CN112602515A - 一种透明多层可生物降解聚酯农膜及其制备方法和应用 - Google Patents
一种透明多层可生物降解聚酯农膜及其制备方法和应用 Download PDFInfo
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- CN112602515A CN112602515A CN202011326602.8A CN202011326602A CN112602515A CN 112602515 A CN112602515 A CN 112602515A CN 202011326602 A CN202011326602 A CN 202011326602A CN 112602515 A CN112602515 A CN 112602515A
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- agricultural film
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Abstract
本发明公开了一种透明多层可生物降解聚酯农膜,所述农膜包括:外层的支撑层,中间的阻水层和内层的可控水解层,所述可控水解层中包含药剂等成分。本发明通过将所述三层不同树脂混合物经螺杆共挤出后,吹塑冷却成型,即可制得上述透明多层可生物降解聚酯农膜。本发明还公开了所述透明多层可生物降解聚酯农膜在农业生产中的应用,所述农膜同时具备保温、保湿及控草防虫作用,节省人力劳动,提高农业生产效率。
Description
技术领域
本发明属于高分子材料加工领域,具体涉及一种透明多层可生物降解聚酯农膜及其制备方法和应用。
背景技术
农用地膜是农业生产中重要的生产资料之一,具有保水保墒、促进增收的效果。我国作为一个农业大国,是世界上农膜消耗最多、覆盖面积最大的国家。农膜覆盖技术在给我国农业生产带来巨大效率的同时,也给土壤带来严重的污染。可生物降解聚酯农膜能够在使用后一段时间内被土壤微生物降解掉,能够较好地解决传统农膜带来的污染问题。例如,中国专利文献CN104072953B介绍了PBAT/PGA/助剂的可控降解的农用地膜,发现农膜在170天后基本无明显农膜碎片。中国专利文献CN103087482A报导了由PBAT/PLA/淀粉/助剂组成的农膜,发现该农膜符合EN13432法规,能够完全降解。
用于农用地膜可生物降解树脂有PBAT、PLA、PPC等。聚碳酸亚丙酯PPC,又称为聚甲基乙撑碳酸酯,它是以二氧化碳和环氧丙烷为原料合成的一种完全可降解的环保型塑料,英文全称Polypropylene carbonate,英文缩写PPC,又称为聚甲基乙撑碳酸酯,它是以二氧化碳和环氧丙烷为原料合成的一种完全可降解的环保型塑料。其具有较好的水汽阻隔性能。PBAT属于热塑性生物降解塑料,是己二酸、丁二醇和对苯二甲酸的三元共聚物,是一种半结晶型聚合物,综合了脂肪族聚酯的优异降解性能和芳香族聚酯的良好力学性能。PBAT的加工性能与LDPE非常相似,是一种良好的膜材料。
LLA为左旋丙交酯,是PLA合成的最主要单体,meso-LA为内消旋丙交酯,其聚合物性能差,易水解,不用于PLA合成,一般作为副产物,回收后可重新用于生产丙交酯。
农膜从外观上看一般包含透明膜和不透明两大类,不透明黑色地膜可以降低地面温度,抑制杂草生长;透明地膜可以保温增湿,加快作物生长。
现有农膜主要包括黑色地膜和透明地膜,前者不透光,所以可以控制杂草生长,后者透光可以帮助土地增温增湿。还没有一种同时实现控草和增温增湿的地膜。
发明内容
为了解决现有技术存在的上述不足,本发明的目的是提供一种透明多层可生物降解聚酯农膜(可生物降解多层农用地膜),能够在保温增湿的同时、抑制杂草生长。同时还能自动缓释出农药制剂;节省人力劳动,提高农业生产效率。
本发明提供了一种透明多层可生物降解聚酯农膜,所述农膜包括三层:外层的支撑层,中间的阻水层和内层的水解层,所述水解层中包含药剂成分。
其中,所述内层的水解层的材料包含PLA树脂100重量份、亲水性聚合物2-30重量份、以及药剂成分1-25重量份;优选地,所述内层的水解层的材料包含PLA树脂100重量份、亲水性聚合物5-20重量份、以及药剂成分2-20重量份。
所述PLA树脂由meso-LA和LLA开环共聚合所得。
所述meso-LA和LLA共聚单体的摩尔比例为10:90~45:55;优选地,为20:80~30:70。
所述PLA树脂的数均分子量在50000-90000;优选地,为60000-80000。
所述亲水性聚合物为PEG、PVA、淀粉的一种或多种。
所述药剂的成分为除草剂、杀虫剂、植物生长调节剂等中的一种或多种。
所述水解层的膜厚度为2-5μm。
本发明设计的水解层由LLA和meso-LA开环共聚而成,LLA和meso-LA根据不同的单体混合比例以及不同的嵌段结构进行共聚,因此可以控制并调节它的降解速度,土壤中散发水汽被阻水层所阻隔,并且持续作用在水解层上,促进水解层PLA逐步降解,而水解层的PLA由meso-LA和LLA以共聚单体摩尔比例为10:90~45:55时制备时,降解速度适当,能有效且缓慢释放出农业药剂,持续改善农作物生长。
其中,所述外层的支撑层包含以下原料组份:生物可降解聚合物树脂100重量份、无机填料0-40重量份。
进一步的,所述外层的支撑层还添加了如下重量份的物质:基于生物可降解聚合物树脂重量0.1-1%wt的增溶剂、基于生物可降解聚合物树脂重量0.1-2%wt的UV稳定剂、基于生物可降解聚合物树脂重量0.1-2%wt的抗老化剂等。
所述生物可降解聚合物树脂包含PBAT和PLA,所述PBAT和PLA两者的质量比例为95:5-65:35;优选地,为85:15-70:30。
所述增溶剂选自多官能环氧化合物。
所述多官能环氧化合物为甲基丙烯酸缩水甘油醚和其它烯类单体通过双键聚合制备的共聚物,可以选自市售产品joncryl ADR4400、joncryl ADR4370、KLE-4370、LotaderAX8900等中的一种或几种。
所述无机填料选自滑石粉、蒙脱土、高岭土、白垩、碳酸钙、二氧化硅、硅灰石中的一种或几种;优选地,为滑石粉、碳酸钙。
所述UV稳定剂选自UV-123、UV-3896、UV-328中的一种或几种。
所述抗老化剂选自抗氧剂1010、抗氧剂1076、抗氧剂168中的一种或多种的混合物。
其中,所述支撑层的膜厚为2-5μm;优选地,为3-4μm。
本发明所述外层支撑层的作用主要是给地膜提供强度,赋予地膜拉伸强度、耐穿刺性能、抗老化性能,同时PBAT/PLA原料具有较好的透光性,可以增加地膜下温度,促进农作物生长。
其中,所述中间阻水层包含以下原料组分及质量配比:PPC树脂100重量份、蜡2-5重量份、环氧大豆油2-5重量份、无机填料0-10重量份。
所述蜡和环氧大豆油总份数不超过10重量份,同时蜡和环氧大豆油、无机填料总份数不超过15重量份。
所述蜡选自石蜡、植物蜡、蜂蜡中的一种或几种。
所述无机填料选自滑石粉、蒙脱土、高岭土、白垩、碳酸钙、二氧化硅、硅灰石中的一种或几种;优选地,为滑石粉、碳酸钙。
所述中间阻水层的膜厚为1-5μm;优选地,为3-4μm。
本发明所述中层所用树脂是聚碳酸亚丙酯PPC,所述PPC树脂具有良好的阻隔性能,可以保证地膜的增湿增温效果,PPC玻璃化温度较高,所以添加少量的蜡、环氧大豆油,可以增加中间层的韧性,同时亲油性的蜡、环氧大豆油填充物可以缓慢的迁移到中间层外面,保护中间层,提高中间层的耐水解性,同时也能进一步起到阻水作用。但是蜡、环氧大豆油、无机填料用量不能过高,PPC树脂100重量份时,蜡和环氧大豆油总份数不超过10重量份,同时蜡和环氧大豆油、无机填料总份数不超过15重量份,否则会影响中间层的阻隔性能。
本发明还提供了所述透明多层可生物降解聚酯农膜在农业生产中的应用。
本发明中设计的这种三层透明复合农膜,使得农膜,能够在保温增湿的同时、抑制杂草生长。中间的阻水层一方面阻挡水份蒸发,给农作物增温增湿,增湿的同时促使内层水解层可控降解,并缓释出农药制剂,提高了施药的效率,节省施药的人力劳动,提高农业生产效率。另一方面,可降解聚酯易水解,而阻水层显著减少了外层支撑层的水解作用,支撑层更加持久的保持了多层膜的力学性能。
附图说明
图1是本发明透明多层可生物降解聚酯农膜的截面示意图。
图2是本发明农膜配方例1水解层PLA分子量、残留药剂量变化趋势图。
图3是本发明农膜配方例1多层膜拉伸强度变化曲线。
图4是本发明农膜配方例2水解层PLA分子量、残留药剂量变化趋势图。
图5是本发明农膜配方例2多层膜拉伸强度变化曲线。
图6是本发明农膜配方例3水解层PLA分子量、残留药剂量变化趋势图。
图7是本发明农膜配方例3多层膜拉伸强度变化曲线。
图8是PBAT/PLA单层膜力学性能变化曲线。
具体实施方式
结合以下具体实施例和附图,对本发明作进一步的详细说明。实施本发明的过程、条件、实验方法等,除以下专门提及的内容之外,均为本领域的普遍知识和公知常识,本发明没有特别限制内容。
实施例1-3
本发明所述透明多层可生物降解聚酯农膜的制备步骤如下:
(1)分别按照表2-4所示农膜各层配方,包括外层的支撑层,中间的阻水层和内层的水解层,将原料充分干燥,分别按照其中组分重量比,计量后加入混合机分别混合分散均匀,获得三层膜材料的混合料。
(2)将三层膜材料的混合料加入双螺杆挤出机挤出造粒,获得三层膜材料的专用料;
(3)将外层的支撑层,中间的阻水层和内层的水解层的专用料,对应三层共挤挤出机的外层、中层、内层,经挤出吹塑冷却成型,即可获得所述透明多层可生物降解聚酯农膜。
本发明所述的透明多层可生物降解聚酯农膜膜制备方法中,步骤(2)中,所述双螺杆挤出机的工艺参数为:1区~5区与机头的温度分别如下表1所示:
表1
1区 | 2区 | 3区 | 4区 | 5区 | 机头 | |
支撑层 | 160-170℃ | 170-200℃ | 170-200℃ | 170-200℃ | 180-190℃ | 170-180℃ |
阻水层 | 145-155℃ | 150-160℃ | 150-160℃ | 150-160℃ | 140-155℃ | 150-160℃ |
水解层 | 160-180℃ | 170-180℃ | 170-180℃ | 170-180℃ | 170-190℃ | 170-180℃ |
多层农膜制备后完成后,在自然环境下,覆盖在土壤表面,定期取样,测试一段时间内农膜力学性能的变化,以及农膜中残留药剂量的变化。
表2农膜配方例1
外层支撑层 | PBAT | PLA | 增溶剂A | 滑石粉 | UV-123 | 抗氧剂1076 |
配方用量/份 | 70 | 30 | 0.003 | 10 | 0.1 | 0.1 |
中间阻水层 | PPC | 液体石蜡 | 环氧大豆油 | 碳酸钙粉末 | ||
配方用量/份 | 100 | 3 | 5 | 5 | ||
内层水解层 | PLA* | PEG2000 | 杀虫剂 | 除草剂 | 植物生长调节剂 | |
配方用量/份 | 100 | 15 | 5 | 5 | 1 |
其中,PLA*为水解层PLA,由meso-LA和LLA两种单体共聚而成,meso-LA和LLA的摩尔比例为20:80,数均分子量为58000。
增容剂A为苯乙烯-甲基丙烯酸缩水甘油醚共聚物,环氧当量为400g/mol,Mn=3500,Mw=9120。
由表2农膜配方制备的透明多层可生物降解聚酯农膜,在吹塑成型后,对多层膜进行测试,所测试的多层膜的支撑层厚度为5μm,阻水层厚度为3μm,水解层厚度为4μm。测试结果如图2和图3所示:图2显示出内层水解层在140天内逐步降解,水解层中的农药制剂缓慢均匀的释放。图3显示出中间阻水层有效保护了支撑层,降低了支撑层的水解,多层膜的力学性能保持较好。
表3农膜配方例2
外层支撑层 | PBAT | PLA | 增溶剂B | 滑石粉 | UV-328 | 抗氧剂1010 |
配方用量/份 | 95 | 5 | 0.003 | 0 | 0.1 | 0.1 |
中间阻水层 | PPC | 液体石蜡 | 环氧大豆油 | 碳酸钙粉末 | ||
配方用量/份 | 100 | 3 | 5 | 5 | ||
内层水解层 | PLA* | 淀粉 | PEG2000 | 杀虫剂 | 除草剂 | 植物生长调节剂 |
配方用量/份 | 100 | 10 | 10 | 5 | 5 | 1 |
其中,PLA*为水解层PLA,由meso-LA和LLA两种单体共聚而成,meso-LA和LLA的摩尔比例为10:90,数均分子量为60000。
增容剂B为BASF市售产品joncrylADR4400(苯乙烯-甲基丙烯酸缩水甘油醚-丙烯酸酯共聚物),环氧当量为438g/mol,Mn=3101,Mw=7520。
由表3农膜配方制备的透明多层可生物降解聚酯农膜,在吹塑成型后,对多层膜进行测试,所测试的多层膜的支撑层厚度为4.5μm,阻水层厚度为3.5μm,水解层厚度为3μm。测试结果如图4和图5所示:图4显示出内层水解层在200天内逐步降解,水解层中的农药制剂缓慢均匀的释放。因为水解层中PLA制备时,meso-LA用量减少,水解速度降低,因此,由配方2制备的农膜相比由配方1制备的农膜中农药制剂释放的更缓慢一些,200天后多层膜中残留药剂35%,更适合生长周期长,施药周期长的农作物。图5显示出中间阻水层有效保护了支撑层,降低了支撑层的水解,多层膜的力学性能保持较好。
表4农膜配方例3
其中,PLA*为水解层PLA,由meso-LA和LLA两种单体共聚而成,meso-LA和LLA的摩尔比例为45:55,数均分子量为75000。
增容剂C为BASF市售产品joncrylADR4370(苯乙烯-甲基丙烯酸缩水甘油醚-丙烯酸酯共聚物),环氧当量为378g/mol,Mn=3805,Mw=7921。
由表4农膜配方制备的透明多层可生物降解聚酯农膜,在吹塑成型后,对多层膜进行测试,所测试的多层膜的支撑层厚度为4.8μm,阻水层厚度为3.1μm,水解层厚度为3.5μm。测试结果如图6和图7所示:图6显示出内层水解层在140天内逐步降解,水解层中的农药制剂缓慢均匀的释放。因为水解层中PLA制备时,meso-LA用量较高,meso-LA和LLA的摩尔比例为45:55,水解速度较快,因此,由配方3制备的农膜相比由配方2制备的农膜中农药制剂释放的更快,140天后多层膜中残留药剂11%,更适合生长周期短,施药周期短的农作物。图7显示出中间阻水层有效保护了支撑层,降低了支撑层的水解,多层膜的力学性能保持较好。
农作物种植时应用测试结果:
上述3个实施例配方所制备的农膜,在农作物田间使用后可增加地积温10℃左右,农膜覆盖周期中,除草效果能够达到99%以上,农作物在生长周期间无需额外增施除草剂,即能有效抑制杂草,无需再次增施杀虫剂,几乎没有病虫害,农作物增产效果显著。
对比例1
无阻水层保护下,单层支撑层PBAT/PLA膜的性能会快速降低,对比测试结果如下:
PBAT:70Phr
PLA:30Phr
增容剂A:0.003Phr
滑石粉:25Phr
UV-328:0.1Phr
抗氧剂1010:0.1Phr
按照上述配方,将原料充分干燥,计量后加入混合机混合分散均匀,将混合料加入双螺杆挤出机挤出;再吹塑冷却成型,获得对比测试的单层农膜,吹出的单层PBAT/PLA膜厚度为11μm。
双螺杆挤出机的工艺参数与多层膜加工时,支撑层的挤出工艺相同:
单层PBAT/PLA膜,在自然环境下,覆盖在土壤表面,定期取样,测试一段时间内农膜力学性能的变化,结果如图8所示:图8结果表明在没有阻水层的情况下,支撑层会在水汽作用下,更快的发生水解,从而导致力学性能降低,膜更加容易损坏。
由此可见,本发明实施例1-3显示内层水解层及中间阻隔层的配合起到了农业药剂缓释的作用,减少了施药量,提升并获得了持续的施药效果。
本发明的保护内容不局限于以上实施例。在不背离本发明构思的精神和范围下,本领域技术人员能够想到的变化和优点都被包括在本发明中,并且以所附的权利要求书为保护范围。
Claims (10)
1.一种透明多层可生物降解聚酯农膜,其特征在于,所述农膜包括:外层的支撑层,中间的阻水层、和内层的水解层,所述水解层中包含药剂成分。
2.如权利要求1所述的可生物降解聚酯农膜,其内层的水解层的材料包含PLA树脂100重量份、亲水性聚合物2-30重量份、以及药剂成分1-25重量份,其特征在于,所述PLA树脂由内消旋丙交酯meso-LA和LLA开环共聚合所得,所述meso-LA和LLA两种共聚单体的摩尔比例为10:90~45:55。
3.如权利要求2所述的可生物降解聚酯农膜,其特征在于,所述内层的水解层的PLA树脂的数均分子量在50000-90000;所述亲水性聚合物为PEG、PVA、淀粉的一种或多种;所述药剂的成分为除草剂、杀虫剂、植物生长调节剂中的一种或多种。
4.如权利要求1所述的可生物降解聚酯农膜,其特征在于,所述外层的支撑层包含以下原料组份:生物可降解聚合物树脂100重量份、无机填料0-40重量份;其中,所述生物可降解聚合物树脂包含PBAT和PLA,所述PBAT和PLA的质量比为95:5-65:35。
5.如权利要求4所述的可生物降解聚酯农膜,其特征在于,所述无机填料选自滑石粉、蒙脱土、高岭土、白垩、碳酸钙、二氧化硅、硅灰石中的一种或几种。
6.如权利要求4所述的可生物降解聚酯农膜,其特征在于,所述外层的支撑层还包括如下重量份的物质:基于所述生物可降解聚合物树脂重量0.1-1%wt的增溶剂、基于所述生物可降解聚合物树脂重量0.1-2%wt的UV稳定剂、基于所述生物可降解聚合物树脂重量0.1-2%wt的抗老化剂。
7.如权利要求1所述的可生物降解聚酯农膜,其特征在于,所述中间的阻水层包含以下原料组分及质量配比:聚碳酸亚丙酯PPC树脂100重量份、蜡2-5重量份、环氧大豆油2-5重量份、无机填料0-10重量份。
8.如权利要求7所述的可生物降解聚酯农膜,其特征在于,所述蜡和环氧大豆油总份数不超过10重量份,同时所述蜡和环氧大豆油、无机填料总份数不超过15重量份。
9.如权利要求7所述的可生物降解聚酯农膜,其特征在于,所述蜡选自石蜡、植物蜡、蜂蜡中的一种或几种。
10.如权利要求1-9之任一项所述的透明多层可生物降解聚酯农膜在农业生产中的应用。
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