CN111422911B - 一种能够促进植物蓝光反应的纳米材料、制剂及制备方法 - Google Patents

一种能够促进植物蓝光反应的纳米材料、制剂及制备方法 Download PDF

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CN111422911B
CN111422911B CN202010138306.9A CN202010138306A CN111422911B CN 111422911 B CN111422911 B CN 111422911B CN 202010138306 A CN202010138306 A CN 202010138306A CN 111422911 B CN111422911 B CN 111422911B
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CN111422911A (zh
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王慎谦
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Xi'an Jibainong Biological Technology Co ltd
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Abstract

本发明涉及一种能够促进植物蓝光反应的纳米材料、制剂及制备方法，其克服了现有技术中转光效率低、生产和使用成本较高的问题，其能有效提高作物的光合作用效率从而达到增产的目的；并能为作物的生长补充必要的微量元素；还能抗菌防腐保鲜，提高产品品质并减少杀菌剂的使用。该纳米材料为氧化铁、氧化锌、氧化铜、氧化亚铜、氧化锰、三氧化钼、二氧化钛中的一种或两种及以上的混合物。该纳米材料制剂组成为：以重量百分比计，纳米氧化物10％‑30％，环糊精聚合物0.1％‑10％，非离子表面活性剂0.1％‑5％，聚羧酸盐分散剂0.1％‑5％，增稠剂0.1％‑3％，杀菌剂0.1％‑2％，消泡剂0.05‑5％，防冻剂0.5％‑10％，余量为水。

Description

一种能够促进植物蓝光反应的纳米材料、制剂及制备方法
技术领域：
本发明涉及一种农用纳米材料，尤其是涉及一种能够促进植物蓝光反应的纳米材料、制剂及制备方法。
背景技术：
光合作用是植物生长的基础，在此过程中植物中的叶绿素吸收太阳光的能量，将二氧化碳和水转变为有机物并释放氧气。叶绿素对太阳光吸收效率的高低将直接影响光合作用的效果。但并不是所有照射到植物表面290-3000nm的太阳光都能被植物所利用或对植物生长有益。波长290-400nm的紫外线除360nm附近的光对促进植物果实着色有益外，会使植物变矮、叶片变厚、诱使温室主要病原菌(灰霉菌和子囊菌)形成，并会诱发植物产生病虫害；而500-580nm的绿光大部分会被叶面反射而不能被利用。
叶绿素对太阳光的吸收有两个明显的吸收带，分别为400-480nm的蓝光区和600-680nm的红光区，植物主要通过对这两种光的吸收完成光合作用。其中植物吸收蓝光后的生理变化称为蓝光反应，它是光合系统活性和光合电子传递能力的重要影响因子。高等植物典型的蓝光反应有向光生长、抑制茎伸长、增加蛋白质含量、促进花色素苷积累、促进气孔开放、调节基因表达等。经研究蓝光能明显缩短蔬菜的节间距、促进蔬菜的横向伸展。同时，蓝光还能促进植株次生代谢产物的积累。
因此如果能通过光能转换，将紫外光转变为波长为400-480nm的蓝光，则首先能消除紫外光对植物的不利影响，其次能大大提高植物的光合作用效率，从而起到增产增收、改善产品品质、提早成熟等效果。具有这种光转化能力的物质称为转光剂，其相当于一种“光肥”。目前，转光剂可分为稀土无机、稀土有机配合物和有机荧光染料转光剂。使用的方法是将转光剂加入高分子中制成农膜对植物进行覆盖。但目前的转光剂和使用方式有较大的缺陷。首先稀土无机和有机转光剂价格昂贵，掺杂工艺较复杂，颗粒容易团聚失去活性。且制成农膜后与基质相容性不好而易发生相分离导致转光效率下降和荧光淬灭；而有机荧光染料转光剂大部分是具有共轭结构的大分子，往往具有一定的毒性。其次这种膜使用起来较不方便，需要通过繁重的体力劳动将膜覆盖到植物上方，生产和使用成本较高。目前也只适用于蔬菜等较矮小的植物，对于果树等高大的植物则无法实现覆膜。且膜较容易老化，难以降解，容易造成对土地的污染。
农户希望能有一种更加方便灵活的方法来使用转光剂。在土地耕种更加集中的当下，也更希望水、药、肥等农资能在最少的施用次数中同时使用，这不但能大大节约劳动力，还往往能为作物的生长带来协同作用。
发明内容：
本发明的目的在于提供一种能够促进植物蓝光反应的纳米材料、制剂及制备方法，其克服了现有技术中转光效率低、生产和使用成本较高的问题，其能有效提高作物的光合作用效率从而达到增产的目的；并能为作物的生长补充必要的微量元素；还能抗菌防腐保鲜，提高产品品质并减少杀菌剂的使用。
为实现上述目的，本发明采用的技术方案为：
一种能够促进植物蓝光反应的纳米材料，其特征在于：该纳米材料为氧化铁、氧化锌、氧化铜、氧化亚铜、氧化锰、三氧化钼、二氧化钛中的一种或两种以上的混合物，纳米材料的粒径为0.1-25nm。
所述纳米材料为微量元素与所述氧化物形成的混合物。
所述微量元素为硼、锰或钼。
混合物为机械混合物或掺杂混合物。
一种能够促进植物蓝光反应的纳米材料制剂，其特征在于：包括以重量百分比计的以下原料
纳米材料10％-30％，环糊精聚合物0.1％-10％，非离子表面活性剂0.1％-5％，聚羧酸盐分散剂0.1％-5％，增稠剂0.1％-3％，杀菌剂0.1％-2％，消泡剂0.05-5％，防冻剂0.5％-10％，余量为水；
环糊精聚合物为β-环糊精与环氧氯丙烷的水溶性聚合物，分子量为4000-100000。
一种能够促进植物蓝光反应的纳米材料制剂的制备方法，其特征在于：包括如下步骤：
按照配比将平均分子量2万的β-环糊精聚合物溶解于去离子水中，然后将所述纳米材料粉末搅拌下加入所得溶液中，25℃搅拌1小时后按顺序分别加入分散剂、表面活性剂、消泡剂、杀菌剂、增稠剂、防冻剂，并搅拌混合均匀。
与现有技术相比，本发明具有的优点和效果如下：
1、本发明的第一个优势是其转光效率高。由于喷施后其直接覆盖于叶面并形成很薄的膜，紫外线通过转光膜变为蓝光后可直接被叶面吸收利用。
2、本发明的第二个优势是上述纳米转光剂是植物生长所必须的微量元素。施用微量元素叶面肥时往往是植物生长的关键时期。如果使用具有转光效果的微量元素叶面肥，则可以实现“光肥”与叶面肥的协同作用，达到增产提质的目的。这种转光膜不但能够将紫外光转变为蓝光来保护植物并促进光合作用，而且可以实现微量元素的缓慢释放，延长肥效。
3、本发明的第三个优势是这种纳米转光剂具有光触效果，能产生具有强氧化和还原能力的电子和空穴。这些电子和空穴一方面通过光水解给叶片的光合作用补充、传递电子能量，以此来达到促进光合作用的主效果；另一方面它们能将很多叶面或果实表面的化学污染物和细菌病毒等分解为二氧化碳、水和其他无害物质。在作物表面分解污染物可以提高叶面的清洁程度从而提高光合作用效率，减少杀菌剂的使用量，并可增加水果的色泽和延长保鲜期。
4、本发明的第四个优势是与传统转光膜相比这种可喷洒的转光剂使用简单方便灵活，既可用于大棚等封闭空间，也可用于田野等开阔空间；可应用于蔬菜等低矮作物，也可用于果树等难以覆膜的高大植物。这种转光剂也不会带来转光膜那样的降解难题，它会被植物逐渐吸收或被微生物降解。
附图说明：
图1为环糊精聚合物的示意图；
图2为环糊精聚合物阻止粒子团聚示意图。
具体实施方式：
下面结合具体实施方式对本发明进行详细的说明。
本发明提供的纳米材料为铁、锌、铜、锰、钼、钛的氧化物，具体为氧化铁、氧化锌、氧化铜、氧化亚铜、氧化锰、三氧化钼、二氧化钛中的一种或两种及以上的混合物，混合的方法可以是掺杂或机械混合。这类氧化物材料中普遍存在晶格缺陷，因此存在着电子从导带底跃迁到缺陷能级或者是从缺陷能级跃迁到价带等多种跃迁方式。粒径对于上述纳米材料的转光效果影响较大，随着颗粒的增长转化后的光波长逐渐增大，蓝光成分会逐渐减少。在将粒子的粒径控制在0.1-25nm后，可以将阳光中高能量紫外光转变为植物所需的蓝光。硼的化合物虽然没有转光能力和光触效果，但可以将硼元素通过掺杂方便地混入上述氧化物中得到能促进植物蓝光反应的纳米肥料。掺杂或复合一方面可以在晶格中用掺杂的元素替代氧原子获得转光效果更好的纳米材料，另一方面可将多种植物所需的微量元素复合在一起施用。上述纳米材料可以通过共沉淀法、水热法或溶胶-凝胶法得到。
本发明还涉及上述纳米材料的一种制剂。制剂由上述纳米氧化物或氧化物与其余元素的混合物及掺杂物、表面活性剂、分散剂、环糊精聚合物、增稠剂、杀菌剂、消泡剂、防冻剂和水组成。其中上述纳米氧化物在配方中的总含量为10％-30％(以元素计)。表面活性剂为非离子表面活性剂，其作用一方面是促进纳米粒子的分散，另外一个作用是使制剂在植物叶面均匀铺展成膜，从而有利于转光膜的形成，其用量为0.1％-5％。分散剂为聚羧酸盐分散剂，用量为0.1％-5％。这类分散剂为枝化或梳状结构，能对纳米粒子形成覆盖和包裹。而其末端为带阴离子的羧基，由于静电斥力使彼此分离从而使纳米粒子均匀分布和悬浮。增稠剂首先能防止纳米粒子在制剂中聚并和沉降，其次在喷洒时能提供合适的流变性能，而在喷洒至叶面后随着水分的蒸发增稠剂能在叶面形成一层均匀的具有转光能力的膜。增稠剂可选自聚乙烯醇、黄原胶、改性淀粉、改性纤维素、海藻酸钠等，用量为0.1％-3％。杀菌剂和消泡剂的含量分别为0.1％-2％和0.05-5％，防冻剂用量为0.5％-10％，余量为水。
虽然上述制剂已使用表面活性剂、分散剂和增稠剂来防止纳米粒子的聚并和成团，但由于纳米粉体的表面能很高，储存与运输过程中团聚倾向依然十分严重，产品制备时虽呈纳米状态，但使用时往往是呈亚微米或微米状态，使得转光能力下降或得到不需要的谱线，有时甚至完全失去了转光功能。环糊精是一种具有环状空腔的多聚糖，其通过交联形成聚合物后可以形成更大的网格化的纳米空腔，且往往具有较好的水溶性。加入制剂后能使纳米转光材料颗粒进入其空腔从而彼此隔离，使其在储存和喷洒以后依然保持具有转光能力的粒径。其另外一个作用是可吸附叶面或果实表面的污染物，加速纳米粒子对污染物的光解速率。常用的环糊精聚合物是β-环糊精与环氧氯丙烷的聚合物，目前已商品化。通常的制备方法是将β-环糊精溶于10％-40％的氢氧化钠水溶液中，滴加环氧氯丙烷后在40℃-60℃来合成聚合物。当环氧氯丙烷：β-环糊精(摩尔比)＜3时，聚合物分子量约为4000-100000，可以以任意比例溶于水；当摩尔比为3-5时聚合物的分子量约为100000-150000，聚合物虽可溶于水，但粘度会随着浓度增加而较快上升；当环氧氯丙烷：β-环糊精＞5时，由于分子量往往大于150000而使聚合物形成凝胶。本发明使用的聚合物为两者摩尔比＜3的水溶性聚合物。其在上述制剂中的用量为0.1％-10％。图1和图2显示了环糊精聚合物及其阻止离子团聚的原理。
具体实施例
下面通过具体实施方式对本发明作进一步详细说明。在以下的实施方式中，很多细节描述是为了使得本申请能被更好的理解。然而，本领域技术人员可以毫不费力地认识到，其中部分特征在不同情况下是可以省略的，或者可以由其他元件、材料、方法所替代。
实施例1：制备具有转光作用的纳米氧化铁
将54克六水合氯化铁溶解于1升乙二醇中，再加入108克三水合醋酸钠，室温搅拌30分钟。然后将所得溶液密封在2升反应釜中，200℃反应20小时。产物冷却至室温，离心后用500毫升的去离子水洗涤两次，然后再用100毫升无水乙醇洗涤，离心分离后60℃烘干3小时，然后在600℃煅烧3小时，得氧化铁纳米粉末16克，平均粒径17nm。用325nm的紫外光激发可观察到420-468nm蓝色发光，其中437nm的发光峰强度最大。
实施例2：制备具有转光作用的纳米氧化锌
将90克硝酸锌溶于600克去离子水中备用，然后将50克碳酸钠溶解于500克水中。将上述两种溶液在快速搅拌下混合。将所得胶体离心后分别用100克去离子水和100克无水乙醇洗涤并离心分离。80℃干燥12小时后在500℃下煅烧5小时，得氧化锌纳米粉末38克，平均粒径21nm。用325nm的紫外光激发可观察到410-475nm蓝色发光，其中441纳米的发光峰强度最大。
实施例3：制备具有转光作用的纳米氧化铜
将60克三水合硝酸铜溶解于100克去离子水中，然后将20克氢氧化钠溶解于1升水-乙醇混合溶液(v/v＝1:1)中。将所得硝酸铜溶液缓缓加入氢氧化钠溶液中，滴加持续1小时。在室温搅拌2小时后，抽滤分离，沉淀物用500毫升去离子水洗涤，然后100℃干燥后得到纳米氧化铜粉体20克，粒径22nm。用325nm的紫外光激发可观察到414-481nm蓝色发光，其中455nm的发光峰强度最大。
实施例4：制备具有转光作用的纳米氧化亚铜
将50克五水合硫酸铜溶解于200毫升蒸馏水备用。然后将16克氢氧化钠溶解于200毫升去离子水中，并将溶液加热至60℃。搅拌下将硫酸铜溶液滴加至氢氧化钠溶液中，滴加持续1小时。然后加入2mol/L的葡萄糖溶液60毫升，60℃继续搅拌反应2小时。然后离心，并用去离子水和无水乙醇各洗涤两遍，产物于60℃干燥12小时后得到氧化亚铜纳米粉末14克，平均粒径23nm。用325nm的紫外光激发后可观察到425-500nm的发光峰，其中462nm的发光峰强度最大。
实施例5：制备具有转光作用的纳米氧化锰
将157克碳酸铵固体配成1升溶液，然后滴加至1升浓度为1mol/L的硝酸锰溶液中，静置陈化3小时后抽滤，用蒸馏水洗涤2-3次。将滤饼置于80℃鼓风干燥箱中4小时后放入马弗炉中500℃煅烧3小时。冷却后重新研磨，得到棕褐色纳米粉末71克，平均粒径为14nm。用325nm的紫外光激发后可观察到407-489nm的发光峰，其中447nm的发光峰强度最大。
实施例6：制备具有转光作用的纳米三氧化钼
将100克四水合钼酸铵溶于1升5％氨水中，然后在搅拌下滴加30％的醋酸水溶液使溶液的pH为3.50，静置24h使沉淀完全。离心后将得到的白色晶体，在120℃干燥36小时得到三氧化钼纳米粉末80克，平均粒径为19nm。用325nm的紫外光激发后可观察到427-509nm的发光峰，其中466nm的发光峰强度最大。
实施例7：制备具有转光作用的纳米二氧化钛
室温下将100克钛酸丁酯搅拌下缓慢滴加到350毫升无水乙醇中得到黄色澄清溶液A备用。将40毫升冰醋酸、100毫升蒸馏水和350毫升无水乙醇中混合均匀，然后滴入1-2滴盐酸使pH≤2.5。快速搅拌下将溶液A缓慢滴加至溶液B中，滴加持续1小时。然后加热至80℃反应1小时。离心后固体分别用300毫升去离子水和无水乙醇洗涤。固体80℃干燥6小时后在500℃煅烧3小时，得到二氧化钛纳米粉末23.5克，平均粒径25nm。用325nm的紫外光激发后可观察到404-469nm的发光峰，其中433nm的发光峰强度最大。
实施例8：制备具有转光作用的硼掺杂氧化铁纳米粉末
将九水合硝酸铁70克溶于1升去离子水，然后加入硼酸三甲酯6克，加热至60℃后在搅拌下加入3mol/L的氢氧化钠溶液直至体系pH值为11，继续在60℃搅拌反应24小时。然后将产物离心，胶体用1升去离子水洗涤后离心。然后在500℃煅烧5小时得到掺杂硼元素的氧化铁红褐色粉末15克，粒径24nm。用325nm的紫外光激发后可观察到419-479nm的发光峰，其中443nm的发光峰强度最大。
实施例9：制备具有转光作用的锰掺杂氧化锌纳米粉末
将30克硝酸锌，5克氯化锰溶于200克去离子水中备用；将21克碳酸钠溶解于110克水中。将上述两种溶液在快速搅拌下混合。将所得胶体离心后分别用100克去离子水和100克无水乙醇洗涤并离心分离。然后在500℃下煅烧5小时，得锰掺杂的氧化锌纳米粉末15.8克，平均粒径13nm。用325nm的紫外光激发可观察到410-475nm蓝色发光，其中439纳米的发光峰强度最大。
实施例10：钼掺杂二氧化钛纳米粉末的制备
搅拌下将60克钛酸四丁酯缓慢滴入150克无水乙醇中，再缓慢滴入乙酰丙酮5毫升混合均匀。然后，将100毫升蒸馏水、50毫升65％硝酸与300毫升无水乙醇混合，然后缓慢滴入不断搅拌的钛酸四丁酯乙醇溶液中。半小时后缓慢滴入6克四水合钼酸铵、10毫升65％硝酸和50毫升蒸馏水混合液，室温搅拌1小时以上，得到淡黄色透明溶液，将其静置陈化24小时。离心后用200毫升蒸馏水洗涤，然后将溶胶于80℃干燥6小时后在500℃煅烧3小时，得到钼掺杂的二氧化钛纳米粉末16克，粒径20nm。用325nm的紫外光激发可观察到430-512nm发光，其中471纳米的发光峰强度最大。
纳米材料制剂的制备
将β-环糊精聚合物(平均分子量2万)溶解于去离子水中，然后将上述纳米粉末搅拌下加入所得溶液中，25℃搅拌1小时后按顺序分别加入分散剂、表面活性剂、消泡剂、杀菌剂、增稠剂、防冻剂，并搅拌混合均匀。最终配方中各组分的含量如下：
名称 百分比 功能
纳米材料 20％ 促进植物蓝光反应
β-环糊精与环氧氯丙烷的交联聚合物 3％ 防止纳米粒子团聚
TERSPERSE 2700 0.3％ 聚羧酸盐分散剂
Tween-80 1.0％ 表面活性剂
SRECN 0.3％ 有机硅消泡剂
KATHON CG 0.2％ 杀菌防腐剂
聚乙烯醇1788(5％水溶液) 0.5％(折纯) 增稠、成膜
1，2-丙二醇 5％ 防冻剂
去离子水 余量 稀释
按照以上流程和配方，将以上实施例得到的纳米转光粉末配制成制剂。
实验例1：
环糊精聚合物对粒径增长的阻止作用：
重复实施例21，但不加入环糊精聚合物，而用水补齐。将得到的制剂与实施例21的制剂54℃热储14天后测其粒径，并分别将制剂涂到载玻片表面成0.2毫米厚的膜后用325nm的紫外光照射，然后检测透射光波长范围。
对比结果说明不添加环糊精聚合物的制剂纳米粒子团聚严重，同时失去转蓝光功能。
实验例2：
对光合作用的促进作用：
选取开花下针期的花生植株，分别用上述制剂配制成0.05％的水溶液进行喷施，对照样采用去离子水喷施，每棵植株喷施量一致，然后置于温室中。15天后采相同位置的叶片，检测叶绿素总含量(叶绿素a+叶绿素b)及光合强度。叶片叶绿素含量采用95％的乙醇浸提，分光光度计比色测定；光合强度的测定采用干重方法。
实验例3：
抗病毒作用：
挑选健康生长的云烟87烟草的心叶烟，暗室放置一夜。每株烟挑选大小相似的3片叶，摩擦接种烟草花叶病毒。6小时后将叶片剪下，分别放入实施例10-20的制剂稀释至0.05％的溶液中处理，对照样放入自来水中处理。将叶片放入培养皿中在28℃光照培养箱中培养。48小时后，待枯斑症状明显，统计试验结果，计算抑制率，每个处理重复3次。计算公式如下：
抑制率(％)＝(对照枯斑数-处理枯斑数)/对照枯斑数×100
实验例4：
对果实的提质保鲜作用：
选取果园中已挂果、长势相当且相隔较远的红冠苹果树12棵，在采摘前一个月分别喷洒实施例10-20稀释至0.05％的制剂并做标记，对照样用自来水喷洒，每棵树喷洒量和均匀程度一致。一个月后采摘时检测每棵树上果实的平均果径、平均着色度(红色面积占全果面积的百分比)；采摘后将果实自然放置3个月，检查平均烂果率(伤口面积≥2cm2/果为坏果)：

Claims (2)

1.一种能够促进植物蓝光反应的纳米材料制剂，其特征在于：该纳米材料制剂包括纳米材料10％-30％，环糊精聚合物0.1％-10％，非离子表面活性剂0.1％-5％，聚羧酸盐分散剂0.1％-5％，增稠剂0.1％-3％，杀菌剂0.1％-2％，消泡剂0.05-5％，防冻剂0.5％-10％，余量为水；纳米材料制剂的粒径为0.1-25nm；上述百分比为重量百分比；
环糊精聚合物为β-环糊精与环氧氯丙烷的水溶性聚合物，分子量为4000-100000；
所述纳米材料为微量元素掺杂的氧化物；
所述微量元素为硼、锰或钼；
所述氧化物为氧化铁、氧化锌、氧化铜、氧化亚铜、氧化锰、三氧化钼、二氧化钛中的一种或两种以上的混合物。
2.根据权利要求1所述的一种能够促进植物蓝光反应的纳米材料制剂的制备方法，其特征在于：包括如下步骤：
按照配比将平均分子量4000-100000的β-环糊精聚合物溶解于去离子水中，然后将所述纳米材料粉末搅拌下加入所得溶液中，25℃搅拌1小时后按顺序分别加入分散剂、表面活性剂、消泡剂、杀菌剂、增稠剂、防冻剂，并搅拌混合均匀。
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