CN113493599A - 一种取向薄膜及含有该取向薄膜的多层薄膜 - Google Patents
一种取向薄膜及含有该取向薄膜的多层薄膜 Download PDFInfo
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- CN113493599A CN113493599A CN202010199486.1A CN202010199486A CN113493599A CN 113493599 A CN113493599 A CN 113493599A CN 202010199486 A CN202010199486 A CN 202010199486A CN 113493599 A CN113493599 A CN 113493599A
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- oriented film
- film
- polyhydroxyalkanoate
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Abstract
本发明提供一种取向薄膜,含有聚乳酸和聚羟基烷酸酯,且以聚乳酸为100重量份计,聚羟基烷酸酯为100~300重量份。本发明所述的取向薄膜具有快速生物降解的能力,受土壤掩埋后,会快速降解,不会较长期的留存在土壤中,同时该取向薄膜又可以通过通用的取向薄膜的制备方法制备,制备工艺简单,生产性好,且具有优异的诸如强度、尺寸均匀性等性能。本发明还提供含有所述取向薄膜的多层薄膜,以及使用所述生物降解树脂薄膜的包装材料薄膜、胶带。
Description
技术领域
本发明属于高分子材料领域,涉及一种取向薄膜及含有该取向薄膜的多层薄膜。
背景技术
塑料薄膜,尤其是通过单向或双向拉伸、吹塑等方法制备的取向薄膜,是一种可以工业化大量制造的、性能优异且可调控、成本较低廉的材料,已被用于人类生产、生活的各个方面。然而,大多数的塑料薄膜在使用寿命结束后,可以长时期留存于自然界中,如果不加以处理,会造成污染。
生物可降解塑料可以被细菌分解,使用此类材料可以有效改善上述问题。目前,市场上较常见的生物降解塑料包括:聚乳酸、聚对苯二甲酸己二酸丁二醇酯、聚羟基烷酸酯、聚丁二酸丁二醇酯、聚乙醇酸、聚己内酯、聚丙撑碳酸脂等。由于聚乳酸的加工性能、力学性能的综合表现较为优异,所以其是目前用量最大的生物可降解塑料之一。但是,如同其它各种树脂一样,聚乳酸在面向各种用途时,也存在一定的缺点。例如,聚乳酸的生物降解速度较慢,尤其在细菌含量较少、环境温度较低的环境中。即,聚乳酸虽然可以通过工业堆肥的标准方法被认定为是可堆肥的,但是其往往难以通过土埋法的标准方法的认定,这意味着其受土壤掩埋后,不会快速降解,而会较长期的留存在土壤中。
为了提高聚乳酸的生物降解速度,一种常见的技术方案是将聚乳酸与淀粉、聚羟基烷酸酯等生物降解速度快的聚合物共混。中国专利申请CN201380029996.2给出了一种聚乳酸与聚羟基烷酸酯的共混物,机械特性如拉伸强度、抗穿刺性、伸长率;热特性如热变形温度以及光学特性如透明度等得到改善。日本专利申请特开平10-147653也给出了一种聚乳酸与聚羟基烷酸酯的共混物,具有较好的机械强度、透明性、耐热性。虽然,上述技术都能够提高聚乳酸的生物降解性,但是发明人发现,共混物中聚羟基烷酸酯的含量较低时其生物降解速度不足,而共混物中聚羟基烷酸酯的含量较高时,薄膜加工性能不足,难以制备性能优异的取向薄膜。
为此,需要一种取向薄膜,其具有快速生物降解的能力,受土壤掩埋后,会快速降解,不会较长期的留存在土壤中,同时该取向薄膜又可以通过通用的取向薄膜的制备方法制备,制备工艺简单,生产性好,且具有优异的诸如强度、尺寸均匀性等性能。
发明内容
为了解决上述问题,本发明提供一种取向薄膜,含有聚乳酸和聚羟基烷酸酯,且以聚乳酸为100重量份计,聚羟基烷酸酯为100~300重量份。
所述的取向薄膜是通过例如挤出、流延、模压、吹塑等方法制的坯料后,再经过单向拉伸、双向拉伸,或通过吹塑方法直接制得的薄膜中聚合物分子链段和/或结晶沿着单向或双向有序排列的薄膜。薄膜的偏振拉曼光谱中,存在某些特定的特征峰,其峰强度与薄膜的取向程度有关。对于含聚乳酸的薄膜,可以使用873cm-1(峰值记为P)和1769cm-1(峰值记为Q)的峰作为特征峰,通过如下方法判断是否是取向薄膜:对样品薄膜的断面进行偏振拉曼光谱的采集,得到薄膜长度方向(MD)方向、薄膜幅宽方向(TD)方向、厚度方向(ZD)方向的P和Q,分别计算三个方向下的P/Q值,记为(P/Q)MD、(P/Q)TD、(P/Q)ZD;再计算(P/Q)MD/(P/Q)ZD和(P/Q)TD/(P/Q)ZD值,按上述办法重复测量5次,每次取点间隔200μm,取点方向任意,求(P/Q)MD/(P/Q)ZD的平均值和(P/Q)TD/(P/Q)ZD的平均值,如果任一平均值≥1.1,优选≥1.3则薄膜是取向薄膜。所述的聚乳酸是乳酸的均聚物或共聚物中的一种或多种。对于乳酸的均聚物,优选由80-100mol%的L-乳酸或D-乳酸的和0-20mol%的其各自的对映体构成。对于乳酸的共聚物,优选含有85-99mol%的L-乳酸或D-乳酸。聚乳酸可以通过乳酸等物质作为原料,通过脱水缩聚而得到;也可以从丙交酯等物质通过开环聚合而得到。其中,丙交酯可以列举出,L-乳酸的环状二聚物即L-丙交酯、D-乳酸的环状二聚物即D-丙交酯、D-乳酸与L-乳酸进行环状二聚化而得到的内消旋丙交酯、或D-丙交酯和L-丙交酯的外消旋混合物即DL-丙交酯。本发明中可以使用上述任何一种丙交酯。
所述的聚羟基烷酸酯是单体单元为碳原子数4个以上的羟基羧酸的均聚物以及单体单元为碳原子数4个以上的羟基羧酸与其它化学结构的共聚物。此类物质一般由细菌菌体内合成。具体的,所述的聚羟基烷酸酯的单体单元可以是2-羟基丁酸酯、3-羟基丁酸酯、3-羟基戊酸酯、3-羟基己酸酯、3-羟基庚酸酯、3-羟基辛酸酯、3-羟基壬酸酯、3-羟基癸酸酯、3-羟基十二酸酯、4-羟基丁酸酯、4-羟基戊酸酯、5-羟基戊酸酯、6-羟基己酸酯等物质。
进一步的,所述的聚羟基烷酸酯是选自聚羟基丁酸脂和羟基丁酸脂的共聚物构成的组中的一种或多种。
本发明所述的取向薄膜中,以聚乳酸为100重量份计,聚羟基烷酸酯为100~300重量份。如果聚乳酸的含量过多,则取向薄膜的生物降解速度不足;如果聚乳酸的含量过低,则取向薄膜在生产后,由于聚羟基烷酸酯未结晶且玻璃化温度较低,难以直接进行后段拉伸工艺造成工艺不稳定、生产性差,同时薄膜的储存稳定性等性能也不佳。优选的,以聚乳酸为100重量份计,聚羟基烷酸酯为151~300重量份。
进一步的,本发明所述的取向薄膜中,所述的聚乳酸是连续相。所述的取向薄膜是具有相分离结构的,相分离结构可以是存在分散相和连续相的海岛分相体系,也可以是同时存在两个连续相的共连续体系。在海岛分相体系中,分散相是彼此独立的,且被连续相包围,而连续相是贯通的。在共连续体系中,两相相互穿插、包围,但都是贯通的。可以通过扫描电子显微镜、透射电子显微镜、原子力显微镜、拉曼面扫描等显微法观察相形貌,判断相结构并判断连续相的成分。聚乳酸是连续相有利于提高薄膜生产性,可以使得薄膜在更宽广的工艺窗口内稳定的制备。
进一步的,所述的聚羟基烷酸酯是分散相,且聚羟基烷酸酯相的平均直径为3μm以下。优选的,所述的聚羟基烷酸酯的相的平均直径为1.5μm以下。聚羟基烷酸酯的相的平均直径小有利于提高薄膜生产性、生物降解速度,并提高薄膜的性能稳定性和均匀性。
进一步的,为了提高薄膜的柔软度,所述的取向薄膜的熔点可以为150℃以下。所述的熔点是指使用差示扫描量热仪(DSC)对取向薄膜进行10℃/min的升温过程中监测到的所有熔融峰峰值温度的最高值。优选,所述的取向薄膜的熔点为140℃以下。
进一步的,为了提高薄膜的柔软度,所述的取向薄膜的熔融焓可以为10~30J/g,优选10~20J/g。所述的熔点是指使用差示扫描量热仪(DSC)对取向薄膜进行10℃/min的升温过程中监测到的所有熔融峰的熔融焓之和。
进一步的,为了提高薄膜的刚性,所述的取向薄膜的熔点可以为151℃以上,优选160℃以上。
进一步的,为了提高薄膜的刚性,所述的取向薄膜的熔融焓可以为31~60J/g,优选40~60J/g。
本发明所述的生物降解树脂中,可以在不妨碍实现本发明的目的的范围内,使用填充剂、增塑剂、增容剂、封端剂、阻燃剂、成核剂、抗氧化剂、润滑剂、抗静电剂、防雾剂、光稳定剂、紫外线吸收剂、颜料、防霉剂、抗菌剂、或发泡剂等添加剂中的一种或多种。
所述的填充剂,可以使用通常用于橡塑行业的纤维状、片状、粒状、或粉末状的填充剂,包括无机或有机填充剂。无机填充剂,具体地可以列举出玻璃纤维、石棉纤维、碳纤维、石墨纤维、金属纤维、钛酸钾晶须、硼酸铝晶须、镁系晶须、硅系晶须、硅灰石、海泡石、石棉、矿渣纤维、硬硅钙石、硅磷灰石、石膏纤维、二氧化硅纤维、二氧化硅/氧化铝纤维、氧化锆纤维、氮化硼纤维、氮化硅纤维或硼纤维等纤维状无机填充剂中的一种或多种,或玻璃薄片、非膨润性云母、膨润性云母、石墨、金属箔、陶瓷珠粒、滑石、粘土、云母、绢云母、沸石、膨润土、蛭石、蒙脱土、白云石、高岭土、微粉硅酸、长石粉、钛酸钾、微细中空玻璃球、碳酸钙、碳酸镁、硫酸钙、二氧化钛、勃姆石氧化铝、氧化硅、石膏、均密石英岩、片钠铝石或白土等片状或粒状的无机填充剂中的一种或多种。有机填充剂,具体地可以列举出淀粉、纤维素、剑麻纤维、或竹纤维等植物性纤维、羊毛纤维等动物性纤维,芳族聚酰胺纤维、或芳族聚酯纤维等有机合成纤维中的一种或多种。上述填充剂可以进行任意形式的表面处理,以增强其同树脂之间的界面黏附性。
所述的增塑剂,没有特别限定,可以列举出羟基苯甲酸-2-乙基己酯等羟基苯甲酸酯、丙三醇的环氧乙烷加成物的乙酸酯等多元醇酯、邻苯二甲酸二-2-乙基己酯等邻苯二甲酸酯、己二酸二辛酯等己二酸酯、马来酸二正丁酯等马来酸酯、乙酰柠檬酸三丁酯等柠檬酸酯、或磷酸三甲苯酯等烷基磷酸酯、偏苯三酸三辛酯等三羧酸酯、琥珀酸与三乙二醇单甲醚形成的酯、己二酸与二乙二醇单甲醚形成的酯、或1,3,6-己三酸与聚乙二醇单甲醚形成的酯等多元羧酸的烷基醚酯、乙酰化聚氧乙烯己基醚等乙酰化聚氧乙烯烷基(烷基的碳数为2-15)醚、环氧乙烷的加成摩尔数为3-20的聚乙二醇二乙酸酯、聚氧化乙烯-1,4-丁二醇醚二乙酸酯、聚乙二醇、聚丙二醇、或聚乙二醇-聚丙二醇共聚物的聚醚、大豆油、或橄榄油等油脂等、或上述化学结构同聚乳酸的共聚物等。优选邻苯二甲酸二辛酯、邻苯二甲酸二丁酯、邻苯二甲酸丁苄酯、癸二酸二辛酯、癸二酸二丁酯、柠檬酸三丁酯、柠檬酸三乙酯、乙酰柠檬酸三乙酯、乙酰柠檬酸三丁酯、三乙酸甘油酯、聚乙二醇、聚丙二醇、聚乙二醇-聚丙二醇共聚物、聚乳酸-乙二醇共聚物、聚乳酸-丙二醇共聚物、大豆油、或环氧大豆油中的一种或多种。上述增塑剂可以单独使用,也可以两种以上组合使用。
所述的增容剂,可以列举出含有环氧官能团、异氰酸酯官能团、碳化二亚胺官能团、酸酐官能团、硅烷官能团、唑啉官能团、或亚磷酸酯官能团中的一种或多种的化合物,且该化合物中含有上述官能团的总数为两个以上。具体而言,增容剂可以是甲苯二异氰酸酯、二苯甲烷二异氰酸酯、对苯二亚甲基二异氰酸酯、己二异氰酸酯、异佛尔酮二异氰酸酯、二环己基甲烷二异氰酸酯、赖氨酸三异氰酸酯、γ-缩水甘油醚氧丙基三甲氧基硅烷、聚碳化二亚胺、乙烯-丙烯酸酯-马来酸酐三元共聚物、或带有环氧官能团的丙烯酸酯类聚合物中的一种或多种。
所述的封端剂,可以列举出含有环氧官能团、异氰酸酯官能团、碳化二亚胺官能团、酸酐官能团、硅烷官能团、唑啉官能团、或亚磷酸酯官能团中的一种的化合物,且该化合物中含有上述官能团的总数为一个。
本发明所述的取向薄膜,具有土壤降解性,即根据ASTM D5988-18规定的条件进行土埋降解性评价时,在24个月内相对生物降解率达到90%以上。
本发明所述的取向薄膜,生物质度为90%以上,优选的,生物质度为95%以上,进一步优选为98%以上。
所述的取向薄膜,其厚度没有特别限定,一般的,可以为1μm~5mm。
所述的取向薄膜,还可以再经过热处理来制备。
此外,为了提高印刷性、层压适应性、涂布适应性等的目的,本发明所述的取向薄膜还可以实施各种表面处理。作为表面处理的方法,可举出电晕放电处理、等离子处理、火焰处理、酸处理、离型处理等。
本发明还提供由上述取向薄膜制备的多层薄膜。所述的多层薄膜,是拥有两个以上层的薄膜。由于不同的层可以具有不同的功能,所以相比于单层薄膜,多层薄膜能提供多种多样的需求。
所述的多层薄膜,其厚度没有特别限定,一般的,可以为1μm~5mm。
进一步的,本发明所述的多层薄膜,含有蒸镀层、热封层、粘着层、接着层中的至少一种。
所述的蒸镀层是由选自由金属、金属氧化物及二氧化硅组成的组中的至少1种的蒸镀材料形成,因此,通过存在这样的蒸镀层,能够抑制水分或氧气、二氧化碳等气体进出,用于提高基体薄膜的阻隔性、力学性能以及外观。
所述的热封层是包含热塑性或热固性树脂的膜层,该膜层在较低的加热、加压条件下,通过熔融、凝固的方式与对置的膜层连接,用于形成密封结构。
所述的粘着层是包含粘接后能被较轻易的再次分离的胶粘剂的固态、半固态或液态层状材料,如丙烯酸酯类、橡胶类、聚氨酯类胶粘剂等,用于连接多层薄膜的不同的层或连接多层薄膜与其它物品。
所述的接着层是包含可通过加热或其他方式实现固化的固态、半固态或液态层状材料,该类材料与上述粘着层的区别是接着固化后无法轻易的分离,该接着层包含固化类胶粘剂、热固性树脂、热塑性树脂中的一种或多种,该接着层用于连接多层薄膜的不同的层。
进一步的,本发明所述的多层薄膜,为了提供更好的阻隔性,水蒸气渗透系数为10g·μm/m2以下,优选5g·μm/m2以下。
进一步的,本发明所述的多层薄膜,为了提供更好的阻隔性,氧气渗透系数为1000cc·μm/m2以下,优选500cc·μm/m2以下。
本发明还提供使用上述取向薄膜的包装材料薄膜。
本发明还提供使用上述取向薄膜的胶带。
本发明还提供使用上述多层薄膜的包装材料薄膜。
本发明还提供使用上述多层薄膜的胶带。
本发明所述的取向薄膜具有快速生物降解的能力,受土壤掩埋后,会快速降解,不会较长期的留存在土壤中,同时该取向薄膜又可以通过通用的取向薄膜的制备方法制备,制备工艺简单,生产性好,且具有优异的诸如强度、尺寸均匀性等性能。本发明所述的多层薄膜,以及使用所述生物降解树脂薄膜的包装材料薄膜、胶带等制品,力学性能、光学性能、阻隔性能良好。
具体实施方式
通过下面给出的本发明的具体实施例以及对比例可以进一步清楚地了解本发明,但本发明的范围不因此局限于下述实施例。
实施例与对比例中所使用的材料如下所示:
A1:聚乳酸,美国Natureworks公司制,规格:4032D,数均分子量11万。
A2:聚乳酸,美国Natureworks公司制,规格:4060D,数均分子量11万。
B1:聚3-羟基丁酸酯,宁波天安制,规格:Y3000。
B2:聚3-羟基丁酸-3-羟基己酸酯,购自清华大学,3-羟基丁酸/3-羟基辛酸=90/10。
C:多环氧官能团化合物,BASF制,规格:Joncryl ADR4468。
实施例与对比例中所使用的原料、样品依据下述的实验方法进行测试。除非具体指明,否则测试条件一律为23℃。
形貌观察:使用超薄切片机制备样品的厚度约70nm或70nm以下的超薄片,然后通过透射电子显微镜(TEM)观察超薄片,区分连续相和分散相。使用图像处理软件,统计100个分散相面积S,并按以下公式计算分散相的直径d(一种等价的直径,即与分散相面积相等的圆的直径),并计算出样品的分散相平均直径dn。
熔点和熔融焓:使用TA公司制Q2000型差示扫描量热仪(DSC)对双向拉伸倍率为1.5×1.5的样品进行10℃/min的升温过程,记录监测到的所有峰值温度的最高值为样品的熔点,记录监测到的所有熔融峰的熔融焓之和为样品的熔融焓。
生产性:按以下实施例和对比例中记载的方法对样品进行双向拉伸。每个拉伸倍率下,取模压品10张,分别进行拉伸,8次以上成功制备取向薄膜的,则判定可在该拉伸倍率下生产取向薄膜,记为○;否则判定为不可在该拉伸倍率下生产取向薄膜,记为×。生产性的判断:可在3×3下生产的,判定为生产性优,记为◎;不可在3×3下生产,但可在2×2下生产的,判定为生产性良,记为○;仅可在1.5×1.5下生产的,判定为生产性中,记为△;仅可在1.5×1.5下生产的,判定为生产性差,记为×。
使用一台TOYOSEIKI产C4150-01型密炼机,将原料于180℃、100rpm下密炼6min。继而,使用一台TOYOSEIKI公司产MINI TEST PRESS型模压机,将生物降解树脂于180℃模压、冰水淬火,制备成厚度为200μm的模压品,继而使用Bruckner公司产KARO-IV型双向拉伸机,于80℃,5%/s的拉伸速率下,分别进行同时1×1、2×2、3×3双向拉伸后,于100℃,3min热处理后制得厚度为22μm的取向薄膜。
拉伸强度、断裂伸长率:由DUMBBELL SD-100测试片制作机制作尺寸为:150mm×10mm的试验片。由日本岛津制作所制拉伸试验机AG-IS 1KN测定试验片的拉伸强度和断裂伸长率,截距为50mm,拉伸速度为100mm/min。测试重复数为5。
生物质度:根据样品成分,将成分中生物来源的有机物的重量份记为M,将成分中非生物来源的有机物的重量份记为N。按下式计算生物质度:
生物质度=M/(M+N)×100%.
土壤降解性:根据ASTM D5988-18规定的条件进行土壤解性评价。在24个月内相对生物降解率达到90%以上的为具有土壤降解性,记为○;否则为不具有土壤降解性,记为×。
厚度:使用三洋仪器公司7050型厚度计测定,取9个数据的平均值。
水蒸气渗透系数:将厚度为T的样品,使用美国AMETEK MOCON公司3/34G型号的水蒸气透过率测试仪,测试环境是38℃、90%RH,根据标准ASTM F1249-13测试水蒸气透过率(WVTR)。按下式计算水蒸气渗透系数:
水蒸气渗透系数=T×WVTR
氧气渗透系数:将厚度为T的样品,使用美国AMETEK MOCON公司2/22H型号的氧气透过率测试仪,测试环境是20℃、0%RH,根据标准ASTM D3985-17测试氧气透过率(OTR)。按下式计算水蒸气渗透系数:
氧气渗透系数=T×OTR
实施例1~14、对比例1~5
使用一台TOYOSEIKI产C4150-01型密炼机,按表1~3所示,将原料于180℃、100rpm下密炼6min。继而,使用一台TOYOSEIKI公司产MINI TEST PRESS型模压机,将生物降解树脂于180℃模压、冰水淬火,制备成厚度为200μm的模压品,继而使用Bruckner公司产KARO-IV型双向拉伸机,于80℃,5%/s的拉伸速率下,分别进行同时1.5×1.5、2×2、3×3双向拉伸后,于100℃,3min热处理后制得厚度为22μm的取向薄膜。对取向薄膜进行各性能测试,结果列于表1~2。
可见,本发明所述的生物降解树脂、生物降解树脂薄膜,兼备生物降解速度快和储存稳定的特点,且生物质度高。另外,生物降解树脂薄膜透明性好。
可以在各实施例所述的取向薄膜上按照需求,再追加一层或多层的蒸镀层、热封层、粘着层、接着层等功能性层。可以通过对蒸镀层的设计,以达到水蒸气渗透系数为10g·μm/m2以下,优选5g·μm/m2以下;氧气渗透系数为1000cc·μm/m2以下,优选500cc·μm/m2以下的性能。
Claims (19)
1.一种取向薄膜,其特征在于,含有聚乳酸和聚羟基烷酸酯,且以聚乳酸为100重量份计,聚羟基烷酸酯为100~300重量份。
2.根据权利要求1所述的取向薄膜,其特征在于,以聚乳酸为100重量份计,聚羟基烷酸酯为151~300重量份。
3.根据权利要求1所述的取向薄膜,其特征在于,所述的聚羟基烷酸酯是选自聚羟基丁酸脂和羟基丁酸脂的共聚物构成的组中的一种或多种。
4.根据权利要求1所述的取向薄膜,其特征在于,所述的聚乳酸是连续相。
5.根据权利要求1所述的取向薄膜,其特征在于,所述的聚羟基烷酸酯是分散相,且聚羟基烷酸酯相的平均直径为3μm以下。
6.根据权利要求1所述的取向薄膜,其特征在于,熔点为150℃以下。
7.根据权利要求1所述的取向薄膜,其特征在于,熔点为151℃以上。
8.根据权利要求1所述的取向薄膜,其特征在于,熔融焓为10~30J/g。
9.根据权利要求1所述的取向薄膜,其特征在于,熔融焓为31~60J/g。
10.根据权利要求1所述的取向薄膜,其特征在于,根据ASTM D5988-18规定的条件进行土壤降解性评价时,在24个月内相对生物降解率达到90%以上。
11.根据权利要求1所述的取向薄膜,其特征在于,生物质度为90%以上。
12.含有权利要求1~11中任一项所述的取向薄膜的多层薄膜。
13.根据权利要求12所述的多层薄膜,其特征在于,含有蒸镀层、热封层、粘着层、接着层中的至少一种。
14.根据权利要求12所述的多层薄膜,其特征在于,水蒸气渗透系数为10g·μm/m2以下。
15.根据权利要求12所述的多层薄膜,其特征在于,氧气渗透系数为1000cc·μm/m2以下。
16.使用权利要求1~11任一项所述的取向薄膜的包装材料薄膜。
17.使用权利要求1~11任一项所述的取向薄膜的胶带。
18.使用权利要求12~15任一项所述的多层薄膜的包装材料薄膜。
19.使用权利要求12~15任一项所述的多层薄膜的胶带。
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