CN113601929A - 一种高性能农用大棚膜 - Google Patents
一种高性能农用大棚膜 Download PDFInfo
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- CN113601929A CN113601929A CN202110875920.8A CN202110875920A CN113601929A CN 113601929 A CN113601929 A CN 113601929A CN 202110875920 A CN202110875920 A CN 202110875920A CN 113601929 A CN113601929 A CN 113601929A
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Abstract
本案涉及一种高性能农用大棚膜，其包括内层、中层和外层；内层由茂金属线性聚乙烯、线性低密度聚乙烯和增强型防雾无滴剂制成；中层原料包括高压聚乙烯、滑石粉、无机纳米粉体、复合防雾无滴助剂；外层由线性低密度聚乙烯、可降解聚酯、酚类抗氧剂和光稳定剂制成。本案以线性低密度聚乙烯作为大棚膜基础树脂，采用三层共挤出制备具有内中外结构的大棚膜；外层通过在线性低密度聚乙烯中添加含氟硅的可降解聚酯，极大的提高了普通聚乙烯膜的抗撕裂强度和透光性；中层利用纳米蒙脱土‑纤维素有效提高流滴性；内层通过添加茂金属聚乙烯以提高膜的力学性能和光学性能；利用纳米蒙脱土‑纤维素与预辐照的聚丙烯挤出造粒，进一步有效延长棚膜流滴时效。
Description
技术领域
本发明涉及塑料膜领域，具体为一种高性能农用大棚膜。
背景技术
农用大棚膜是现代农业中常用的生产工具，是我国塑料工业中的重要组成部分。将农用大棚膜搭配竹结构或钢结构的框架形成一个温室空间，不仅能促进作物生长、早熟、增长，同时也使得人们可以吃到反季节蔬菜。农用塑料主要以聚氯乙烯(PVC)和聚乙烯(PE)为原料，PVC棚膜应用于上个世纪60年代，然而PVC膜不能燃烧处理，易产生有毒气体逐渐被市场淘汰；PE膜透光性好且无毒，但耐候性和保温性较差，使用寿命短。茂金属聚乙烯分子结构规整，相对分子质量分布窄、支链少，因而力学强度和光学性能表现较为优异，是新一代的线型低密度聚乙烯，目前已被应用于农用大棚膜上。然而，较窄的茂金属聚乙烯的加工性能较差，在吹塑时常出现膜泡不稳定、熔体破裂等情况，挤出造粒时也更加困难。
目前普遍使用的PE单层吹塑膜的机械性能较差，通过添加各种功能助剂有望提高各方面的性能，但也会出现各种助剂之间，助剂与基础树脂之间的相容性差的问题。而有些大棚膜虽然机械强度得以提升，但相应的又带来棚膜雾度提高、韧性变差等问题。因此，如何提高大棚膜的机械强度，同时保证消雾流滴效果以及抗撕裂性是目前大棚膜制备的关键。
发明内容
针对现有技术中的不足之处，本发明通过内中外三层共挤技术制备大棚膜，其以聚乙烯为基础树脂，通过添加其它具备高强度、耐候性、消雾防滴性的材料，使制得的大棚膜具备优异的综合性能。
为实现上述目的，本发明提供如下技术方案：
一种高性能农用大棚膜，包括内层、中层和外层；其中，内层由10～20份茂金属线性聚乙烯、50～70份线性低密度聚乙烯和10～15份增强型防雾无滴剂制成；中层原料包括50～70份高压聚乙烯、2～8份滑石粉、5～8份无机纳米粉体、5～10份复合防雾无滴助剂；外层由50～70份线性低密度聚乙烯、20～30份可降解聚酯、0.5～1.5份酚类抗氧剂和0.5～1.0份光稳定剂制成；其中，
所述可降解聚酯的结构式如下：
所述复合防雾无滴助剂是以纳米蒙脱土为载体插层有改性纤维素制得的材料。
进一步地，所述复合防雾无滴助剂的制备过程为：
1)将一定量的羟乙基纤维素溶于水中，随后加入一定量的丙烯酸丁酯继续搅拌至完全溶解；将溶解好的单体溶液升温至30～40℃，加入一定量的过硫酸铵绝热反应，反应完成后用乙醇清洗，并用丙酮抽提产物，得到接枝改性的羟乙基纤维素；
2)将接枝改性的羟乙基纤维素分散在水中，加入0.1mol/L的氢氧化钠溶液调节pH值至7～8；随后将其在搅拌条件下滴加至蒙脱土悬浮液中，升高温度至60℃，搅拌反应5～6h，离心、水洗、干燥、研磨得纳米蒙脱土-纤维素；即复合防雾无滴助剂。
进一步地，所述羟乙基纤维素、丙烯酸丁酯和过硫酸铵的质量比为1:8～12:0.01。
进一步地，所述蒙脱土悬浮液的配制方法为：将纳米蒙脱土粉按照5wt％的质量分数分散在水中，超声搅拌均匀，随后加入十六烷基三甲基溴化铵，搅拌过夜即得。
进一步地，所述增强型防雾无滴剂是由所述复合防雾无滴助剂与聚丙烯共挤出制得的。
进一步地，所述增强型防雾无滴剂是将预辐照好的聚丙烯与所述复合防雾无滴助剂按照0.5～1:1.5的质量比一同加入到双螺杆挤出机熔融共混后挤出制得。
进一步地，所述无机纳米粉体选自纳米SiO2，纳米CaCO3、纳米TiO2中的一种或多种。
与现有技术相比，本发明的有益效果是：以线性低密度聚乙烯作为大棚膜基础树脂，采用三层共挤出制备具有内中外三层结构的大棚膜；通过三层结构使大棚膜具备优异的流滴性、高强度和消雾性、高透光性。
外层通过在线性低密度聚乙烯中添加含氟硅的可降解聚酯，极大的提高了普通聚乙烯膜的抗撕裂强度和透光性；聚酯材料降解性能好，添加至聚乙烯膜中对环境不会造成影响；抗氧剂和光稳定剂保证大棚膜具备耐候性和耐老化性，有效延长使用寿命。
中层利用羟乙基纤维素接枝疏水性单体丙烯酸丁酯，得到一种两亲性大分子聚合物；丙烯酸丁酯的长侧链能够提高纤维素与蒙脱土的插层反应，同时疏水侧链之间产生疏水缔合作用，易于形成分子间的网状结构，从而有利于维持纳米蒙脱土-纤维素复合材料结构稳定性，在分子迁移过程中有效提高流滴性。
内层通过在线性低密度聚乙烯中添加茂金属聚乙烯以提高膜的力学性能和光学性能；利用纳米蒙脱土-纤维素与预辐照的聚丙烯挤出造粒，使得纳米蒙脱土-纤维素与聚乙烯具有适中的相容性，在制成棚膜时，使之向棚膜表面迁移的速率适中，进一步有效延长棚膜流滴时效。
具体实施方式
下面将结合实施例对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
此外，下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
一种高性能农用大棚膜，包括内层、中层和外层；其中，内层由10～20份茂金属线性聚乙烯、50～70份线性低密度聚乙烯和5～10份复合防雾无滴助剂制成；中层原料包括50～70份高压聚乙烯、2～8份滑石粉、5～8份无机纳米粉体、10～15份增强型防雾无滴剂；外层由50～70份线性低密度聚乙烯、20～30份可降解聚酯、0.5～1.5份酚类抗氧剂和0.5～1.0份光稳定剂制成；其中，
所述复合防雾无滴助剂可通过如下步骤制得：
1)将一定量的羟乙基纤维素溶于水中，随后加入一定量的丙烯酸丁酯继续搅拌至完全溶解；将溶解好的单体溶液升温至30～40℃，加入一定量的过硫酸铵绝热反应，反应完成后用乙醇清洗，并用丙酮抽提产物，得到接枝改性的羟乙基纤维素；
2)将纳米蒙脱土粉按照5wt％的质量分数分散在水中，超声搅拌均匀，随后加入十六烷基三甲基溴化铵，搅拌过夜得蒙脱土悬浮液；
3)将接枝改性的羟乙基纤维素分散在水中，加入0.1mol/L的氢氧化钠溶液调节pH值至7～8；随后将其在搅拌条件下滴加至蒙脱土悬浮液中，升高温度至60℃，搅拌反应5～6h，离心、水洗、干燥、研磨得纳米蒙脱土-纤维素，即复合防雾无滴助剂；
所述增强型防雾无滴剂是在上述复合防雾无滴助剂挤出上复合聚丙烯制得：
4)将预辐照好的聚丙烯与所述纳米蒙脱土-纤维素一同加入到双螺杆挤出机熔融共混后挤出制得纳米粒料，即增强型防雾无滴剂。
羟乙基纤维素表面含有大量羟基，是一种水溶性纤维素，在纤维素表面接枝疏水性单体丙烯酸丁酯，得到一种两亲性大分子聚合物；丙烯酸丁酯的长侧链能够提高纤维素与蒙脱土的插层反应，同时疏水侧链之间产生疏水缔合作用，易于形成分子间的网状结构，从而有利于维持纳米蒙脱土-纤维素复合材料结构稳定性，在分子迁移过程中有效提高内层膜的流滴性。
再利用纳米蒙脱土-纤维素与预辐照的聚丙烯挤出造粒，使得纳米蒙脱土-纤维素与聚乙烯具有适中的相容性，在制成棚膜时，使之向棚膜表面迁移的速率适中，进一步有效延长棚膜流滴时效。
所述可降解聚酯的结构式如下：
在以优选实施例中，其聚合反应如下：在氮气氛围下，将氟硅乙烯基单体和MPDL按照2:8的摩尔比添加到反应瓶中，加入引发剂AIBN和溶剂四氢呋喃，在60℃下搅拌反应24h，聚合物在无水乙醚中沉淀，真空干燥即得。通过GPC检测分子量Mn＝10400g/mol，PDI＝1.56，通过核磁检测m/n比值3/1。
上述反应中的氟硅乙烯基单体通过如下反应方程式制得：
上述反应中的MPDL结构式为：
其可依据文献Chem.Rev.2017,117,1319-1406合成。
由于MPDL的反应活性较低，通过提高反应体系中的MPDL投料量来提高聚合物中聚酯结构的含量，同时使聚合物倾向于无规共聚物，从而使聚合物主链降解更加彻底。引入的聚酯结构可以使后续制备的大棚膜具备更高的透光性能，而通过与氟硅乙烯基单体的共聚也使得大棚膜具备更高的拉伸强度，抗撕裂能力得以提升。氟硅乙烯基单体以硅原子为中心，氟原子以三氟甲基形式连接于单体末端，在迁移的过程中伸向棚膜的内侧，加快水蒸气转化为流滴铺展于棚膜表面，从而起到消雾的作用。
实施例1：
按照羟乙基纤维素、丙烯酸丁酯和过硫酸铵的质量比为1:8:0.01制备复合防雾无滴助剂。
按照预辐照好的聚丙烯与所述纳米蒙脱土-纤维素的质量比为0.5：1制备增强型防雾无滴剂。
内层：10份茂金属线性聚乙烯、50份线性低密度聚乙烯和10份增强型防雾无滴剂；
中层：50份高压聚乙烯、4份滑石粉、5份无机纳米粉体(纳米CaCO3、纳米TiO2)、5份复合防雾无滴助剂；
外层：50份线性低密度聚乙烯、20份可降解聚酯、0.5份酚类抗氧剂和0.5份光稳定剂。
将内中外三层的原料分别混匀，采用三层共挤吹膜机吹塑成型，得内中外三层结构厚度比为1:3:1的大棚膜。
实施例2：
按照羟乙基纤维素、丙烯酸丁酯和过硫酸铵的质量比为1:10:0.01制备复合防雾无滴助剂。
按照预辐照好的聚丙烯与所述纳米蒙脱土-纤维素的质量比为0.8：1制备增强型防雾无滴剂。
内层：15份茂金属线性聚乙烯、60份线性低密度聚乙烯和13份增强型防雾无滴剂；
中层：60份高压聚乙烯、6份滑石粉、6份无机纳米粉体(纳米CaCO3、纳米SiO2)、8份复合防雾无滴助剂；
外层：60份线性低密度聚乙烯、25份可降解聚酯、1.0份酚类抗氧剂和0.7份光稳定剂。
将内中外三层的原料分别混匀，采用三层共挤吹膜机吹塑成型，得内中外三层结构厚度比为2:5:2的大棚膜。
实施例3：
按照羟乙基纤维素、丙烯酸丁酯和过硫酸铵的质量比为1:10:0.01制备复合防雾无滴助剂。
按照预辐照好的聚丙烯与所述纳米蒙脱土-纤维素的质量比为0.9：1制备增强型防雾无滴剂。
内层：20份茂金属线性聚乙烯、70份线性低密度聚乙烯和15份增强型防雾无滴剂；
中层：70份高压聚乙烯、8份滑石粉、8份无机纳米粉体(纳米CaCO3、纳米SiO2)、10份复合防雾无滴助剂；
外层：70份线性低密度聚乙烯、30份可降解聚酯、1.5份酚类抗氧剂和1份光稳定剂。
将内中外三层的原料分别混匀，采用三层共挤吹膜机吹塑成型，得内中外三层结构厚度比为2:5:2的大棚膜。
对比例1：
可降解聚酯制备工艺同上，其中，将单体MPDL替换成BMDO(同样文献Chem.Rev.2017,117,1319-1406合成)，其余条件不变。
其余成分及含量同实施例1。
对比例2：
可降解聚酯制备工艺同上，其中，在氟硅乙烯基单体的制备过程中将3,3,3-三氟-1-丙醇替换成四氟丙醇，其余条件同实施例1。
对比例3：
复合防雾无滴助剂和增强型防雾无滴剂为直接采用未经丙烯酸丁酯接枝改性的纤维素与蒙脱土复合；其余条件同实施例1。
对比例4：
同实施例1，区别在于将内层原料中的增强型防雾无滴剂用复合防雾无滴助剂代替，并去除外层中的可降解聚酯。
分别对实施例1-3以及对比例1-4制备得到的大棚膜进行性能测试，性能测试结果见表1。
透光率按照GB/T 2410-2008测试，拉伸性能按照GB/T 1040.3-2006测试；撕裂强度按照GB/T 16578.2-2009测试；老化后断裂伸长保持率是将棚膜试样制成哑铃型拉伸条，60℃下得紫光照射4h，再在50℃冷凝4h，循环进行1000h，将老化后的试样按照GB/T1040-2006测试，所测结果除以老化前的断裂伸长率。棚膜防雾无滴持效时间测试：在水浴锅中放入一装有400ml去离子水的大烧杯，然后将大棚膜覆盖在杯口上，记录膜表面出现水珠的时间。
表1
从表1中可以看出本案实施例1-3制备的大棚膜在各项性能上较优；对比例1和对比例2在可降解聚酯制备的单体选择上有所区别，以BMDO替换MPDL，苯环位置或氟位置的改变造成聚合物链中空间位阻增大或氢键能力减弱，拉伸强度和抗撕裂能力有所下降；对比例3采用未经复合的纤维素制备复合防雾无滴剂，没有丙烯酸丁酯的长侧链在其中起到的疏水缔合作用，导致无滴效果减弱，而对比例4中可以看到与聚丙烯共挤出制得的增强型防雾无滴剂可以有效延长棚膜的流滴时效。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。
Claims (7)
1.一种高性能农用大棚膜，其特征在于，包括内层、中层和外层；其中，内层由10～20份茂金属线性聚乙烯、50～70份线性低密度聚乙烯和10～15份增强型防雾无滴剂制成；中层原料包括50～70份高压聚乙烯、2～8份滑石粉、5～8份无机纳米粉体、5～10份复合防雾无滴助剂；外层由50～70份线性低密度聚乙烯、20～30份可降解聚酯、0.5～1.5份酚类抗氧剂和0.5～1.0份光稳定剂制成；其中，
所述可降解聚酯的结构式如下：
m＞n＞10；
所述复合防雾无滴助剂是以纳米蒙脱土为载体插层有改性纤维素制得的材料。
2.如权利要求1所述的高性能农用大棚膜，其特征在于，所述复合防雾无滴助剂的制备过程为：
1)将一定量的羟乙基纤维素溶于水中，随后加入一定量的丙烯酸丁酯继续搅拌至完全溶解；将溶解好的单体溶液升温至30～40℃，加入一定量的过硫酸铵绝热反应，反应完成后用乙醇清洗，并用丙酮抽提产物，得到接枝改性的羟乙基纤维素；
2)将接枝改性的羟乙基纤维素分散在水中，加入0.1mol/L的氢氧化钠溶液调节pH值至7～8；随后将其在搅拌条件下滴加至蒙脱土悬浮液中，升高温度至60℃，搅拌反应5～6h，离心、水洗、干燥、研磨得纳米蒙脱土-纤维素；即复合防雾无滴助剂。
3.如权利要求2所述的高性能农用大棚膜，其特征在于，所述羟乙基纤维素、丙烯酸丁酯和过硫酸铵的质量比为1:8～12:0.01。
4.如权利要求2所述的高性能农用大棚膜，其特征在于，所述蒙脱土悬浮液的配制方法为：将纳米蒙脱土粉按照5wt％的质量分数分散在水中，超声搅拌均匀，随后加入十六烷基三甲基溴化铵，搅拌过夜即得。
5.如权利要求1所述的高性能农用大棚膜，其特征在于，所述增强型防雾无滴剂是由所述复合防雾无滴助剂与聚丙烯共挤出制得的。
6.如权利要求5所述的高性能农用大棚膜，其特征在于，所述增强型防雾无滴剂是将预辐照好的聚丙烯与所述复合防雾无滴助剂按照0.5～1:1.5的质量比一同加入到双螺杆挤出机熔融共混后挤出制得。
7.如权利要求1所述的高性能农用大棚膜，其特征在于，所述无机纳米粉体选自纳米SiO2，纳米CaCO3、纳米TiO2中的一种或多种。
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