CN108342046B - 机械强化的透明抗生物污损热塑性树脂组合物和其制造方法 - Google Patents
机械强化的透明抗生物污损热塑性树脂组合物和其制造方法 Download PDFInfo
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Abstract
本发明公开一种透明的独立树脂或母料浓缩物组合物,和通过挤出或任何类似的热熔混合工艺将商业透明级基底热塑性塑料转化成抗生物污损树脂的制造方法。再复合的固体允许许多产品重新形成方法,包括但不限于热成形、型材挤出、注塑成型、吹塑成型、吹膜、薄膜铸塑和旋压成不同形状和几何的物品或二次成型在塑料基材上,其在固化后可以抵御微生物、哺乳动物细胞、蛋白质、肽、核酸、类固醇和其它细胞组分的表面吸附。由其形成的物品另外展现机械强化且无浸出,同时在透光率和雾度方面保持相同产品形式的基底热塑性塑料的光学透明度。
Description
相关申请的交叉参考
没有相关的现有申请。
技术领域
本发明涉及用于对透明级的基底热塑性塑料改性以增加其表面生物污损抗性并且附加机械强化,同时在产品形成过程之后保留基底热塑性塑料的透光性和雾度的方法。具体来说,本发明涉及通过挤出或热熔混合将合适的化学改性剂引入到基底材料中以便增加基底热塑性塑料的表面生物污损抗性的方法。本发明还涉及由其形成的产品。
背景技术
透明塑料通常是刚性热塑性塑料,例如聚(甲基丙烯酸甲酯)(PMMA)、聚苯乙烯(PS)、聚对苯二甲酸乙二酯(PET)、聚碳酸酯(PC)、聚甲基戊烯(PMP)、聚砜、聚酰胺(PA)、聚氯乙烯(PVC)、苯乙烯丙烯腈(SAN)、基于苯乙烯-甲基丙烯酸酯的共聚物、基于聚丙烯的共聚物、丙烯腈丁二烯苯乙烯(ABS)、聚酰亚胺(PI)和纤维素树脂。透明塑料被视为透光率百分比超过80%的塑料。由于成本低并且容易加工以及具有重量轻、防碎、耐低温冲击和耐化学特性,这些塑料可以应用在水族馆、广告牌、汽车尾灯、浴缸垫、水槽、手机显示屏、液晶显示器(LCD)的背光光波导、照明灯泡壳和飞机窗户面板中。因此预期在不远的将来,除了包括食品和化妆品包装、建筑、电器、玩具、文具、眼镜等的日用品中的大型应用基础之外,它们可以在更广范的应用中替代不可弯曲的氧化物玻璃。
将日常生活应用中可见的光学透明塑料进行抗生物污染改性是具有强烈的市场需求,这些透明塑料在日常生活的常见应用包括真空吸尘器的集尘室、可再填充的液体皂分配器和卷纸架等,它们需要满足针对微生物的卫生条件。先前研究显示约50%的真空吸尘器刷子含有粪便细菌和大肠杆菌。另一项数据表明超过25%的公共厕所的再填充肥皂分配器被每毫升超过1百万菌落形成单位(CFU)的细菌污染并且约16%的肥皂样品含有大肠菌群。一般来说,细菌群体可以在未消毒且富含营养物的环境中于5小时内增加至少10,000倍。
聚合物的常规防污改性通常通过在成型后进行表面改性和在聚合物表面上涂布亲水层来实现。这可以在如下的许多公开中证明。
CN102942708公开一种用于获得膜、网、线、粒子或微球形式的表面亲水性聚丙烯材料的湿式化学方法,其通过将单体马来酸酐接枝到聚丙烯上然后将聚乙二醇接枝到马来酸酐上实现。这仍然是对于聚丙烯材料的预成型坯的一种表面改性方法,用于赋予抗污损性质。
一个非专利引用描述了一种组合型水凝胶自生成和自我抛光交联聚合物涂料,其中可水解的聚合物链保持从顶部伸出以保持表面抗污损(Xie等人Polymer 2011,52,3738)。
DE19643585揭示一种针对微生物、病毒、寄生虫和原生动物的含有鞘脂类的防粘剂。
US20110177237利用苯并吡喃-4-酮衍生物作为无毒的对环境友好的防污剂,这是一种用于被淹没在水下且经历生物污损的物体的涂料。
WO2016015005公开一种三组分的排拒蛋白质的牙齿粘合系统,其是基于作为活性蛋白排拒剂的2-甲基丙烯酰氧乙基磷酸胆碱。
US20090094954公开一种通过将无机精细粒子层安置在基材表面而获得的防污复合材料。
一些使用各种类别和结构的功能聚合物作为涂层以赋予相关兼容基材针对海洋生物的防污性,如US20160002489、US20150197644、US20100130665和US6303078所举例说明。
特别是针对生命物质,人们甚至采用抗微生物化合物从聚合物材料中的延时释放(例如US20150218390)以避免微生物粘附而形成生物膜和/或杀死已经粘附的微生物从而抑制其生长,这不环保并且对人类潜在地有毒。
基础研究表明,基材的表面能在材料的抗微生物吸附性中扮演重要角色。如果需要微生物在材料表面实现最小限度的长期粘附,材料的表面张力需介于20与30mN/m之间,即该抗吸附性能是与低能表面相关的。硅酮和含氟聚合物是两种众所周知的不污损有机化合物,因为它们的表面能较低,所以已被用作基本涂料成分。
WO2016110271公开一种通过将微生物从基于防污剂的物品表面排拒开来而实现聚合物的抗微生物性质的内置改性方法。防污剂选自由多元醇、聚氧醚、聚胺、聚羧酸酯、聚丙烯酸酯、聚乙烯吡咯烷酮、多糖、两性离子型聚电解质、混合电荷的聚合物区段的共聚系统和/或阳离子聚合物与阴离子聚合物的互穿掺混混合物组成的亲水形成组。所述试剂必须与聚合物载体上的作为偶合连接物的马来酸酐反应并且必须与基底聚合物掺混。
US20100280174公开一种用于将HLB值小于或等于10的非离子型表面活性剂掺入到疏水聚合物中的熔融掺混方法。由于表面活性剂的表面迁移,成型的物品显示蛋白质抗性。然而,没有相关的权利要求表明在所述改性之后存在主体物理变化和机械强化,以及光学性质的保留。
发明内容
因此,在本发明的第一方面,将用于使防污部分非共价地掺混(blend)或共价地接枝到各种光学透明共聚物树脂的主链上的熔融复合策略应用到改性透明级热塑性塑料的方法中,其中所述方法包括首先使用螺杆挤出机上的反应性熔融挤出以从包含所述透明级热塑性塑料的组合物制造具有防污性质的颗粒状树脂,然后从早先制备的粒化颗粒注塑成型以形成产物。通过本发明方法改性的透明级热塑性塑料包括但不限于聚烯烃、环状聚烯烃、丙烯酸类塑料(acrylics)、乙酸酯塑料、苯乙烯类塑料(styrenics)、聚酯、聚酰亚胺、聚芳醚酮、聚碳酸酯、聚氨酯和热塑性弹性体的均聚物、共聚物和掺混物。在一个优选实施方案中,通过本发明方法改性的透明级热塑性塑料包括但不限于聚(甲基丙烯酸甲酯)(PMMA)、聚苯乙烯(PS)、聚对苯二甲酸乙二酯(PET)、聚碳酸酯(PC)、聚甲基戊烯(PMP)、聚砜、聚酰胺(PA)、聚氯乙烯(PVC)、苯乙烯丙烯腈(SAN)、基于苯乙烯-甲基丙烯酸酯的共聚物、基于聚丙烯的共聚物、丙烯腈丁二烯苯乙烯(ABS)、聚酰亚胺(PI)和纤维素树脂、甲基丙烯酸甲酯丁二烯苯乙烯(MBS)、苯乙烯乙烯丁烯苯乙烯嵌段热塑性弹性体(SEBS)等。本发明的方法还包括在基底热塑性塑料的熔融加工之前或期间将作为防污改性剂的一种或多种线性或多臂结构的非离子型表面活性剂、作为抗冲改性剂的聚烯烃弹性体和聚氨酯、引发剂、交联剂、成核剂、抗氧化剂和/或其它辅助添加剂与透明级基底热塑性塑料掺混。当上述透明级基底热塑性塑料、化学改性剂和辅助添加剂在所述通过挤出的熔融加工之前被添加到组合物中时,它们应当被彻底掺混,然后被挤出以形成功能母料。所形成的母料然后进一步与透明级基底热塑性塑料掺混以用于后续挤出。所述熔融加工可以在单螺杆或双螺杆挤出机上实现,所述单螺杆或双螺杆挤出机根据透明级基底热塑性塑料和用于改性透明级基底热塑性塑料的其它主要组分的不同熔融温度在适当加工温度范围内、例如150到250℃下工作。在一个优选实施方案中,所述熔融加工的加工温度在170到220℃的范围。在所述熔融加工后,熔融加工的组合物然后经历冷却,随后从同一个挤出机单独制粒或连续地制粒到同一个挤出机中以获得独立固体或母料浓缩树脂。获得的固体或母料浓缩树脂然后经历注塑成型以重新形成具有期望形状和尺寸的物品。除注塑成型以外,还可以应用其它成型方法以重新形成物品,例如型材挤出、吹塑成型、吹膜、薄膜铸塑、旋压和将所述独立或母料浓缩树脂二次成型在塑料基材上。
本发明的第二方面涉及用于形成功能聚合物或母料浓缩树脂的组合物。所述组合物包含如第一方面和下文所描述的所述透明级基底热塑性塑料(70-99wt%)、抗冲改性剂(0-30wt%)、化学或功能改性剂(0.5-10wt%)(包括防污改性剂(0.1-5wt%))和其它添加剂(0.1-2wt%),例如引发剂、交联剂、成核剂、抗氧化剂和/或辅助添加剂中的一种或多种(0.1-6wt%)。在需要抗冲改性剂的情况下,其重量百分比在0.1-30wt%的范围。所述防污改性剂包括线性和/或多臂结构的非离子型表面活性剂中的一种或多种。在一个优选实施方案中,所述非离子型表面活性剂包括脂肪醇聚氧亚烷基醚、聚氧亚烷基山梨聚糖/山梨醇脂肪酸酯、聚氧亚烷基烷基胺、聚醚二醇、脂肪酸烷醇酰胺和其衍生物。更具体地说,所述非离子型表面活性剂包括聚乙二醇(PEG)山梨醇六油酸酯、AEO-5和聚醚胺(例如D-230或T-5000),其中PEG山梨醇六油酸酯具有在2,000到20,000Da范围的分子量;聚醚胺具有在200到6,000Da范围的分子量。所述抗冲改性剂包括聚烯烃弹性体、氯化聚烯烃、苯乙烯嵌段共聚物、乙烯丙烯橡胶、乙烯乙烯醇、丙烯酸树脂、聚氨酯、乙烯共聚的极性三元共聚物、反应性改性的弹性体。所述引发剂包括酸/碱催化剂。更具体地说,所述引发剂包括对甲苯磺酸、四甲基氢氧化铵或有机过氧化物,例如过氧化二异丙苯、双(叔丁基过氧异丙基)苯、2,5-双(叔丁基过氧基)-2,5-二甲基己烷和过氧化苯甲酰,其可以独立形式或负载于填充剂粒子上的形式存在。所述交联剂是橡胶硫化剂。更具体地说,所述交联剂包括三烯丙基异氰脲酸酯、N,N’-间苯撑双马来酰亚胺和/或硫。更具体地说,所述成核剂包括NX8000、3988、ADK STAB NA-18和/或ADK STAB NA-25。更具体地说,所述抗氧化剂包括丁基化羟基甲苯、1010、1076、1098、168或B 225。所述其它辅助添加剂包括氧化铝纳米粒子、光稳定剂、防结块剂、强化填充剂、光学增白剂、着色剂、阻燃剂和除臭剂。更具体地说,所述辅助添加剂是氧化铝纳米粒子(Alu C)。通过本发明的方法和组合物,透明级基底热塑性塑料的光学透射率和雾度的偏离根据ASTM D1003标准在1mm厚度下小于20%,意味着基底热塑性塑料的透明度得以良好维持,同时它们还符合不同应用的各种标准,包括对于食品和饮料很安全的那些塑料,因为添加到组合物中以用于根据本发明改性透明级基底热塑性塑料的改性剂和其它主要组分能够使得最终产物或由其重新形成的成型物品针对流体生物物质(例如微生物、哺乳动物细胞、蛋白质、肽、核酸、类固醇和其它细胞组分)具有生物污损抗性和机械强化。
本发明和方法的这些和其它实施例和特征将在以下具体实施方式中部分阐述。本发明内容意图提供本发明的综述,但不意在提供排他性或穷尽的解释。以下的具体实施方式用于提供关于本公开和方法的进一步信息。
附图说明
本专利或申请文件含有至少一幅以彩色绘制的图。带有彩图的本专利或专利申请公开的副本将基于请求和支付必要费用由专利局提供。
图1是示意图,显示在不同成型圆板样品上的微生物吸附测试的孵育方案,所述成型圆板样品是通过根据本发明的某些实施方案从包含经改性的透明级基底热塑性塑料的熔融加工的组合物注塑成型而重新形成的。
图2说明用于根据本发明的某些实施方案改性透明级基底热塑性塑料的组合物中的主要组分。
图3是示意图,显示用于根据本发明的某些实施方案改性透明级基底热塑性塑料的单步法和两步法两者的工作流程。
图4说明相对于对照(MBS),由经改性的透明级基底热塑性塑料(MBS-M)中的一种制成的成型板样品的测试结果:(A)是放置在一张纸上面的成型MBS和MBS-M板样品的图片;(B)通过从俯视获取的图片显示成型MBS和MBS-M圆板样品的微生物吸附测试。左边三组图片表示MBS针对大肠杆菌(Escherichia Coli)的微生物吸附,右边三组图片表示MBS针对金黄色葡萄球菌(Staphylococcus Aureus)的微生物吸附。
图5说明相对于对照(PPM),由经改性的透明级基底热塑性塑料(PPM-M)中的一种制成的成型板样品的测试结果:(A)是放置在一张纸上面的成型PPM和PPM-M板样品的图片;(B)是在根据如下文所述的方案于蛋白质排拒分析中测试之后,成型PPM和PPM-M板样品的图片;其中,左侧成型PPM板样品上呈现蓝色,右侧成型PPM-M板样品上呈现棕色;(C)通过从俯视获取的图片显示成型PPM和PPM-M圆板样品的微生物吸附测试。左边三组图片表示PPM针对大肠杆菌的微生物吸附,右边三组图片表示PPM针对金黄色葡萄球菌的微生物吸附。
具体实施方式
说明书中提及“一个实施方案”、“一实施方案”、“一实例实施方案”等时,表示所描述的实施方案可以包括特定特征、结构或特性,但每个实施方案不是一定包括该特定特征、结构或特性。此外,此类措辞不是一定指相同实施方案。另外,当结合一个实施方案描述特定特征、结构或特性时,认为所属领域技术人员了解结合其它实施方案来影响该特征、结构或特性,无论所述其他实施方案是否明确描述或未明确描述该特征、结构或特性。
以范围格式表达的值应以灵活方式解释以不仅包括作为范围限度明确叙述的数值,而且还包括在该范围内涵盖的所有个别数值或子范围,就如同每一数值和子范围被明确叙述一般。举例来说,“约0.1%到约5%”的浓度范围应被解释为不仅包括明确叙述的约0.1wt.%到约5wt.%的浓度,而且还包括所指范围内的个别浓度(例如1%、2%、3%和4%)和子范围(例如0.1%到0.5%、1.1%到2.2%和3.3%到4.4%)。
如本文所描述,除非另外指定,否则术语“a/an(一)”用于包括一个或多于一个,且术语“或,,用于指非排他性的“或”。此外,应理解本文使用的且未另外定义的措辞或术语是用于仅描述而非限制的目的。此外,本文中涉及的所有公开、专利和专利文献以全文引用的方式并入本文中,就如同以引用方式个别地并入一般。如果本文与如此以引用方式并入的文献之间存在用法不一致,那么并入的参考文献中的用法应被视为本文中的用法的补充;对于不可调和的不一致,以本文中的用法为准。
在本文描述的制造方法中,在不脱离本发明原则的情况下,步骤可以任何次序执行,除了当明确叙述时间顺序或操作顺序时。权利要求中大意是执行第一步骤,然后执行若干其它步骤的叙述应被解释为意味着第一步骤在所述其它步骤中的任一个之前执行,但所述其它步骤可以任何合适顺序执行,除非在所述其它步骤内另外叙述顺序。举例来说,叙述“步骤A、步骤B、步骤C、步骤D和步骤E”的权利要求要素应被解释为意味着首先实施步骤A,最后实施步骤E,且步骤B、C和D可在步骤A与E之间以任何顺序实施,并且该顺序仍然属于要求保护的方法的文字范围内。给定步骤或步骤子集合也可以重复。
此外,除非明确的权利要求用语叙述指定步骤被分开实施,否则指定步骤可以同时实施。举例来说,要求保护的进行X的步骤和要求保护的进行Y的步骤可以在单个操作内同时实施,并且得到的方法将属于要求保护的方法的文字范围内。
定义
除非上下文另外明确指示,否则单数形式“一”和“所述”可以包括复数个指示物。
术语“约”可以允许值或范围的一定程度的可变性,例如在陈述的值或陈述的范围极限的10%以内或5%以内。
除非上下文另外明确指示,否则术语“独立地选自”是指所提及的组是相同的、不同的或其混合物。因此,在这个定义下,措辞“X1、X2和X3独立地选自惰性气体”将包括例如X1、X2和X3全部相同、X1、X2和X3全部不同、X1和X2相同但X3不同、以及存在其它类似排列的情况。
优选实施方案的详细描述
本发明不受任何以下说明的范围的限制。以下实施例或实施方案仅用于举例说明。
根据本发明的透明级基底热塑性塑料的改性可以在单步或两步方法中加工(图3)。透明级基底聚合物在挤出之前或期间与化学改性剂和/或辅助添加剂掺混或反应以产生功能聚合物(单步)或母料(两步)。透明级基底热塑性塑料的代表性实例包括(经抗冲改性的)聚丙烯无规(PPR)共聚物和均聚物(PPH)和若干热塑性弹性体,例如甲基丙烯酸甲酯丁二烯苯乙烯(MBS)、苯乙烯乙烯丁烯苯乙烯嵌段热塑性弹性体(SEBS)和聚氨酯。熔融加工可以在以适当加工温度窗操作的单螺杆或双螺杆挤出机上实现。挤出机可以配备有冷却水浴和制粒机以在例如通过注塑成型重新形成物品之前获得独立固体或母料浓缩树脂。对于所述透明级基底热塑性塑料和用于改性其的其它主要组分,加工温度在170到220℃的范围。
选择线性和/或多臂结构的非离子型表面活性剂中的一种或多种作为防污改性剂。非离子型表面活性剂选自脂肪醇聚氧亚烷基醚、聚氧亚烷基山梨聚糖/山梨醇脂肪酸酯、聚氧亚烷基烷基胺、聚醚二醇、脂肪酸烷醇酰胺和其衍生物。聚二乙醇(PEG)山梨醇六油酸酯、AEO-5和聚醚胺(D-230或T-5000)是优选的防污改性剂。功能改性剂的适当比率和组合对于透明级基底热塑性材料的抗生物污损性能和保持透明度是关键的。典型比率为相对于组合物总重量基于重量从0.5%到10%调节。在一个具体实施方案中,PEG山梨醇六油酸酯具有从2,000到20,000Da(或2到20kDa)范围的分子量。在另一个具体实施方案中,所述聚醚胺具有从200到6,000Da范围的分子量。
选择例如聚烯烃弹性体(POE)和热塑性聚氨酯(TPU)等弹性体作为抗冲改性剂以用于改性不同的透明级基底热塑性塑料。VISTAMAXXTM和ENGAGETM系列POE和系列TPU在这种情况下是优选建议的。建议的比率在相对于组合物总重量的基于重量的0.1%到30%的范围以便增加冲击强度。添加相对于组合物总重量的0.01%到0.2%的重量百分比的引发剂和添加剂(包括对甲苯磺酸、四甲基氢氧化铵和/或有机过氧化物,例如过氧化二异丙苯、双(叔丁基过氧异丙基)苯、2,5-双(叔丁基过氧基)-2,5-二甲基己烷和过氧化苯甲酰)以引发防污改性剂共价接枝到基底聚合物和/或抗冲改性剂上。
选择例如抗氧化剂、交联剂、光学增白剂、色母料、气味吸收剂等其它添加剂以控制物品的外观和气味。抗氧化剂优选地选自丁基化羟基甲苯、1010、1076、1098、168或B 225,相对于组合物总重量的重量百分比为0.1重量%到2重量%。交联剂优选地选自三烯丙基异氰脲酸酯、N,N’-间苯撑双马来酰亚胺或硫,相对于组合物总重量的重量百分比为0到1重量%。引发剂优选地选自过氧化二异丙苯、双(叔丁基过氧异丙基)苯或过氧化苯甲酰,相对于组合物总重量的重量百分比为0.01重量%到0.2重量%。成核剂优选地选自NX8000、3988、ADK STAB NA-18或ADK STAB NA-25,相对于组合物总重量的重量百分比为0到3重量%。辅助添加剂优选地是氧化铝纳米粒子(Alu C),用于增加基底聚合物的热变形温度,相对于组合物总重量的建议重量百分比为0.1重量%到4重量%。
在注塑成型期间,壁极厚的部件每次注塑的循环时间典型地在几秒到5分钟的范围。平均来说,在适当的料筒和模具温度控制下,良好设计的模具的注塑落在20秒到60秒的范围。举例来说,在150吨注塑成型机上在从模腔的一个单次注塑中制造狗骨拉伸测试棒(I型,ASTM D638)、Izod冲击测试棒(ASTM D256)、厚度为1.5mm且直径为60mm的用于光学雾度/透射率(ASTM D1003)和黄度指数(ASTM E313)测量的圆形平板、和用于热变形温度测量(ISO 75)的矩形条的样品。在共旋转双螺杆挤出机上进行挤出复合。挤出机具有26mm的螺杆直径、42∶1的螺杆长度/直径(L/D)比和50-500rpm的可调节速度。其料筒被分成7个温度区,其中一个位于模口。挤出机配备有由两个独立隔室构成的定体积给料器,所述两个独立隔室可以相等比率进料两种不同类型的原料。
蛋白质排拒分析程序在本文中描述如下:
(a)将0.5ml牛血清白蛋白(BSA)/0.01M磷酸盐缓冲盐水(0.1g/ml,pH7.4)蛋白质溶液湿润在成型圆板样品的平坦表面上;
(b)将蛋白质溶液在室温下放置半小时以进行吸附;
(c)通过吸走来去除蛋白质溶液;
(d)将相同体积的Bradford试剂(目录号B6916,Sigma)沉积在受影响区域上以染色可能被蛋白质污损的样品表面;
(e)Bradford试剂的颜色改变(从棕色变成蓝色)定性地指示存在吸附的蛋白质。
成型圆板样品上的微生物吸附测试的孵育方案在本文中通过图1中的示意图描述。大肠杆菌(8739TM)和金黄色葡萄球菌(6538PTM)的起始接种物浓度是约0.9×106和8×108细胞/ml于1/500NB溶液(1/500NB是指pH被调节到6.8-7.2的500倍稀释的营养肉汤)中,用于攻击样品表面。以下实施例以及图4B和图5C中说明吸附测试的结果。
实施例
本发明的实施方案可以通过参考经由说明而提供的以下实施例被更好地理解。本发明不限于本文中给出的实施例。
实施例1
通过将94%MBS树脂与1%B 225和5%AEO-5(一种脂肪醇乙氧基化物),基于重量,在180℃到210℃范围的加工温度下挤出复合以直接获得功能树脂而实现MBS(一种高度透明的甲基丙烯酸甲酯丁二烯苯乙烯塑料化合物)的改性。将改性的制剂再制粒为独立树脂(本文中注释为MBS-M),所述独立树脂可以被进料到注塑成型机(利用210℃的加工温度)中以获得由模具工具设计所指定的塑料样品。图4A显示由根据本发明方法的MBS-M制成的成型板样品基本上保持透明。表征结果总结在表1中。MBS-M的冲击强度几乎是基底MBS塑料的冲击强度的两倍,另外还附加了针对革兰氏阴性菌大肠杆菌和革兰氏阳性菌金黄色葡萄球菌的微生物排拒性能。基于在和对应的成型板样品紧密接触之后显示细菌计数几乎log-4的降低,MBS-M通过了ISO 22196的抗菌需求,具有经鉴定合格的报告证书。所述板样品还在ASTM G21和ASTM G22标准下、21天一致地显示零生长等级,具有经鉴定合格的报告证书。此外,MBS-M颗粒的好氧微生物总数以及总计组合霉菌和酵母根据USP<61>计数测试小于10CFU/g,具有经鉴定合格的报告证书。
表1:
实施例2
通过将PPR树脂与30%聚烯烃弹性体(VISTAMAXXTM 6202,ExxonMobil)、2%D-230、2%聚(乙二醇)山梨醇六油酸酯、3.75%氧化铝纳米粒子、0.1%过氧化二异丙苯、0.05%三烯丙基异氰脲酸酯和0.01%CBS-127(一种光学增白剂),基于重量,在170℃到190℃范围的加工温度下挤出复合以在制粒后获得功能母料浓缩物(本文中注释为PPR-M)而实现PPR(一种透明聚丙烯无规共聚物)的改性。将母料以1∶1.5w∶w PPR的比率与0.1%基于总重量的NX8000一起干式掺混,并随后进料到注塑成型机(在190℃的加工温度下)中以获得塑料样品。表征结果总结在表2中。氧化铝纳米粒子通过抵消添加聚烯烃弹性体的影响来帮助最小化热变形温度(HDT)的下降。
表2
实施例3
通过将PPM树脂与2%D-230、2%AEO-5、1%NX8000、0.1%过氧化二异丙苯和0.05%三烯丙基异氰脲酸酯在170℃到190℃范围的加工温度下挤出复合以在制粒后获得功能母料浓缩物(本文中注释为PPM-M)而实现PPM(一种经过抗冲改性的聚丙烯化合物)的改性。将母料以1∶1.5 w∶w PPM的比率与0.1%基于总重量的1010和0.1%基于总重量的168一起干式掺混,用于在190℃的加工温度下注塑成型。图5A显示PPM-M的成型板样品是基本上透明的。表征结果总结于表3以及图5B和图5C中。图5B显示当添加BSA蛋白溶液于由PPM-M制成的成型板样品上时,有效地排拒表面上的蛋白吸附。将牛血清白蛋白(BSA)(一种蛋白质分子)的溶液滴在样品表面上维持5分钟,随后吸走。然后将可以与BSA中的氮反应的Bradford试剂(考马斯蓝)滴在样品表面上。其上吸附BSA的样品表面将Bradford试剂从棕色改变成蓝色,表明表面上蛋白质的吸附(如左侧由PPM制成的成型板样品)。那些排拒蛋白质吸附的表面将保持Bradford试剂呈现棕色,表明样品表面的蛋白质排拒(如右侧由PPM-M制成的成型板样品)。图5C显示大肠杆菌和金黄色葡萄球菌被由PPM-M制成的成型板样品大量排拒(>99%)。基于在和对应的成型板样品紧密接触之后显示细菌计数几乎log-4的降低,PPM-M通过了ISO 22196,具有经鉴定合格的报告证书。基于21天一致的显示零生长等级,PPM-M还通过了ASTM G21和ASTMG22,具有经鉴定合格的报告证书。此外,PPM-M显示零等级,意味着针对网状轮枝链霉菌(Streptoverticillium reticulum)的粉红染色的完全抗性,具有经鉴定合格的报告证书。依据ASTM E2149(一种动态摇瓶抗菌测试),PPM-M成型板在孵育24小时后显示大肠杆菌和金黄色葡萄球菌分别100%和90.7%的减少,具有经鉴定合格的报告证书。依据ISO 20645(一种琼脂扩散平板测试),观察到样品下方大肠杆菌、金黄色葡萄球菌、鼠伤寒沙门氏杆菌(Salmonella typhimurium)、空肠弯曲杆菌(Campylobacter jejuni)的零生长,同时获得零抑制区域,具有经鉴定合格的测试证书,从而暗示无游离杀生物剂浸出。基于依据ASTME2180甚至在与琼脂浆液接触24小时后显示72%的总数降低,样品针对肺炎克雷伯氏菌(Klebsiella pneumoniae)具有抗菌性,具有经鉴定合格的报告证书。此外,PPM-M颗粒的好氧微生物总数以及总计组合霉菌和酵母根据USP<61>计数测试小于10CFU/g,具有经鉴定合格的报告证书。样品还符合三种类型的所用刺激物(3%w/v乙酸、10%v/v乙醇溶液和精馏橄榄油)在70℃、2小时的全面迁移限,以及两种类型的刺激物(3%w/v乙酸、10%v/v乙醇溶液)在100℃、4小时的全面迁移限,如EU No.10/2011所阐述,以及作为欲用于食品接触物品中的聚丙烯共聚物,符合US FDA 21CFR 177.1520(d)第3.1a和3.2a条,。由授权代理机构颁发的相关证书是可获得的。此外,PPM-M颗粒的好氧微生物总数以及总计组合霉菌和酵母根据USP<61>计数测试小于10CFU/g,具有经鉴定合格的报告证书。样品也被证实在ISO10993-4(直接接触和萃取方法两者)溶血测试和ISO 10993-5(MEM洗脱方法)细胞毒性测试中是生物相容的,具有经鉴定合格的报告证书。最后但同样重要的,基底PPM塑料的冲击强度在改性后甚至有轻微的增加。
表3:
实施例4
通过将PPH树脂与30%VISTAMAXXTM 3980FL、2%D-230、2%聚(乙二醇)山梨醇六油酸酯、0.1%过氧化二异丙苯、0.05%三烯丙基异氰脲酸酯和3.75%氧化铝纳米粒子在180℃到200℃范围的加工温度下挤出复合而实现PPH(一种透明聚丙烯均聚物)的改性。再配制的颗粒然后直接进行注塑成型(在200℃的加工温度下)以得到成型样品。表征结果总结在下表中。相对于基底PPH塑料,冲击强度显著增加了超过120%。添加氧化铝纳米粒子以保持PPH的热变形温度(HDT)高达约80℃以用于温水接触应用。表征结果总结在表4中。
表4:
实施例5
通过将SEBS树脂与0.1%对甲苯磺酸、2.5%聚乙二醇(平均分子量10,000)和2.5%AEO-5,基于重量,在170℃到220℃范围的加工温度下挤出复合来实现SEBS(一种苯乙烯乙烯丁烯苯乙烯嵌段热塑性弹性体)的改性。再配制的颗粒直接进行注塑成型(在210℃的加工温度下)以得到成型样品。表征结果总结在表5中。
表5:
Claims (44)
1.一种用于改性透明级基底热塑性塑料以使其形成机械强化和针对流体生物物质具有生物污损抗性的独立固体或母料浓缩物形式的物品的方法,所述方法包括:
(a)提供所述透明级基底热塑性塑料以形成组合物;
(b)将所述透明级基底热塑性塑料与非离子型表面活性剂、与抗冲改性剂、和与其它添加剂直接掺混,或将包含所述透明级基底热塑性塑料、所述非离子型表面活性剂、其它添加剂和抗冲改性剂的母料浓缩物与稀释形式的所述透明级基底热塑性塑料掺混,以形成所述组合物,其中所述非离子型表面活性剂选自由以下各项组成的组:脂肪醇聚氧亚烷基醚、聚氧亚烷基山梨聚糖/山梨醇脂肪酸酯、聚氧亚烷基烷基胺、聚醚二醇、和脂肪酸烷醇酰胺;其中所述抗冲改性剂选自由以下各项组成的组:聚烯烃弹性体(POE)和热塑性聚氨酯(TPU);所述其它添加剂包括引发剂、交联剂、成核剂、抗氧化剂和/或辅助添加剂中的一种或多种;其中所述引发剂选自由以下各项组成的组:对甲苯磺酸、四甲基氢氧化铵和选自过氧化二异丙苯、双(叔丁基过氧异丙基)苯、2,5-双(叔丁基过氧基)-2,5-二甲基己烷和过氧化苯甲酰的有机过氧化物;所述交联剂选自由以下各项组成的组:三烯丙基异氰脲酸酯、N,N’-间苯撑双马来酰亚胺和硫;以及所述辅助添加剂是氧化铝纳米粒子;
(c)熔融加工所述组合物;
(d)在所述熔融加工之后制粒所述组合物以形成颗粒;
(e)将所述颗粒成型成具有期望形状和尺寸的物品。
2.根据权利要求1所述的方法,其中所述熔融加工包括挤出或热熔混合。
3.根据权利要求1所述的方法,其中所述成型包括型材挤出、注塑成型、吹塑成型、吹膜、薄膜铸塑、旋压和二次成型于塑料基材上。
4.根据权利要求1所述的方法,其中所述熔融加工在150到250℃范围的温度下实施。
5.根据权利要求1所述的方法,其中所述熔融加工在170到220℃的温度下实施。
6.根据权利要求1所述的方法,其中所述透明级基底热塑性塑料包括聚烯烃、环状聚烯烃、丙烯酸类塑料、乙酸酯塑料、苯乙烯类塑料、聚酯、聚酰亚胺、聚芳醚酮、聚碳酸酯、聚氨酯和热塑性弹性体的均聚物、共聚物和掺混物。
7.根据权利要求1所述的方法,其中所述透明级基底热塑性塑料包括聚(甲基丙烯酸甲酯)(PMMA)、聚苯乙烯(PS)、聚对苯二甲酸乙二酯(PET)、聚碳酸酯(PC)、聚甲基戊烯(PMP)、聚砜、聚酰胺(PA)、聚氯乙烯(PVC)、苯乙烯丙烯腈(SAN)、基于苯乙烯-甲基丙烯酸酯的共聚物、基于聚丙烯的共聚物、丙烯腈丁二烯苯乙烯(ABS)、聚酰亚胺(PI)、纤维素树脂、甲基丙烯酸甲酯丁二烯苯乙烯(MBS)、苯乙烯乙烯丁烯苯乙烯嵌段热塑性弹性体(SEBS)。
8.根据权利要求7所述的方法,其中所述基于聚丙烯的共聚物包括聚丙烯无规共聚物(PPR)和抗冲改性的聚丙烯化合物(PPM)。
9.根据权利要求7所述的方法,其中所述透明级基底热塑性塑料包括聚丙烯均聚物(PPH)。
10.根据权利要求1所述的方法,其中所述透明级基底热塑性塑料和所述颗粒在熔融加工后具有根据ASTM D1003标准在1mm厚度下低于20%的雾度偏离。
11.根据权利要求1所述的方法,其中所述非离子型表面活性剂选自:聚乙二醇(PEG)山梨醇六油酸酯、AEO-5和聚醚胺。
12.根据权利要求11所述的方法,其中所述PEG山梨醇六油酸酯具有2000到20,000Da的平均分子量。
13.根据权利要求11所述的方法,其中所述聚醚胺具有200到6,000Da的分子量。
15.根据权利要求1所述的方法,其中所述非离子型表面活性剂具有0.5wt%到10wt%的重量百分比。
16.根据权利要求1所述的方法,其中所述聚烯烃弹性体包括VISTMAXXTM系列或ENGAGETM系列。
17.根据权利要求1所述的方法,其中所述抗冲改性剂具有0.1wt%到30wt%的重量浓度。
21.根据权利要求1所述的方法,其中所述引发剂以独立形式存在或负载于填充剂粒子上,所述引发剂的重量百分比为0.01wt%到0.2wt%。
22.根据权利要求1所述的方法,其中所述交联剂具有0.01wt%到0.2wt%的重量百分比。
23.根据权利要求1所述的方法,其中所述成核剂具有0.1wt%到3wt%的重量百分比。
24.根据权利要求1所述的方法,其中所述抗氧化剂具有0.1wt%到2wt%的重量浓度。
25.根据权利要求1所述的方法,其中所述辅助添加剂具有0.1wt%到4wt%的重量百分比。
26.根据权利要求1所述的方法,其中所述母料浓缩物是通过在所述母料浓缩物与稀释形式的所述透明级基底热塑性塑料掺混之前将所述透明级基底热塑性塑料、所述非离子型表面活性剂、其它添加剂和所述抗冲改性剂挤出形成。
27.一种用于形成具有机械强化和针对流体生物物质具有生物污损抗性的功能聚合物或母料浓缩树脂的组合物,其包含70-99wt%的透明级基底热塑性塑料、0.1-30wt%的抗冲改性剂、0.5-10wt%的非离子型表面活性剂和0.1-6wt%的其它添加剂,
其中所述非离子型表面活性剂包括0.1-5wt%的选自以下各项组成的组的物质:脂肪醇聚氧亚烷基醚、聚氧亚烷基山梨聚糖/山梨醇脂肪酸酯、聚氧亚烷基烷基胺、聚醚二醇、和脂肪酸烷醇酰胺;
其中所述其它添加剂包括0.1-6wt%的引发剂、交联剂、成核剂、抗氧化剂和/或辅助添加剂中的一种或多种。
28.根据权利要求27所述的组合物,其中所述透明级基底热塑性塑料包括聚烯烃、环状聚烯烃、丙烯酸类塑料、乙酸酯塑料、苯乙烯类塑料、聚酯、聚酰亚胺、聚芳醚酮、聚碳酸酯、聚氨酯和热塑性弹性体的均聚物、共聚物和掺混物。
29.根据权利要求27所述的组合物,其中所述透明级基底热塑性塑料包括聚(甲基丙烯酸甲酯)(PMMA)、聚苯乙烯(PS)、聚对苯二甲酸乙二酯(PET)、聚碳酸酯(PC)、聚甲基戊烯(PMP)、聚砜、聚酰胺(PA)、聚氯乙烯(PVC)、苯乙烯丙烯腈(SAN)、基于苯乙烯-甲基丙烯酸酯的共聚物、基于聚丙烯的共聚物、丙烯腈丁二烯苯乙烯(ABS)、聚酰亚胺(PI)、纤维素树脂、甲基丙烯酸甲酯丁二烯苯乙烯(MBS)和苯乙烯乙烯丁烯苯乙烯嵌段热塑性弹性体(SEBS)。
30.根据权利要求29所述的组合物,其中所述基于聚丙烯的共聚物包括聚丙烯无规共聚物(PPR)、和抗冲改性的聚丙烯化合物(PPM)。
31.根据权利要求29所述的组合物,其中所述透明级基底热塑性塑料包括聚丙烯均聚物(PPH)。
32.根据权利要求27所述的组合物,其中所述非离子型表面活性剂选自:聚乙二醇(PEG)山梨醇六油酸酯、AEO-5和聚醚胺。
33.根据权利要求32所述的组合物,其中所述PEG山梨醇六油酸酯具有2000到20,000Da的平均分子量。
34.根据权利要求32所述的组合物,其中所述聚醚胺具有200到6,000Da的分子量。
35.根据权利要求27所述的组合物,其中所述抗冲改性剂包括聚烯烃弹性体(POE)和热塑性聚氨酯(TPU)。
36.根据权利要求27所述的组合物,其中所述引发剂包括酸催化剂或碱催化剂,并且以独立形式存在或负载于填充剂粒子上,所述引发剂的重量百分比为0.01wt%到0.2wt%。
37.根据权利要求27所述的组合物,其中所述引发剂包括对甲苯磺酸、四甲基氢氧化铵或有机过氧化物,并且以独立形式存在或负载于填充剂粒子上,所述引发剂的重量百分比为0.01wt%到0.2wt%。
38.根据权利要求37所述的组合物,其中所述有机过氧化物包括过氧化二异丙苯、双(叔丁基过氧异丙基)苯、2,5-双(叔丁基过氧基)-2,5-二甲基己烷、过氧化苯甲酰。
39.根据权利要求27所述的组合物,其中所述交联剂包括三烯丙基异氰脲酸酯、N,N’-间苯撑双马来酰亚胺或硫,并且浓度为0.01wt%到0.2wt%。
42.根据权利要求27所述的组合物,其中所述辅助添加剂包括氧化铝纳米粒子,并且浓度为0.1wt%到4wt%。
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CN111363293B (zh) * | 2020-05-14 | 2022-03-18 | 徐州海天石化有限公司 | 一种可用于生产高刚性高韧性聚丙烯薄壁注塑料的助剂体系的制备方法 |
CN113717485B (zh) * | 2020-05-25 | 2022-12-02 | 合肥杰事杰新材料股份有限公司 | 一种透明聚合物及其制备方法 |
CN114618317B (zh) * | 2020-12-10 | 2024-03-19 | 财团法人纺织产业综合研究所 | 抗结垢过滤膜及其制备方法 |
WO2022135500A1 (en) * | 2020-12-23 | 2022-06-30 | Nano And Advanced Materials Institute Limited | Food contact safe, germ repellent material |
WO2022135501A1 (en) * | 2020-12-23 | 2022-06-30 | Nano And Advanced Materials Institute Limited | Mechanically-strong, biocompatible, food-contact safe and germ-repellent engineering plastics |
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