明涉及制造先前公开的任一方面或实施方式的材料的方法,其包括以下步骤:以包含阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物(PEC)的组合物将第一层施加至所述材料;任选地在15℃至90℃的温度下干燥所述材料直至基本上干燥;随后再次以第二组合物或相同的组合物将第二层施加到第一层上;并且任选地固化所述材料。在一个实施方式中,固化在20℃至200℃、更优选在50℃至200℃、最优选在90℃至180℃下进行。
所述方法可以通过使用以下处理技术中的至少一种施加第一和第二组合物来进行:喷涂;辊涂;薄漆涂布;浸涂;丝网涂布;浸轧、浸渍或使用施胶压榨;直接涂布法,包括刮刀涂布、刮板涂布、线绕棒涂布、圆棒涂布和挤压泡沫涂布;间接涂布方法包括迈尔棒涂布、直接辊涂、吻合涂布、凹版涂布和逆转辊涂布;优选地,使用辊涂或薄漆涂布进行施加。
在本发明的一个实施方式中,进行其中施用的第二组合物与第一组合物相同的方法。
在本发明的另一个实施方式中,第一组合物具有与第二组合物不同的pH。优选地,第一组合物具有高于第二组合物的pH。还优选地,第一组合物包含5至20重量%的CS、1至5重量%的CMC和1至15重量%的缓冲系统,所述缓冲系统由酸-碱对组成,其优选为源自有机酸的相应酸-碱对,更优选地,所述缓冲系统选自柠檬酸和柠檬酸的相应羧酸盐以及乳酸和乳酸的相应羧酸盐,并且甚至更优选地,该组合物包含等量(以重量计)的柠檬酸和柠檬酸三价盐,并且具有3至6的pH。还优选地,第二组合物包含5至20重量%的CS、1至5重量%的CMC、和有机酸或无机酸,从而提供pH为1至3的组合物,优选地,所述酸以0.01至30重量%的量存在,优选地,所述酸选自柠檬酸、乳酸、草酸和酒石酸,更优选地,所述酸是5至15重量%的柠檬酸和/或乳酸。
具体实施方式
方法、仪器、化学品和配方
实验中使用的仪器:
·使用来自VWR的pHenomenal pH 1000H测量pH,其具有Hamilton Polilyte LabTemp BNC电极(用pH 4、7和10的缓冲液校准)。
·使用Mütek PCD 02设备测量颗粒电荷。
·使用来自IKA(Eurostar digital IKA-Werke或IKA RW28 basic)的顶置式搅拌器连同叶片轴进行制剂和纸浆悬浮液的搅拌。
·使用IKA T25 digital Ultra-Turrax进行制剂的均化。
·材料的涂布用使用钢棒的台式涂布机(称为“涂布机”)或Wichelhaus WI-MU505A水平浸轧机(称为“浸轧机”)进行。
·使用XT 220A Precisa瑞士制天平进行称重。
方法:
方法1-固体含量(SC)
将5克粉末或10克制剂放入铝杯中并置于105℃的烘箱中过夜。然后使用式(4)计算固体含量。
SC=(W2-W0)/W1 (4)
其中W0=杯子的重量,
W1=初始样品的重量
W2=杯子和最终样品的重量。
方法2-电荷密度和电荷比
使用Mütek PCD 02仪器测量电荷密度。电荷(符号:q,单位:meqv)使用式(1)计算。
q[meqv]=C抗衡离子[eqv/l]·V抗衡离子[l]·1000 (1)
其中抗衡离子是聚乙烯硫酸钠(PES-Na,阴离子)或聚二烯丙基二甲基氯化铵(poly-dadmac,阳离子)中的一种,这取决于胶体的电荷。如果将不同浓度的电荷对当前胶体的质量作图,则电荷密度(单位:meqv/g)是线性曲线的斜率。胶体的质量可以使用式(2)计算。
所有电荷密度以完全干燥物质计算。当电荷密度对于一种聚阳离子(例如,阳离子淀粉)和一种聚阴离子(例如,羧甲基纤维素)是已知的时,可计算聚电解质之间的电荷比,使得复合物的总电荷变为正(即电荷比<1),参见式(3)。
方法3-制剂的制备
使用均化器在60℃至70℃下在杀生物剂存在下将阳离子淀粉溶解在水中或用作预煮淀粉浓缩物。将CMC加入到溶解的阳离子淀粉中并利用均化溶解。如果使用添加剂,则在最后步骤中加入它们并混合。
方法4-通过辊涂布纸
使用圆柱形钢棒手动将组合物添加到材料的片材中。将处理过的纸在150℃的烘箱中干燥2至3分钟。
方法5-KIT测试/T 599 pm-96
根据T 599 pm-96测量纸和纸板的抗油脂性测试,其中等级在1(不良屏障)和12(最好的可能屏障)之间。
方法6-COBB法/ISO 536:191(E)
根据ISO 536:191(E)测量60秒(COBB60)或1800秒(COBB1800)期间的吸水率的测定。
方法7-使用浸轧机浸渍纸
将制剂倾倒在浸轧机中的辊之间,并将压力设定为0.1MPa,速度设定为11.6rpm。将处理过的纸在150℃下干燥2至3分钟。
方法8-喷雾测试
织物的耐表面润湿性测定(喷雾试验):欧洲标准EN 24920(ISO4920:1981)。原理:将指定量的水喷洒在安装在环上的纺织品样品上。样品相对于喷嘴以45°的角度设置。标准化喷嘴的中心设置在样本中心上方给定距离处。将给定量的水填充到设置在喷嘴上方并与其连通的贮液器中。喷雾等级通过视觉和/或照相确定。ISO 1-5的阶梯式喷雾等级标准对应于50%至100%的样品经受住润湿。
化学品、材料和组合物:
实验中使用的化学品列于表1和2中。
表1.所用的聚合物
表2.所用的化学品
表3和4中列出了实验中使用纸和纸板。
表3:纸类型
单位 | 1型纸 | 2型纸 | 模制用浆 | |
克重 | g/m2 | 40 | 55 | 400 |
厚度 | μm | 55 | 72 | 1500 |
表4:纸板类型
单位 | 1型纸板 | 2型纸板 | |
克重 | g/m2 | 330 | 260 |
实验中使用的组合物列于表5中。表5的组合物中生物聚合物的重量百分比通过考虑表1中它们的固体含量来计算。还应当注意,在表5中,无论何时单独使用CS和CMC作为参照物,配方均基于溶解在具有少量杀生物剂的自来水中的10至15重量%的生物聚合物。
表5:实施例中使用的组合物
本发明的实施例
实施例1:与PEC相比,仅生物聚合物的比较阻隔性能测试
为了阐明阳离子淀粉和羧甲基纤维素是否分别产生阻隔性能以及当它们结合成PEC时如何表现,进行以下测试。根据方法4涂布2型纸。施加两层,结果示于表6中。
表6.具有其相应组分的PEC组合物6和8的比较
*以水溶液形式制备的组合物,其具有10至13重量%的相应生物聚合物,0.09重量%的Acticide AB6,并加满自来水。
实施例2:层数的重要性
根据方法4用组合物8涂布2型纸,其具有一层和高载量,或具有12.5g/m2或14.2g/m2的两层,参见表7。
表7.在对用一层或两层施加的以不同载量处理的纸测量的KIT值
结果不仅强调了性能取决于载量,而且与一层相比,添加具有足够载量的两层对于获得由KIT数表示的高抗油脂性非常有利。
实施例3:具有不同电荷的PEC组合物的应用
由于PEC可以具有不同的电荷,因此决定评估它们对抗油脂性的影响,参见表8。使用方法4将两层相应的组合物施加到2型纸上。此后使用方法5记录KIT值。
表8.具有不同电荷的PEC组合物
结果显示,利用不同电荷的PEC组合物可以实现高油脂屏障。
实施例4:不同PEC组合物层的组合
一些含有阳离子淀粉的组合物在经处理的材料上产生粘性/发粘的表面,有时这是理想的,而有时是不想要的。在该实施例中,说明了如何在第一层和第二层上选择不同的组合物以降低粘性,并改善KIT和/或COBB值。对2型纸使用施涂方法4。结果见表9。选择更具疏水特征的被称为OC-Biobinder 5401的市售粘合剂以与本发明的组合物1组合。
表9.施加屏障材料后KIT、COBB和表面粘性的观察结果
2型纸 | KIT数 | COBB60 | 观察结果 |
组合物1 | 5 | 55* | 非常粘 |
5401 | 1 | 80 | 不粘 |
层1:组合物1,层2:5401 | 11 | 77 | 不粘 |
层1:5401,层2:组合物1 | 5 | 39 | 非常粘 |
1型纸 | KIT数 | COBB60 | 观察结果 |
组合物1 | 9 | 33* | 非常粘 |
5401 | 0 | 80 | 不粘 |
层1:组合物1,层2:5401 | 11 | 53 | 不粘 |
层1:5401,层2:组合物1 | 11 | 37 | 非常粘 |
*纸片非常粘,并且膜在与水接触时溶胀,这影响了结果
可以得出结论,施用顺序对处理材料的粘性/粘着性、COBB和KIT值有影响。可以根据所需的材料特性选择添加顺序。
实施例5:添加增塑剂对KIT和COBB值的影响
已知碳水化合物基聚合物在其结构上是刚性的,因此期望经处理的材料的手感和外观是刚性的。为了改善经处理的材料的折叠性能、降低刚度、减少干燥纸的褶皱并增加屏障涂层的柔软度,使用常用的生物基增塑剂并优化用量,参见表10。使用方法4,用表10中给出的组合物涂布2型纸。
表10.向PEC组合物中加入山梨醇后的KIT和COBB值
*加入初始PEC制剂中的山梨醇的量(重量%)
除了对屏障涂层具有软化效果之外,还可以看出一定量的山梨醇对经处理的材料的KIT和COBB值具有积极影响。
实施例6:不同pH对阻隔性能的影响
使用pH调节剂作为添加剂(酸和碱)进行测试,以观察是否可以控制粘性,同时仍然保持KIT阻隔性能。使用方法4,将2型纸涂布为2层,参见表11。
表11.PEC组合物的pH调节后的KIT和COBB值
*由于粘性,COBB60无法测量。
关于与原始组合物pH相比已调节至较高pH的组合物,可以看出,用与原始组合物相比已调节至较低pH的制剂处理的纸的粘性小得多。粘性在一些情况下是重要的特征,例如在热密封过程中。
当将柠檬酸一水合物加入到组合物6中时得到的另一观察结果是稀释度变得更好,这意味着当将水加入到制剂中时,PEC组合物没有形成大的沉淀。
实施例7:不同纤维素基材料上的经增塑和pH调节的组合物
在另一实施例中,研究了增塑剂与pH调节添加剂之间的组合。用2型纸、模塑浆纸、1型和2型纸板评价了组合物12和13。使用方法4,用两层组合物涂布所有材料。
表12.经pH调节和增塑的PEC组合物对几种材料的阻隔性能
材料 | 层1 | 层2 | KIT数 | COBB<sub>60</sub> | 评述 |
2型纸 | 组合物12 | 组合物13 | 12 | 35 | |
模塑浆纸 | - | - | 0 | 244 | 参照物 |
模塑浆纸 | 组合物12 | 组合物12 | 10 | 50 | |
模塑浆纸 | 组合物12 | 组合物13 | 11 | 33 | |
1型纸板 | - | - | 0 | 96* | 参照物 |
1型纸板 | 组合物12 | 组合物12 | 12 | 102* | |
1型纸板 | 组合物12 | 组合物13 | 12 | 96* | |
1型纸板 | 组合物13 | 组合物12 | 12 | 103* | |
2型纸板 | - | - | 0 | 103* | 参照物 |
2型纸板 | 组合物12 | 组合物12 | 12 | 87* | |
2型纸板 | 组合物12 | 组合物13 | 12 | 75* | |
2型纸板 | 组合物13 | 组合物12 | 12 | 86* |
*由于材料为纸板,因此进行了COBB1800。
PEC与增塑剂和pH调节添加剂的组合在COBB和KIT值方面都产生了非常有前途的结果,并因此在经涂布材料上产生良好的水和油脂屏障。还清楚的是,组合物12的施加产生良好的油脂屏障,而组合物13产生良好的水屏障,并且最重要的是,这些涂层看起来彼此不干扰,但协同地起作用。
实施例8:各种材料上的PEC和非PEC涂层的组合
为了进一步扩展本发明的用途,涂布了织物材料。根据方法4,分别用PEC组合物1和2涂布克重为150g/m2的白色聚酯织物,随后使用方法7,利用可商购获得的疏水化产品OC-aquasil Tex 310或OC-aquasil Tex 303进一步涂布。结果显示在表13中。
表13.涂布有组合物的聚酯织物
第一层和第二层 | 第三层 | 喷雾评分 | KIT数 |
组合物1和组合物2 | OrganoTex 310 | -2防性 | 5-6 |
组合物1和组合物2 | Tex 303+10%XAN | +3防性 | 7 |
可以得出结论,本发明还能够在与例如纸相比密度低得多的纺织品上产生对水和油脂的良好屏障。
Claims (38)
1.一种具有抗油抗水的屏障涂层的纤维基材料,所述材料具有来自至少两层的屏障,所述屏障由至少一种组合物形成,所述组合物包含阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物(PEC)以及包含缓冲系统的pH调节剂,其中,与具有单层所述至少一种组合物的相同材料相比,所述两层产生抗油性和抗水性的改善。
2.如权利要求1所述的材料,其中,所述阳离子生物聚合物选自阳离子淀粉(CS)和壳聚糖,所述阴离子生物聚合物选自木质素碱、木质素磺酸或多糖,特别是羧甲基纤维素钠(CMC)、海藻酸、果胶、角叉菜胶、阿拉伯树胶、半纤维素和纳米晶纤维素(NCC)中的至少一种,其中,海藻酸和木质素磺酸优选以其钠盐形式存在。
3.如权利要求2所述的材料,其中,所述两层由包含CS和CMC的聚电解质复合物(PEC)的两种组合物形成。
4.如权利要求3所述的材料,其中,所述两种组合物包含0.1至20重量%的CMC和0.1至20重量%的CS,优选0.5至10重量%的CMC和0.5至20重量%的CS。
5.如权利要求1至4中任一项所述的材料,其中,所述至少一种组合物包含pH调节剂,所述pH调节剂选自酸和碱。
6.如权利要求5所述的材料,其中,所述酸为有机或无机酸中的一种或多种,其以0.01至30重量%的量存在于层形成组合物中,优选地,所述酸选自柠檬酸、乳酸、草酸和酒石酸,更优选地,所述酸为5至15重量%的柠檬酸和/或乳酸。
7.如权利要求5所述的材料,其中,所述缓冲系统向所述组合物提供0.01至30重量%的酸-碱对,优选地,相应的酸-碱对允许pH为2至9。
8.如权利要求7所述的材料,其中,所述组合物包含1至10重量%的柠檬酸和1至10重量%的柠檬酸三盐,优选二者为等量的。
9.如权利要求5所述的材料,其中,所述碱是碳酸氢钠(NaHCO3)。
10.如权利要求3至9中任一项所述的材料,其中,所述两种组合物包含具有相同相对量的CS和CMC的PEC。
11.如权利要求1至10中任一项所述的材料,其中,所述层形成组合物的至少一种包含增塑剂,优选地,所述增塑剂是多元醇型增塑剂,更优选地,所述增塑剂是以1至20重量%的量存在的山梨醇。
12.如前述权利要求中任一项所述的材料,其中,至少一种层形成组合物包含选自以下的添加剂:碳酸锆铵;防腐剂;消泡剂;发泡剂;润湿剂;聚结剂;催化剂;表面活性剂;乳化剂;交联剂;流变改性剂;填料;非离子聚合物;染料和颜料。
13.如前述权利要求中任一项所述的材料,其中,所述屏障的根据T 999pm-96测量的KIT值为5以上,根据ISO 536:191(E)测量的COBB60值为50以下。
14.如前述权利要求中任一项所述的材料,其中,第一层由具有第一pH值的组合物制成,第二层由具有第二pH值的组合物制成,优选地,所述第二层由具有比提供所述第一层的组合物更低的pH值的组合物制成。
15.如权利要求14所述的材料,其中,所述第一层的组合物包含权利要求7或8所述的缓冲系统,并且所述第二层的组合物包含权利要求6所述的酸。
16.如权利要求15所述的材料,其中,所述第一层由pH值为3至6的组合物制成,其包含5至20重量%的CS、1至5重量%的CMC和缓冲系统,所述缓冲系统包含选自柠檬酸和柠檬酸的羧酸盐以及乳酸和乳酸的相应羧酸盐的酸-碱对,并且其中,所述第二层由pH值为1至3的组合物制成,其包含5至20重量%的CS、1至5重量%的CMC和选自柠檬酸和乳酸的酸。
17.如权利要求14至16中任一项所述的材料,其中,所述第一层和第二层由具有以重量计相同相对量的CS和CMC的两种组合物制成。
18.如权利要求16或17所述的材料,其中,第一层形成组合物包含5至15重量%的柠檬酸和柠檬酸三盐,第二层形成组合物包含5至15重量%的柠檬酸。
19.如权利要求14至18中任一项所述的材料,其中,所述第一层是所述屏障的内层,所述第二层是所述屏障的外层。
20.如前述权利要求中任一项所述的材料,其中,PEC的电荷比≤1。
21.如前述权利要求中任一项所述的材料,其中,屏障包含至少一个包含氨基官能硅氧烷的层,或包含疏水剂如蜡或油的层。
22.如权利要求21所述的材料,其包含权利要求14至21中任一项所述的两层和权利要求21所述的附加层。
23.一种施用于纤维基材料的水性聚电解质(PEC)组合物,其用于获得抗油抗水的屏障涂层,其中,所述组合物包含:
(a)0.1至20重量%的CMC和0.1至20重量%的CS,优选0.5至10重量%的CMC和10至20重量%的CS,条件是PEC的电荷比≤1;
(b)1至20重量%的增塑剂,其优选山梨醇;和
(c)1至15重量%的pH调节剂,其选自酸、缓冲系统和碱。
24.如权利要求23所述的组合物,其包含5至20重量%的CS、1至5重量%的CMC和1至15重量%的缓冲系统,所述缓冲系统由酸-碱对组成,其优选为源自有机酸的相应酸-碱对,更优选地,所述缓冲系统选自柠檬酸和柠檬酸的相应羧酸盐以及乳酸和乳酸的相应羧酸盐。
25.如权利要求24所述的组合物,其包含以重量计等量的柠檬酸和柠檬酸三盐。
26.如权利要求24或25所述的组合物,其pH为3至6。
27.如权利要求23所述的组合物,其包含5至20重量%的CS,1至5重量%的CMC和有机酸或无机酸,从而提供pH为1至3的组合物,优选地,所述酸以0.01至30重量%的量存在,更优选地,所述酸选自柠檬酸、乳酸、草酸和酒石酸,更优选地,所述酸为5至15重量%的柠檬酸和/或乳酸。
28.如权利要求23所述的组合物,其包含5至20重量%的CS、1至5重量%的CMC和碱,从而提供pH为8至9的组合物,优选地,所述碱为碳酸氢钠(NaHCO3)。
29.如权利要求23至28中任一项所述的材料,其包含选自以下中至少一种的添加剂:碳酸锆铵;防腐剂;消泡剂;发泡剂;润湿剂;聚结剂;催化剂;表面活性剂;乳化剂;交联剂;流变改进剂;填料;非离子聚合物;染料和颜料。
30.一种试剂盒,其包含至少两种如权利要求23所述的组合物,其施用于纤维基材料以获得抗油抗水的屏障涂层,所述试剂盒包含:包含具有缓冲系统的组合物的第一隔室,和具有pH低于第一组合物的包含酸的组合物的第二隔室。
31.如权利要求30所述的试剂盒,其中,所述第一组合物是权利要求24至26中任一项所述的组合物,并且其中,所述第二组合物是权利要求27所述的组合物。
32.一种制造权利要求1至22中任一项所述的材料的方法,其包括以下步骤:
以包含阳离子生物聚合物和阴离子生物聚合物的聚电解质复合物(PEC)的第一组合物将第一层施加至所述材料;
任选地,在15℃至90℃的温度下干燥所述材料;
以第二组合物将第二层施加到所述第一层上;并且
在15℃至90℃的温度下固化所述材料。
33.如权利要求32所述的方法,其中,固化在20℃至200℃、更优选在90℃至200℃、最优选在90℃至180℃下进行。
34.如权利要求32或33所述的方法,其包括通过使用以下方法中的至少一种施加第一和第二组合物:喷涂;辊涂;薄漆涂布;浸涂;丝网涂布;浸轧、浸渍或施胶压榨;直接涂布法,包括刮刀涂布、刮板涂布、线绕棒涂布、圆棒涂布和挤压泡沫涂布;间接涂布法,包括迈尔棒涂布、直接辊涂、吻合涂布、凹版涂布和逆转辊涂布;优选地,使用辊涂或薄漆涂布进行施加。
35.如权利要求32至34中任一项所述的方法,其中,所述第二组合物与所述第一组合物相同。
36.如权利要求32至34中任一项所述的方法,其中,所述第一组合物具有与所述第二组合物不同的pH。
37.如权利要求36所述的方法,所述第一组合物具有高于所述第二组合物的pH。
38.如权利要求37所述的方法,其中,所述第一组合物是权利要求24至26中任一项所述的组合物,所述第二组合物是权利要求27所述的组合物。
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PCT/SE2020/051003 WO2021086247A1 (en) | 2019-10-31 | 2020-10-20 | Flourocarbon free and biobased oil and water barrier materials comprising polyelectrolyte complexes |
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CN114929816B (zh) | 2023-08-04 |
AU2020376727A1 (en) | 2022-05-12 |
CA3155118A1 (en) | 2021-05-06 |
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US20220356652A1 (en) | 2022-11-10 |
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