CN115386205A - 一种可降解抗菌园林膜及其制备方法 - Google Patents
一种可降解抗菌园林膜及其制备方法 Download PDFInfo
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- CN115386205A CN115386205A CN202211153170.4A CN202211153170A CN115386205A CN 115386205 A CN115386205 A CN 115386205A CN 202211153170 A CN202211153170 A CN 202211153170A CN 115386205 A CN115386205 A CN 115386205A
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
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- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明涉及一种可降解抗菌园林膜及其制备方法,属于功能膜制备技术领域,包括以下重量份原料:PBAT树脂70‑80份、PLA树脂20‑30份、桥联抗菌组分5‑10份、缓释增强组分1‑2份、抗氧剂1份、抗紫外剂1份、热稳定剂1份和开口剂0.5‑1份;将上述原料混合,挤出造粒,吹塑成型,得到园林膜,本发明利用PBAT树脂对PLA树脂进行增韧、PLA树脂对PBAT树脂进行补强,调节两者用量,在不牺牲可降解性能的前提下得到强度和韧性都良好的园林膜,引入桥联抗菌组分、缓释增强组,赋予所制备的园林膜具有良好的力学性能和优异的抗菌性,并且能够促进园林苗嫁接伤口的愈合与生长,具有很高的应用价值。
Description
技术领域
本发明属于功能膜制备技术领域,具体地,涉及一种可降解抗菌园林膜及其制备方法。
背景技术
园林膜是指在园林建设中使用的薄膜,其中尤为重要的是嫁接用膜。影响嫁接成活的因素有很多种,尤其是下列因素:1)苗木内在因素;2)外界环境因素);3)嫁接技术水平和新材料的应用。其中内因主要是指受植物亲缘关系远近的影响,外界环境因素主要包括:温度、湿度、空气、光线、细菌等,嫁接技术水平则体现在高效科学利用植物生长因子来提高嫁接存活率的能力,新材料的应用即体现于嫁接用膜的选择与应用。现有园林嫁接用膜一般是采用PE、PVC等高分子材料制成,虽然能够满足植株嫁接用膜基本需求,但是针对性差,一是这些嫁接用膜容易形成白色垃圾,难以降解,污染环境,二是这些嫁接用膜无抗菌性,不能保证苗木嫁接伤口生长环境的无菌性,容易引起伤口腐烂嫁接失败等现象的发生,因此,提供一种可降解抗菌园林膜是目前需要解决的技术问题。
发明内容
为了解决背景技术中提到的技术问题,本发明提供一种可降解抗菌园林膜及其制备方法。
本发明的目的可以通过以下技术方案实现:
一种可降解抗菌园林膜,包括以下重量份原料:PBAT树脂70-80份、PLA树脂20-30份、桥联抗菌组分5-10份、缓释增强组分1-2份、抗氧剂1份、抗紫外剂1份、热稳定剂1份和开口剂0.5-1份;
该可降解抗菌园林膜由以下步骤制成:
将PBAT树脂、PLA树脂、桥联抗菌组分、缓释增强组分、抗氧剂、抗紫外剂、热稳定剂和开口剂加入混合机中混合均匀后转移至双螺杆挤出机中挤出造粒,然后挤出吹塑成型,得到降解抗菌园林膜。
其中,双螺杆挤出机工作温区为120-180℃,螺杆转速70-90r/min,挤出吹塑的温度为150-200℃,吹胀比为2-8,拉伸比为1-5。
进一步地,桥联抗菌组分包括以下步骤制成:
步骤S1、将1,4-丁二醇二缩水甘油醚、2-甲基烯丙胺和无水甲醇加入圆底烧瓶中,转速500rpm搅拌反应72h,反应结束后,利用乙醚沉淀纯化,具体为:将反应产物滴加至乙醚中,转速1000rpm搅拌0.5-1h,静置4-6h,倒出乙醚,沉淀于40℃下干燥至恒重,得到中间体1,1,4-丁二醇二缩水甘油醚、2-甲基烯丙胺和无水甲醇的用量比为4mmol:4-4.15mmol:10-15mL;
步骤S2、将中间体1加入甲醇中,加入3-(二甲基氨基)-1-丙硫醇和2,2-二甲氧基-2-苯基苯乙酮,氮气保护下,紫外光(波长λ=365nm)下反应8-10h,反应结束后,利用乙醚沉淀纯化,具体操作同步骤S1,得到中间体2,中间体1、甲醇、3-(二甲基氨基)-1-丙硫醇和2,2-二甲氧基-2-苯基苯乙酮0.9-1g:6-7g:0.7g:0.1-0.5g;
步骤S3、将中间体2加入DMF中,加入三氟化硼乙醚,边搅拌边滴加环氧氯丙烷,升温至65℃,搅拌反应2-3h,旋蒸去除DMF,将旋蒸产物转移至反应器中,缓慢滴加25wt%氢氧化钠水溶液,升温至80℃保持2-3h后,旋蒸去除水分,旋蒸产物过滤,得到中间体3,中间体2、DMF、三氟化硼乙醚、环氧氯丙烷和氢氧化钠水溶液的用量比为1-1.5g:10-15mL:0.02-0.04g:0.3-0.5g:3-5mL;
步骤S4、将中间体3加入DMF中,加入溴代十二烷,氮气保护下,磁力搅拌反应48h,反应结束后,利用乙醚沉淀纯化,具体操作同步骤S1,得到桥联抗菌组分,中间体3、DMF和溴代十二烷的用量比为1.1-1.3g:10-13mL:1g。
首先使1,4-丁二醇二缩水甘油醚的氨基与2-甲基烯丙胺的环氧基发生开环反应,得到含有乙烯基侧链、多羟基和叔胺基的中间体1;然后在光引发剂的作用下,使中间体1的乙烯基侧链与3-(二甲基氨基)-1-丙硫醇的巯基发生加成反应,使中间体1再次引入叔胺结构,得到中间体2,进而在三氟化硼乙醚的催化作用下,使中间2上的羟基与环氧氯丙烷发生脱出HCl反应引入环氧基,得到中间体3,最后利用叔胺结构与溴代烃发生季铵化反应,得到桥联抗菌组分,由上述反应可知,该桥联抗菌组分为大分子结构,并且含有环氧基、季铵盐结构。
进一步地,缓释增强组分包括以下步骤制成:
将萘乙酸钠饱和溶液(在25℃下,萘乙酸钠的溶解度为53.0g/100mL)、六水合硝酸锌、九水合硝酸铝和氢氧化钠置于玛瑙罐中,然后放入行星式球磨机中,公转速度为240-260rmp,自转速度480-500rpm,球磨35-45min,球磨结束后,球磨产物减压抽滤,滤饼用去离子水冲洗分散洗涤,再次减压抽滤,将得到的滤饼置于70℃烘箱中干燥至恒重,再研磨10min,过400目筛,得到缓释增强组分;
其中,六水合硝酸锌、九水合硝酸铝、氢氧化钠和萘乙酸钠的摩尔比为2:1:6:1-1.5,萘乙酸钠是一种典型的生长类植物生产调节剂,能促进细胞分裂与扩大,作用在伤口部位,诱导植物伤口愈合,具有低浓度促进生长,高浓度抑制生长的特点,在果实等植株嫁接处直接涂抹容易造成用量较高抑制植株生长的问题出现,类水滑石是一类拥有纳米级片层结构的无机黏土,较大的比表面积带有丰富的阴离子结合位点,是有机阴离子类药物的理想载体,因此,本发明以萘乙酸钠为插层剂,六水合硝酸锌、九水合硝酸铝为原料,制备了萘乙酸钠插层类水滑石,即缓释增强组分,通过插层处理,一方面实现了萘乙酸钠的缓释,有效控制萘乙酸钠对植株的作用量,促进植株嫁接出伤口的快速愈合,克服高浓度抑制生长问题的出现;另一方面,通过插层处理使类滑石片层间拥有更多的空间,较大的层间距使分子链段更容易进入层间结构,产生更多的结合位点,从而提高其与聚合物的相容性。
进一步地,抗氧剂为抗氧剂1010、抗氧剂264和抗氧剂168中的一种或多种按照任意比例混合。
进一步地,抗紫外剂为2-(2-羟基-5-苯甲基)苯并三唑。
进一步地,热稳定剂为硬脂酸钡、硬脂酸钙和硬脂酸锌中的一种或多种按照任意比例混合。
进一步地,开口剂为油酸酰胺和芥酸酰胺中的一种。
本发明的有益效果:
1、本发明以可完全降解材料PBAT树脂、PLA树脂为基料,复配桥联抗菌组分、缓释增强组分等助剂,经过挤出造粒、吹塑形成,得到可降解抗菌园林膜,利用PBAT树脂对PLA树脂进行增韧、PLA树脂对PBAT树脂进行补强,调节两者用量,在不牺牲可降解性能的前提下得到强度和韧性都良好的园林膜。
2、本发明在园林膜中引入缓释增强组分,一方面实现了萘乙酸钠的缓释,有效控制萘乙酸钠对植株的作用量,促进植株嫁接出伤口的快速愈合,另一方面作为增强颗粒,提高园林膜的力学性能。
3、本发明在园林膜中引入桥联抗菌组分,还组分为大分子抗菌物质,含有丰富的环氧基和季铵盐结构,不仅能够通过阳离子与细胞膜上的磷脂双子层发生静电吸附进行抗菌,赋予园林膜优异的抗菌性,而且由于活性环氧基团的存在发挥桥联作用,一方面体现于高反应活性的环氧基能够与PBAT树脂、PLA树脂分子链上的羟基和羧基反应,从而实现两相聚合物的紧密结合,另一方面体现于能够与缓释增强组分表面的羟基反应,提高缓释增强组分在基体中的相容性,使缓释增强组分更好地发挥促进嫁接伤口愈合和增强园林膜力学性能的特点。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅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作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
一种桥联抗菌组分,包括以下步骤制成:
步骤S1、将4mmol 1,4-丁二醇二缩水甘油醚、4mmol 2-甲基烯丙胺和10mL无水甲醇加入圆底烧瓶中,转速500rpm搅拌反应72h,反应结束后,利用乙醚沉淀纯化,具体为:将反应产物滴加至乙醚中,转速1000rpm搅拌0.5h,静置4h,倒出乙醚,沉淀40℃下干燥至恒重,得到中间体1;
步骤S2、将0.9g中间体1加入6g甲醇中,加入0.7g3-(二甲基氨基)-1-丙硫醇和0.1g 2,2-二甲氧基-2-苯基苯乙酮,氮气保护下,紫外光(波长λ=365nm)下反应8h,反应结束后,利用乙醚沉淀纯化,具体操作同步骤S1,得到中间体2;
步骤S3、将1g中间体2加入10mL DMF中,加入0.02g三氟化硼乙醚,边搅拌边滴加0.3g环氧氯丙烷,升温至65℃,搅拌反应2h,旋蒸去除DMF,旋蒸产物转移至反应器中,缓慢滴加3mL 25wt%氢氧化钠水溶液,升温至80℃保持2h后,旋蒸去除水分,旋蒸产物过滤,得到中间体3;
步骤S4、将1.1g中间体3加入10mL DMF中,加入1g溴代十二烷,氮气保护下,磁力搅拌反应48h,反应结束后,利用乙醚沉淀纯化,具体操作同步骤S1,得到桥联抗菌组分。
实施例2
一种桥联抗菌组分,包括以下步骤制成:
步骤S1、将4mmol 1,4-丁二醇二缩水甘油醚、4.15mmol 2-甲基烯丙胺和15mL无水甲醇加入圆底烧瓶中,转速500rpm搅拌反应72h,反应结束后,利用乙醚沉淀纯化,具体为:将反应产物滴加至乙醚中,转速1000rpm搅拌1h,静置6h,倒出乙醚,沉淀于40℃下干燥至恒重,得到中间体1;
步骤S2、将1g中间体1加入7g甲醇中,加入0.7g 3-(二甲基氨基)-1-丙硫醇和0.5g2,2-二甲氧基-2-苯基苯乙酮,氮气保护下,紫外光(波长λ=365nm)下反应10h,反应结束后,利用乙醚沉淀纯化,具体操作同步骤S1,得到中间体2;
步骤S3、将1.5g中间体2加入15mL DMF中,加入0.04g三氟化硼乙醚,边搅拌边滴加0.5g环氧氯丙烷,升温至65℃,搅拌反应3h,旋蒸去除DMF,旋蒸产物转移至反应器中,缓慢滴加5mL 25wt%氢氧化钠水溶液,80℃保持3h后,旋蒸去除水分,旋蒸产物过滤,得到中间体3;
步骤S4、将1.3g中间体3加入13mL DMF中,加入1g溴代十二烷,氮气保护下,磁力搅拌反应48h,反应结束后,利用乙醚沉淀纯化,具体操作同步骤S1,得到桥联抗菌组分。
实施例3
一种缓释增强组分,包括以下步骤制成:
将萘乙酸钠饱和溶液(在25℃下,萘乙酸钠的溶解度为53.0g/100mL)、六水合硝酸锌、九水合硝酸铝和氢氧化钠置于玛瑙罐中,然后放入行星式球磨机中,公转速度为240rmp,自转速度480rpm,球磨35min,球磨结束后,球磨产物减压抽滤,滤饼用去离子水冲洗分散洗涤,再次减压抽滤,将得到的滤饼置于70℃烘箱中干燥至恒重,再研磨10min,过400目筛,得到缓释增强组分,六水合硝酸锌、九水合硝酸铝、氢氧化钠和萘乙酸钠的摩尔比为2:1:6:1。
实施例4
一种缓释增强组分,包括以下步骤制成:
将萘乙酸钠饱和溶液(在25℃下,萘乙酸钠的溶解度为53.0g/100mL)、六水合硝酸锌、九水合硝酸铝和氢氧化钠置于玛瑙罐中,然后放入行星式球磨机中,公转速度为260rmp,自转速度500rpm,球磨45min,球磨结束后,球磨产物减压抽滤,滤饼用去离子水冲洗分散洗涤,再次减压抽滤,将得到的滤饼置于70℃烘箱中干燥至恒重,再研磨10min,过400目筛,得到缓释增强组分,六水合硝酸锌、九水合硝酸铝、氢氧化钠和萘乙酸钠的摩尔比为2:1:6:1.5。
实施例5
一种可降解抗菌园林膜,包括以下重量份原料:PBAT树脂70份、PLA树脂20份、实施例1的桥联抗菌组分5份、实施例3的缓释增强组分1份、抗氧剂1份、抗紫外剂1份、热稳定剂1份和开口剂0.5份;
该可降解抗菌园林膜由以下步骤制成:
将PBAT树脂、PLA树脂、桥联抗菌组分、缓释增强组分、抗氧剂、抗紫外剂、热稳定剂和开口剂加入混合机中混合均匀后转移至双螺杆挤出机中挤出造粒,然后挤出吹塑成型,得到降解抗菌园林膜。
其中,双螺杆挤出机工作温区为120-180℃,螺杆转速70r/min,挤出吹塑的温度为150-200℃,吹胀比为2,拉伸比为3。
其中,抗氧剂为抗氧剂1010,抗紫外剂为2-(2-羟基-5-苯甲基)苯并三唑,热稳定剂为硬脂酸钡,开口剂为油酸酰胺。
实施例6
一种可降解抗菌园林膜,包括以下重量份原料:PBAT树脂75份、PLA树脂25份、实施例2的桥联抗菌组分8份、实施例3的缓释增强组分1.5份、抗氧剂1份、抗紫外剂1份、热稳定剂1份和开口剂0.8份;
该可降解抗菌园林膜由以下步骤制成:
将PBAT树脂、PLA树脂、桥联抗菌组分、缓释增强组分、抗氧剂、抗紫外剂、热稳定剂和开口剂加入混合机中混合均匀后转移至双螺杆挤出机中挤出造粒,然后挤出吹塑成型,得到降解抗菌园林膜。
其中,双螺杆挤出机工作温区为120-180℃,螺杆转速80r/min,挤出吹塑的温度为150-200℃,吹胀比为5,拉伸比为3。
其中,抗氧剂为抗氧剂264,抗紫外剂为2-(2-羟基-5-苯甲基)苯并三唑,热稳定剂为硬脂酸钙,开口剂为芥酸酰胺。
实施例7
一种可降解抗菌园林膜,包括以下重量份原料:PBAT树脂80份、PLA树脂30份、实施例2的桥联抗菌组分10份、实施例4的缓释增强组分2份、抗氧剂1份、抗紫外剂1份、热稳定剂1份和开口剂1份;
该可降解抗菌园林膜由以下步骤制成:
将PBAT树脂、PLA树脂、桥联抗菌组分、缓释增强组分、抗氧剂、抗紫外剂、热稳定剂和开口剂加入混合机中混合均匀后转移至双螺杆挤出机中挤出造粒,然后挤出吹塑成型,得到降解抗菌园林膜。
其中,双螺杆挤出机工作温区为120-180℃,螺杆转速90r/min,挤出吹塑的温度为150-200℃,吹胀比为8,拉伸比为3。
其中,抗氧剂为抗氧剂168,抗紫外剂为2-(2-羟基-5-苯甲基)苯并三唑,热稳定剂为硬脂酸锌,开口剂为芥酸酰胺。
对比例1
将实施例4中桥联抗菌组分替换成重庆临水环保科技有限公司出售的1227季铵盐杀菌剂,其原料及组分同实施例4。
对比例2
将实施例5中缓释增强组分去除,其原料及组分同实施例5。
一、将实施例5-7和对比例1-2所制备的园林膜进行测试,拉伸性能:按照标准GB/T1040-1992测试,拉伸速度为50mm/min;抗菌性能:将各组待测膜剪裁成50×50mm的薄片,按照QB/T2591-2003《抗菌塑料的抗菌性能试验方法》标准规定的贴膜法测试抗菌效果,其试验结果如表1中所示:
表1
项目 | 拉伸强度/MPa | 大肠杆菌抑菌率/% | 金黄色葡萄球菌抑菌率/% |
实施例5 | 29.7 | 99.99 | 99.99 |
实施例6 | 30.2 | 99.99 | 99.99 |
实施例7 | 30.9 | 99.99 | 99.99 |
对比例1 | 26.54 | 95.24 | 93.17 |
对比例2 | 23.22 | 98.74 | 99.05 |
由表1可以看出,相比于对比例1-2,实施例5-7由于桥联抗菌组分和缓释增强组分的引入,得到的园林膜力学性能更高,抗菌性更佳。
二、采用实施例和对比例所制备的园林膜对橡胶苗木嫁接成活率进行试验,橡胶芽条采自同种条件下培育生长的橡胶苗木枝条,砧木为抗性强、产量较高的优良品质GT1橡胶小苗(塑料培育带培育的育袋苗,生长至4蓬叶稳定期),通过人工嫁接后,缠绑各组的园林膜,每组嫁接100株,采用同样的水肥管理,嫁接后30d测试芽接成活率,芽接成活率为接穗成活珠数占总珠数的百分比,测试结果如表2所示:
表2
由表2可以看出,相比于对比例1-2,实施例5-7由于桥联抗菌组分和缓释增强组分的引入,得到的园林膜对植株的嫁接伤口愈合以及新芽生长的促进作用更佳。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”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一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (8)
1.一种可降解抗菌园林膜,其特征在于,包括以下重量份原料:PBAT树脂70-80份、PLA树脂20-30份、桥联抗菌组分5-10份、缓释增强组分1-2份、抗氧剂1份、抗紫外剂1份、热稳定剂1份和开口剂0.5-1份;
桥联抗菌组分包括以下步骤制成:
步骤S1、将1,4-丁二醇二缩水甘油醚、2-甲基烯丙胺和无水甲醇混合,搅拌反应72h,利用乙醚沉淀纯化,得到中间体1;
步骤S2、将中间体1加入甲醇中,加入3-(二甲基氨基)-1-丙硫醇和2,2-二甲氧基-2-苯基苯乙酮,氮气保护下,紫外光下反应8-10h,利用乙醚沉淀纯化,得到中间体2;
步骤S3、将中间体2加入DMF中,加入三氟化硼乙醚,边搅拌边滴加环氧氯丙烷,升温至65℃,搅拌反应2-3h,旋蒸去除DMF,将旋蒸产物转移至反应器中,缓慢滴加25wt%氢氧化钠水溶液,升温至80℃保持2-3h后,旋蒸去除水分,旋蒸产物过滤,得到中间体3;
步骤S4、将中间体3加入DMF中,加入溴代十二烷,氮气保护下,磁力搅拌反应48h,利用乙醚沉淀纯化,得到桥联抗菌组分。
2.根据权利要求1所述的一种可降解抗菌园林膜,其特征在于,步骤S1中1,4-丁二醇二缩水甘油醚、2-甲基烯丙胺和无水甲醇的用量比为4mmol:4-4.15mmol:10-15mL。
3.根据权利要求1所述的一种可降解抗菌园林膜,其特征在于,步骤S2中中间体1、甲醇、3-(二甲基氨基)-1-丙硫醇和2,2-二甲氧基-2-苯基苯乙酮0.9-1g:6-7g:0.7g:0.1-0.5g。
4.根据权利要求1所述的一种可降解抗菌园林膜,其特征在于,步骤S3中中间体2、DMF、三氟化硼乙醚、环氧氯丙烷和氢氧化钠水溶液的用量比为1-1.5g:10-15mL:0.02-0.04g:0.3-0.5g:3-5mL。
5.根据权利要求1所述的一种可降解抗菌园林膜,其特征在于,步骤S4中中间体3、DMF和溴代十二烷的用量比为1.1-1.3g:10-13mL:1g。
6.根据权利要求1所述的一种可降解抗菌园林膜,其特征在于,缓释增强组分包括以下步骤制成:
将萘乙酸钠饱和溶液、六水合硝酸锌、九水合硝酸铝和氢氧化钠混合,球磨35-45min,球磨产物减压抽滤,滤饼洗涤干燥,研磨,得到缓释增强组分。
7.根据权利要求6所述的一种可降解抗菌园林膜,其特征在于,六水合硝酸锌、九水合硝酸铝、氢氧化钠和萘乙酸钠的摩尔比为2:1:6:1-1.5。
8.根据权利要求1所述的一种可降解抗菌园林膜的制备方法,其特征在于,包括以下步骤:
将PBAT树脂、PLA树脂、桥联抗菌组分、缓释增强组分、抗氧剂、抗紫外剂、热稳定剂和开口剂混合,挤出造粒,吹塑成型,得到降解抗菌园林膜。
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