CN114891251A - 一种高阻隔、可降解农用保水地膜及制备方法 - Google Patents
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Abstract
本发明涉及农用地膜的技术领域,提供了一种高阻隔、可降解农用保水地膜及制备方法。该方法以微米级粒径的层状氨基黏土负载纳米级粒径的层状六方氮化硼,然后以1H,1H,2H,2H‑全氟癸基硫醇进行表面修饰,得到具有疏水性的片层状的表面修饰复合填料,再将该复合填料分散于PBAT的二氯甲烷溶液中,并进行流延成膜,制得高阻隔、可降解的PBAT农用地膜。一方面,片层状填料可有效延长水蒸汽在薄膜中的扩散路径,另一方面,复合填料的疏水性可进一步阻碍水蒸汽透过薄膜,因此,本发明制得的PBAT农用地膜具有良好的保水性。
Description
技术领域
本发明属于农用地膜的技术领域,提供了一种高阻隔、可降解农用保水地膜及制备方法。
背景技术
农用地膜不仅可以提高地温、保水、保土、保肥,而且可以灭草、防病虫、抑盐保苗、改进近地面光热条件,能够有效增加农业生产效益,在现代化农业中具有重要地位。聚乙烯地膜较为常用,其存在难以降解的问题,使用后的残膜留在土壤中,导致土壤质量下降。为解决这一问题,可降解地膜应运而生。
可降解地膜按照降解类型主要分为光降解、生物降解、光-生物降解等。其中,生物降解地膜主要是利用自然界中的微生物实现降解,这类材料又分为天然生物降解地膜(如淀粉、蛋白质、纤维素等)和合成生物降解地膜(如聚乳酸、聚乙醇酸、聚己内酯、聚羟基脂肪酸酯、聚己二酸对苯二甲酸丁二醇酯等)。
聚己二酸对苯二甲酸丁二醇酯(PBAT)是一种热塑性生物降解塑料,兼具聚己二酸丁二醇酯(PBA)和聚对苯二甲酸丁二醇酯(PBT)的特性,在具有优良生物可降解性的同时,还有着较好的延展性、断裂伸长率、耐热性和抗冲击性。因此,PBAT成为目前生物降解塑料中具有发展前景的材料之一。
然而,PBAT薄膜自身的水汽阻隔性能较差,用于地膜时水蒸汽透过率高,保水性差,限制了其作为农用地膜的应用。
发明内容
可见,PBAT地膜具有水蒸汽透过率高、保水性差的缺陷。针对这种情况,本发明提出一种高阻隔、可降解农用保水地膜及制备方法,通过添加低表面能修饰的负载六方氮化硼的氨基黏土,可降低PBAT地膜的水蒸汽透过率,提高保水性能。
为实现上述目的,本发明涉及的具体技术方案如下:
一种高阻隔、可降解农用保水地膜的制备方法,所述农用保水地膜制备的具体步骤如下:
(1)将微米级粒径的层状氨基黏土、纳米级粒径的层状六方氮化硼加入甲苯中,调节pH值为9-10,超声分散一定时间,再过滤,真空干燥,得到负载六方氮化硼的氨基黏土,即微纳米复合填料;
(2)将微纳米复合填料加入1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中,先搅拌一定时间,然后静置一定时间,再过滤,真空干燥,得到表面修饰复合填料;
(3)将聚己二酸对苯二甲酸丁二醇酯加入二氯甲烷中,搅拌至充分溶解,加入表面修饰复合填料,搅拌均匀,然后进行流延成膜,二氯甲烷完全挥发后喷洒去离子水,揭膜,真空干燥,得到所述农用保水地膜。
公知的,氨基黏土和六方氮化硼均为片层状结构。其中,六方氮化硼由B原子和N原子共价连接而成,在边缘或缺陷部位的B原子具有空轨道,具有与有机配体发生络合的能力,而氨基黏土的表面含有大量-NH2,可提供孤对电子。因此,本发明采用氨基黏土与六方氮化硼进行络合,并且,氨基黏土为微米级,六方氮化硼为纳米级,二者络合后,六方氮化硼负载于氨基黏土的表面,形成具有微纳米结构的片层状复合填料。另外,试验表明,氨基黏土与六方氮化硼的络合与pH值有关,增大pH值有利于二者的络合,优选的pH值为9-10。
优选的,步骤(1)中,所述氨基黏土包括但不限于镁氨基黏土、钙氨基黏土、铝氨基黏土、铁氨基黏土、铜氨基黏土、锌氨基黏土、锰氨基黏土中的一种或几种。
优选的,步骤(1)中,所述氨基黏土的粒径为100-150μm,所述六方氮化硼的粒径为100-300nm。
进一步优选的,步骤(1)中,氨基黏土、六方氮化硼、甲苯的质量比为30-40:4-8:100。
优选的,步骤(1)中,所述超声分散的超声频率为25-30kHz,分散时间为2-4h。
步骤(2)采用1H,1H,2H,2H-全氟癸基硫醇对微纳米复合填料进行表面修饰,1H,1H,2H,2H-全氟癸基硫醇与微纳米复合填料之间可形成氢键结合,降低复合填料的表面能。步骤(2)得到的表面修饰复合填料既具有微纳米粗糙结构,又具有低表面能,因而具有良好的疏水性能。
优选的,步骤(2)所述1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的质量浓度为3-5%,该溶液的用量为微纳米复合填料质量的至少10倍。
优选的,步骤(2)中,所述搅拌的时间为5-10min,所述静置的时间为20-30min。
步骤(3)是配制成膜液及流延成膜的过程,PBAT在二氯甲烷中搅拌至充分溶解,所需时间为3h左右。优选的,步骤(3)中,聚己二酸对苯二甲酸丁二醇酯、表面修饰复合填料、二氯甲烷的质量比为3-5:0.1-0.2:100。
本发明还提供了上述制备方法制备得到的高阻隔、可降解农用保水地膜。与现有技术相比,有益效果在于:首先,本发明在PBAT地膜中添加了层状氨基黏土,层状氨基黏土可阻碍水蒸汽透过,水蒸汽在PBAT薄膜中扩散时需绕过层状氨基黏土,因而可有效延长水蒸汽在薄膜中的扩散路径,从而降低水蒸汽透过率;进一步的,本发明在微米级层状氨基黏土表面负载了纳米级六方氮化硼,构建了微纳米粗糙结构,再以含氟物质进行表面修饰,赋予复合填料低表面能,使复合填料具有良好的疏水性,从而可进一步阻碍水蒸汽透过薄膜。因此,本发明制得的PBAT可降解地膜具有良好的保水性能。
具体实施方式
以下通过具体实施方式对本发明作进一步的详细说明,但不应将此理解为本发明的范围仅限于以下的实例。在不脱离本发明上述方法思想的情况下,根据本领域普通技术知识和惯用手段做出的各种替换或变更,均应包含在本发明的范围内。
实施例1
(1)将微米级粒径的氨基黏土、纳米级粒径的六方氮化硼加入甲苯中,调节pH值为10,超声分散2h,再过滤,真空干燥,得到负载六方氮化硼的氨基黏土,即微纳米复合填料;氨基黏土、六方氮化硼、甲苯的质量比为30:4:100;
(2)将微纳米复合填料加入质量浓度为4%的1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中,先搅拌10min,然后静置20min,再过滤,真空干燥,得到表面修饰复合填料;1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的用量为微纳米复合填料质量的15倍;
(3)将聚己二酸对苯二甲酸丁二醇酯加入二氯甲烷中,搅拌至充分溶解,加入表面修饰复合填料,搅拌均匀,然后进行流延成膜,二氯甲烷完全挥发后喷洒去离子水,揭膜,真空干燥,得到厚度为0.01mm的农用保水地膜;聚己二酸对苯二甲酸丁二醇酯、表面修饰复合填料、二氯甲烷的质量比为5:0.1:100。
实施例2
(1)将微米级粒径的氨基黏土、纳米级粒径的六方氮化硼加入甲苯中,调节pH值为9,超声分散3h,再过滤,真空干燥,得到负载六方氮化硼的氨基黏土,即微纳米复合填料;氨基黏土、六方氮化硼、甲苯的质量比为34:5:100;
(2)将微纳米复合填料加入质量浓度为4%的1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中,先搅拌5min,然后静置30min,再过滤,真空干燥,得到表面修饰复合填料;1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的用量为微纳米复合填料质量的15倍;
(3)将聚己二酸对苯二甲酸丁二醇酯加入二氯甲烷中,搅拌至充分溶解,加入表面修饰复合填料,搅拌均匀,然后进行流延成膜,二氯甲烷完全挥发后喷洒去离子水,揭膜,真空干燥,得到厚度为0.01mm的农用保水地膜;聚己二酸对苯二甲酸丁二醇酯、表面修饰复合填料、二氯甲烷的质量比为5:0.13:100。
实施例3
(1)将微米级粒径的氨基黏土、纳米级粒径的六方氮化硼加入甲苯中,调节pH值为10,超声分散3h,再过滤,真空干燥,得到负载六方氮化硼的氨基黏土,即微纳米复合填料;氨基黏土、六方氮化硼、甲苯的质量比为37:7:100;
(2)将微纳米复合填料加入质量浓度为4%的1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中,先搅拌7min,然后静置25min,再过滤,真空干燥,得到表面修饰复合填料;1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的用量为微纳米复合填料质量的12倍;
(3)将聚己二酸对苯二甲酸丁二醇酯加入二氯甲烷中,搅拌至充分溶解,加入表面修饰复合填料,搅拌均匀,然后进行流延成膜,二氯甲烷完全挥发后喷洒去离子水,揭膜,真空干燥,得到厚度为0.01mm的农用保水地膜;聚己二酸对苯二甲酸丁二醇酯、表面修饰复合填料、二氯甲烷的质量比为5:0.17:100。
实施例4
(1)将微米级粒径的氨基黏土、纳米级粒径的六方氮化硼加入甲苯中,调节pH值为9,超声分散4h,再过滤,真空干燥,得到负载六方氮化硼的氨基黏土,即微纳米复合填料;氨基黏土、六方氮化硼、甲苯的质量比为40:8:100;
(2)将微纳米复合填料加入质量浓度为4%的1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中,先搅拌8min,然后静置25min,再过滤,真空干燥,得到表面修饰复合填料;1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的用量为微纳米复合填料质量的12倍;
(3)将聚己二酸对苯二甲酸丁二醇酯加入二氯甲烷中,搅拌至充分溶解,加入表面修饰复合填料,搅拌均匀,然后进行流延成膜,二氯甲烷完全挥发后喷洒去离子水,揭膜,真空干燥,得到厚度为0.01mm的农用保水地膜;聚己二酸对苯二甲酸丁二醇酯、表面修饰复合填料、二氯甲烷的质量比为5:0.2:100。
对比例1
制备过程中,未使用纳米级粒径的六方氮化硼,直接将微米级粒径的氨基黏土加入1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中并进行后续制备过程,其他制备条件与实施例4一致。
对比例2
制备过程中,未使用1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液进行表面修饰,直接以未表面修饰的微纳米复合填料进行后续制备过程,其他制备条件与实施例4一致。
上述实施例和对比例中,使用的氨基黏土为铁氨基黏土,粒径范围为100-120μm;使用的六方氮化硼的平均粒径为250nm;使用的PBAT中,己二酸丁二醇酯、对苯二甲酸丁二醇酯的摩尔比例为1:1,PBAT的数均分子量为7.2×104。
水蒸汽透过率测试:参照GB/T 1037-2021,使用水蒸气透过率测试仪进行测试。将上述实施例和对比例的地膜分别切割成面积为33.2cm2的圆形样品,将样品与适量的超纯水一起放入样品架,置于测试仪的样品室内,测试每个样品的水蒸气透过率,每个样品测试2次计算平均值。测试参数为:输出气压为4-5MPa,自动干燥过滤器的压力为0.3-0.35MPa,温度为38℃,相对湿度为90%。所得数据如表1所示。
表1:
Claims (10)
1.一种高阻隔、可降解农用保水地膜的制备方法,其特征在于,所述农用保水地膜制备的具体步骤如下:
(1)将微米级粒径的层状氨基黏土、纳米级粒径的层状六方氮化硼加入甲苯中,调节pH值为9-10,超声分散一定时间,再过滤,真空干燥,得到负载六方氮化硼的氨基黏土,即微纳米复合填料;
(2)将微纳米复合填料加入1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液中,先搅拌一定时间,然后静置一定时间,再过滤,真空干燥,得到表面修饰复合填料;
(3)将聚己二酸对苯二甲酸丁二醇酯加入二氯甲烷中,搅拌至充分溶解,加入表面修饰复合填料,搅拌均匀,然后进行流延成膜,二氯甲烷完全挥发后喷洒去离子水,揭膜,真空干燥,得到所述农用保水地膜。
2.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(1)中,所述氨基黏土包括但不限于镁氨基黏土、钙氨基黏土、铝氨基黏土、铁氨基黏土、铜氨基黏土、锌氨基黏土、锰氨基黏土中的一种或几种。
3.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(1)中,所述氨基黏土的粒径为100-150μm,所述六方氮化硼的粒径为100-300nm。
4.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(1)中,氨基黏土、六方氮化硼、甲苯的质量比为30-40:4-8:100。
5.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(1)中,所述超声分散的超声频率为25-30kHz,分散时间为2-4h。
6.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(2)所述1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的质量浓度为3-5%。
7.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(2)中,所述1H,1H,2H,2H-全氟癸基硫醇的乙醚溶液的用量为微纳米复合填料质量的至少10倍。
8.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(2)中,所述搅拌的时间为5-10min,所述静置的时间为20-30min。
9.根据权利要求1所述一种高阻隔、可降解农用保水地膜的制备方法,其特征在于:步骤(3)中,聚己二酸对苯二甲酸丁二醇酯、表面修饰复合填料、二氯甲烷的质量比为3-5:0.1-0.2:100。
10.权利要求1-9任一项所述制备方法制备得到的高阻隔、可降解农用保水地膜。
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