CN115260711A - 一种耐水解高阻隔性可生物降解薄膜及其制备方法 - Google Patents
一种耐水解高阻隔性可生物降解薄膜及其制备方法 Download PDFInfo
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Abstract
本发明属于降解薄膜材料技术领域,公开了一种耐水解高阻隔性可生物降解薄膜及其制备方法。所述耐水解高阻隔性可生物降解薄膜含有PBAT/PPC的组合物,按重量份数计,含有52‑75份PBAT、5‑20份PPC、5‑20份改性蒙脱土填料、1‑3份硅油类物质、1‑4份抗水解剂、2‑3份相容剂、0.1‑2份抗氧剂和0.1‑2份润滑剂。其中添加的改性层状蒙脱土大幅降低了生产成本并提高了薄膜的阻水能力,抗水解剂为复配抗水解剂,耐湿热能力比单一添加明显提高,硅油与基体相容性不好,向材料表面迁移,在复合薄膜表面形成一层疏水层,三者的协同作用大幅提高复合材料的耐久性和阻水性,机械性能衰减慢,使用寿命长,用其包装产品,可以有效延长产品货架期。
Description
技术领域
本发明涉及降解薄膜材料技术领域,具体是涉及一种耐水解高阻隔性可生物降解薄膜及其制备方法。
背景技术
聚己二酸对苯二甲酸丁二酯(PBAT)因含柔性的脂肪链和刚性的芳香链而具有高韧性和耐高温性,是目前市场应用最好的降解材料之一。然而,PBAT树脂制得的膜袋产品在储存和使用过程中,由于微生物、光照、辐射、空气及所接触的物质环境的作用,在储存和使用过程比较容易发生降解,极大的影响了产品的使用寿命,同时其较差的阻水和阻氧性能也一直被人们所诟病。
中国专利CN 106750438公开了一种阻氧/阻水PBAT薄膜材料,通过溶液固化法在PBAT薄膜表面涂覆一层含有活性基团的二维片状材料(蒙脱土)的预聚物,在150℃干燥30min,得到阻水阻氧复合材料,该方法水蒸气透过率下降明显,但是工艺较为复杂,且在实际生产应用过程中,涂层受外力易脱落。中国专利申请CN 102382423公开了一种可降解聚酯用抗水解剂使用方法,发现脂肪族聚碳化二亚胺抗水解效果弱于芳香族聚碳化二亚胺,而要想达到理想的抗水解效果需要碳化二亚胺单体和聚碳化二亚胺复配。中国专利申请CN113211920公开了一种多层共挤全降解高阻隔包装薄膜及其制备方法,该包装薄膜由5层构成:第一层为外防护层A,其成分为PLA、PBAT、碳化二亚胺抗水解剂和抗紫外光剂的共混物;第二层为粘合层B,其成分为PLA和多活性官能团增容剂的共混物;第三层为高阻隔层C,其成分为PGA;第四层为粘合层D,其成分为PLA和多活性官能团增容剂的共混物;第五层为热封层E,其成分为PLA和PCL的共混物。该方法加工较为复杂且设备昂贵,生产成本高,对各层材料延展性要求比较高。
发明内容
本发明的目的是为了克服上述背景技术的不足,提供一种耐水解高阻隔性可生物降解薄膜及其制备方法。本发明的可生物降解薄膜是一种可全降解的多层共挤高阻隔包装薄膜,其中添加的改性层状蒙脱土大幅降低了生产成本并提高了薄膜的阻水能力,抗水解剂为复配抗水解剂,耐湿热能力比单一添加明显提高,硅油与基体相容性不好,向材料表面迁移,在复合薄膜表面形成一层疏水层,三者的协同作用大幅提高复合材料的耐久性和阻水性,机械性能衰减慢,使用寿命长,用其包装产品,可以有效延长产品货架期,且本发明生产工艺简单,可用于生产购物袋、连卷袋、快递袋、垃圾袋等。
为达到本发明的目的,本发明的耐水解高阻隔性可生物降解薄膜含有PBAT/PPC的组合物,按重量份数计,所述PBAT/PPC的组合物中含有52-75份PBAT、5-20份PPC、5-20份改性蒙脱土填料、1-3份硅油类物质、1-4份抗水解剂、2-3份相容剂、0.1-2份抗氧剂和0.1-2份润滑剂。
进一步地,在本发明的一些实施例中,所述PBAT为己二酸丁二醇酯和对苯二甲酸丁二醇酯的共聚物,优选地,所述PBAT的密度为1.15-1.36g/cm3,重均分子量为50000-80000,熔点为100-130℃。
优选地,在本发明的一些实施例中,所述PPC聚碳酸亚丙酯的Mw=5.87×104g/mol,Mw/Mn=3.65。
进一步地,在本发明的一些实施例中,所述改性蒙脱土填料是通过表面改性助剂对蒙脱土填料改性,所述表面改性助剂为硬脂酸、硬脂酸盐、硅烷偶联剂、铝酸酯偶联剂、硼酸酯、钛酸酯类偶联剂中的一种或多种的混合物,优选硅烷偶联剂,以增加蒙脱土填料与树脂之间的界面结合力。进一步优选地,所述蒙脱土填料的粒径为1250-3000目。
进一步地,在本发明的一些实施例中,所述硅油类物质选自甲基硅油、甲基含氢硅油、甲基苯基硅油、甲基乙烯基硅油中的一种或多种;优选地,所述硅油类物质为甲基硅油和/或甲基含氢硅油。
进一步地,在本发明的一些实施例中,所述抗水解剂为芳香族单体的碳二亚胺与芳香族低聚和/或芳香族多聚的碳二亚胺的混合物,其中芳香族单体的碳二亚胺与芳香族低聚和/或芳香族多聚碳二亚胺之比是0.8-1.2:0.8-1.2。
进一步地,在本发明的一些实施例中,所述相容剂为苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯、苯乙烯-丙烯腈-马来酸酐共聚物、乙烯-丙烯酸酯-缩水甘油酯共聚物、乙烯-缩水甘油酯或乙烯-丙烯酸正丁酯-缩水甘油酯共聚物中的一种或多种。
进一步地,在本发明的一些实施例中,所述抗氧剂为受阻酚类抗氧剂或亚磷酸酯类抗氧剂中的一种或几种;优选地,所述抗氧剂为抗氧剂1010、抗氧剂168。
进一步地,在本发明的一些实施例中,所述润滑剂为乙烯基双硬脂酰胺、聚硅氧烷、硬脂酸钙、硬脂酸镁、硬脂酸锌、PE蜡、PP蜡中的一种或多种。
进一步地,本发明还提供了一种上述耐水解高阻隔性可生物降解薄膜的制备方法,所述方法包括以下步骤:
(1)将填料和表面改性助剂在110-140℃混合,搅拌分散均匀得改性纳米层状填料,再将改性纳米层状填料、PBAT、PPC、硅油类物质、抗水解剂、相容剂、抗氧剂和润滑剂加入到混合机中,常温混合,分散均匀;
(2)采用双螺杆挤出机将经步骤(1)充分混合后的混合物挤出造粒得到样品,冷却,切粒,烘干,得到PBAT/PPC合金;
(3)将干燥后的颗粒物通过单螺杆挤出机进行吹塑成膜。
进一步地,在本发明的一些实施例中,所述双螺杆挤出机的温度设置从加料口到机头为90-120-130-130-120-110-110-135℃,螺杆转速为180rpm;优选地,所述单螺杆挤出机的长度和直径比为20-35:1,挤出模头温度为120-140℃。
与现有技术相比,本发明的优点如下:
(1)本发明的耐水解高阻隔性可生物降解薄膜能采用一步法挤出吹塑的方法制备得到,工艺简单。
(2)本发明的耐水解高阻隔性可生物降解薄膜中添加了PPC,具有良好的透明性和阻隔性,可提高透光率和保水作用。
(3)本发明的耐水解高阻隔性可生物降解薄膜中同时还添加具有良好保水作用的蒙脱土,改性后的蒙脱土表面有大量的环氧基团,可提高与树脂的结合力,片层结构也能防止水分的快速蒸发,两者的协同作用,提高了复合膜的阻隔性能。
(4)本发明的耐水解高阻隔性可生物降解薄膜中添加硅油、相容剂和抗水解剂可提高膜的力学性能、耐水解性能,硅油随着时间的延长向表面迁移,使材料表面疏水性提高,延缓水分子进入基体,从而延长降解周期,三者协同作用,更高效的实现了膜的耐老化、耐温、保水效果,保证降解周期超过产品储存和使用周期。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。本发明的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。应当理解,以下描述仅仅用以解释本发明,并不用于限定本发明。
本文中所用的术语“包含”、“包括”、“具有”、“含有”或其任何其它变形,意在覆盖非排它性的包括。例如,包含所列要素的组合物、步骤、方法、制品或装置不必仅限于那些要素,而是可以包括未明确列出的其它要素或此种组合物、步骤、方法、制品或装置所固有的要素。
连接词“由…组成”排除任何未指出的要素、步骤或组分。如果用于权利要求中,此短语将使权利要求为封闭式,使其不包含除那些描述的材料以外的材料,但与其相关的常规杂质除外。当短语“由…组成”出现在权利要求主体的子句中而不是紧接在主题之后时,其仅限定在该子句中描述的要素;其它要素并不被排除在作为整体的所述权利要求之外。
当量、浓度、或者其它值或参数以范围、优选范围、或一系列上限优选值和下限优选值限定的范围表示时,这应当被理解为具体公开了由任何范围上限或优选值与任何范围下限或优选值的任一配对所形成的所有范围,而不论该范围是否单独公开了。例如,当公开了范围“1至5”时,所描述的范围应被解释为包括范围“1至4”、“1至3”、“1至2”、“1至2和4至5”、“1至3和5”等。当数值范围在本文中被描述时,除非另外说明,否则该范围意图包括其端值和在该范围内的所有整数和分数。
本发明要素或组分前的不定冠词“一种”和“一个”对要素或组分的数量要求(即出现次数)无限制性。因此“一个”或“一种”应被解读为包括一个或至少一个,并且单数形式的要素或组分也包括复数形式,除非所述数量明显只指单数形式。
此外,下面所描述的术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不是必须针对相同的实施例或示例。而且,本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。实施例所用材料均为市购,优选地,本发明实施例和对比例中采用以下原材料,但不限于这些材料:聚碳酸亚丙酯(PPC):Mw=5.87×104g/mol,Mw/Mn=3.65,河南天冠集团有限公司;聚对苯二甲酸丁二醇-己二酸丁二醇共聚酯(PBAT),牌号:TH801T,Mw=4.26×104g/mol;有机蒙脱土:DK2,浙江丰虹新材料股份有限公司;抗水解剂:芳香族单体的碳化二亚胺:Stabaxol I,芳香族多聚碳化二亚胺:Stabaxol P,上海莱恩化学有限公司。
实施例1
将水分含量≤0.2%、粒径为1250-3000目的蒙脱土加入到温度为110-140℃的高速搅拌机中以400~800r/min的速度搅拌10分钟后,加入KH-560硅烷偶联剂表面改性,表面改性助剂含量为填料的2%,再搅拌5分钟出料,得到改性蒙脱土(有机蒙脱土DK2)备用。
将PBAT75份、有机蒙脱土DK2 20份、碳化二亚胺单体I 0.5份、聚碳化二亚胺P 0.5份,甲基硅油1份、乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯(EMA-GMA)2份,加工助剂(抗氧剂1010 0.2份、抗氧剂168 0.4份、润滑剂芥酸酰胺0.4份)1份,加入到高速混合机中常温下搅拌3min,混合均匀后出料。将上述混合均匀后的物料添加到双螺杆挤出机中,在90-135℃温度下熔融挤出,冷却切粒,制得粒料;
将所述粒料加入吹膜机,吹膜机温度设定为120-140℃,收卷后的薄膜经制袋、喷胶、分切工序得到成品包装膜袋。
实施例2
本实施例与实施例1不同的是:PBAT 65.5份,PPC 10份,有机蒙脱土DK2 20份、碳化二亚胺单体I 0.5份、聚碳化二亚胺P 0.5份,甲基硅油1份、乙烯-丙烯酸甲酯-甲基丙烯酸缩水甘油酯(EMA-GMA)2份,加工助剂(抗氧剂1010 0.2份、抗氧剂168 0.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
实施例3
本实施例与实施例1不同的是:PBAT 55份,PPC 20份,有机蒙脱土DK220份、碳化二亚胺单体I 0.5份、聚碳化二亚胺P 0.5份,甲基硅油1份、EMA-GMA 2份,加工助剂(抗氧剂1010 0.2份、抗氧剂1680.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
实施例4
本实施例与实施例1不同的是:PBAT 63份,PPC 20份,有机蒙脱土DK210份、碳化二亚胺单体I 1份、聚碳化二亚胺P 1份,甲基硅油1份、EMA-GMA 2份,加工助剂(抗氧剂1010 0.2份、抗氧剂168 0.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
实施例5
本实施例与实施例1不同的是:PBAT 52份,PPC 20份,有机蒙脱土DK220份、碳化二亚胺单体I 2份、聚碳化二亚胺P2份,甲基硅油1份、EMA-GMA 2份,加工助剂(抗氧剂1010 0.2份、抗氧剂168 0.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
实施例6
本实施例与实施例1不同的是:PBAT 54份,PPC 20份,有机蒙脱土DK220份、碳化二亚胺单体I 0.5份、聚碳化二亚胺P 0.5份,甲基硅油1份、EMA-GMA 2份,加工助剂(抗氧剂1010 0.2份、抗氧剂1680.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
对比例1
本实施例与实施例1不同的是:PBAT 76份、有机蒙脱土DK2 20份、聚碳化二亚胺P 1份,加工助剂(抗氧剂1010 0.2份、抗氧剂168 0.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
对比例2
本实施例与实施例1不同的是:PBAT 74份、PPC 20份、碳化二亚胺单体I 0.5份、聚碳化二亚胺P 0.5份、EMA-GMA 2份甲基硅油1份、加工助剂(抗氧剂1010、抗氧剂168、润滑剂芥酸酰胺)1份。其它步骤和参数与实施例1相同。
对比例3
本实施例与实施例1不同的是:PBAT 56份、PPC 20份、有机蒙脱土DK220份、EMA-GMA 2份、甲基硅油1份、加工助剂(抗氧剂1010 0.2份、抗氧剂168 0.4份、润滑剂芥酸酰胺0.4份)1份。其它步骤和参数与实施例1相同。
表1各实施例和对比例材料组分表
性能测试
1.拉伸强度及断裂伸长率的测定
按照国家标准《塑料拉伸性能的测定》(GB\T1040.3-2006)第3部分,薄膜和薄片的试验条件:哑铃型样条为长度150mm,窄平行宽度为10mm的,拉伸速度为50mm/min,室温25℃。
2.湿热老化实验
将样条放入85℃,相对湿度85%的湿热老化烘箱中,实验时间24h;老化后,测试拉伸强度断裂伸长率。
3.参照GB/T 26253—2010,利用透湿仪对样品膜的水蒸气透过性进行测试。
测试结果如下
表2老化前后力学性能
表3共混薄膜的水蒸气透过率和透过系数
对比例3与实施案例3、5、6数据显示随着芳香族碳化二亚胺单体和聚碳化二亚胺含量的增加,所得到PBAT/PPC复合材料经双85湿热老化测试后,其拉伸强度衰减明显减弱,这是因为单体型碳化二亚胺和聚合型碳化二亚胺复配能够有效的减少端羧基的含量,减缓了在高湿热的条件下,PBAT发生自催化降解的程度,从而提高了PBAT/PPC复合材料的耐湿热能力。
从实施例1和对比例1可以看出硅油的加入降低了薄膜的水蒸气透过率,这是因为硅油提高了材料表面的疏水性,不利于水分子的进入,大大提高了PBAT/PPC材料的抗水解性能,延长了降解周期和使用周期。
由表3的对比例2和纯PBAT水蒸气透过率系数数据可知,PPC材料本身具有高阻水阻氧性能,在PBAT/PPC复合材料中形成一层阻隔层,同时通过对比例1可以看出随着片状蒙脱土的加入,复合材料的水蒸气透过率系数也大幅降低,这是因为片状的蒙脱土分散在基材中,形成连续的阻隔层,阻断了水分子进入基材的通路,延长了水分子进入的时间,提高了材料的耐久性和阻水能力。
本领域的技术人员容易理解,以上所述仅为本发明的实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种耐水解高阻隔性可生物降解薄膜,其特征在于,所述耐水解高阻隔性可生物降解薄膜含有PBAT/PPC的组合物,按重量份数计,所述PBAT/PPC的组合物中含有52-75份PBAT、5-20份PPC、5-20份改性蒙脱土填料、1-3份硅油类物质、1-4份抗水解剂、2-3份相容剂、0.1-2份抗氧剂和0.1-2份润滑剂。
2.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述PBAT为己二酸丁二醇酯和对苯二甲酸丁二醇酯的共聚物,优选地,所述PBAT的密度为1.15-1.36g/cm3,重均分子量为50000-80000,熔点为100-130℃。
3.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述PPC聚碳酸亚丙酯的Mw=5.87×104g/mol,Mw/Mn=3.65。
4.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述改性蒙脱土填料是通过表面改性助剂对蒙脱土填料改性,所述表面改性助剂为硬脂酸、硬脂酸盐、硅烷偶联剂、铝酸酯偶联剂、硼酸酯、钛酸酯类偶联剂中的一种或多种的混合物,优选硅烷偶联剂。
5.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述硅油类物质选自甲基硅油、甲基含氢硅油、甲基苯基硅油、甲基乙烯基硅油中的一种或多种;优选地,所述硅油类物质为甲基硅油和/或甲基含氢硅油。
6.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述抗水解剂为芳香族单体的碳二亚胺与芳香族低聚和/或芳香族多聚的碳二亚胺的混合物,其中芳香族单体的碳二亚胺与芳香族低聚和/或芳香族多聚碳二亚胺之比是0.8-1.2:0.8-1.2。
7.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述相容剂为苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯、苯乙烯-丙烯腈-马来酸酐共聚物、乙烯-丙烯酸酯-缩水甘油酯共聚物、乙烯-缩水甘油酯或乙烯-丙烯酸正丁酯-缩水甘油酯共聚物中的一种或多种。
8.根据权利要求1所述的耐水解高阻隔性可生物降解薄膜,其特征在于,所述抗氧剂为受阻酚类抗氧剂或亚磷酸酯类抗氧剂中的一种或几种;优选地,所述抗氧剂为抗氧剂1010、抗氧剂168;优选地,所述润滑剂为乙烯基双硬脂酰胺、聚硅氧烷、硬脂酸钙、硬脂酸镁、硬脂酸锌、PE蜡、PP蜡中的一种或多种。
9.权利要求1-8任一项所述的耐水解高阻隔性可生物降解薄膜的制备方法,其特征在于,所述方法包括以下步骤:
(1)将填料和表面改性助剂在110-140℃混合,搅拌分散均匀得改性纳米层状填料,再将改性纳米层状填料、PBAT、PPC、硅油类物质、抗水解剂、相容剂、抗氧剂和润滑剂加入到混合机中,常温混合,分散均匀;
(2)采用双螺杆挤出机将经步骤(1)充分混合后的混合物挤出造粒得到样品,冷却,切粒,烘干,得到PBAT/PPC合金;
(3)将干燥后的颗粒物通过单螺杆挤出机进行吹塑成膜。
10.根据权利要求9所述的耐水解高阻隔性可生物降解薄膜的制备方法,其特征在于,所述双螺杆挤出机的温度设置从加料口到机头为90-120-130-130-120-110-110-135℃,螺杆转速为180rpm;优选地,所述单螺杆挤出机的长度和直径比为20-35:1,挤出模头温度为120-140℃。
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