CN108276434A - 一种红橙光转光膜 - Google Patents
一种红橙光转光膜 Download PDFInfo
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Abstract
本发明公开了一种基于铕配合物转光剂的红橙光转光膜，属于农用转光膜技术领域。该红橙光转光农膜可由转光剂[Eu(2‑BIT)(phen)3]Cl3、分散剂、混合有机溶剂和农膜基础树脂按一定重量百分组成的原料制备。该红橙光转光膜制备方法是先将一定量的[Eu(2‑BIT)(phen)3]Cl3用混合有机溶剂浸润后连同一定量的分散剂加入到农膜基础树脂颗粒中掺混均匀，热熔混炼，最后按一定的吹胀比吹塑成膜而制得。本发明基于铕配合物的红橙光转光膜，配方简单，制备方法简便，操作安全，光能利用率，是一种成本低廉环境友好的转光农膜产品。
Description
技术领域
本发明涉及一种基于铕配合物转光剂的红橙光转光膜，属于农用转光膜技术领域。
背景技术
植物的光合作用是其生命过程的基础，植物进行光合作用主要靠叶片中叶绿素吸收太阳光能来完成。光生态学研究表明，在太阳光谱中叶绿素α及叶绿素β吸收波段集中于蓝紫光(400～480nm)及红橙光(600～700nm)，因此蓝紫光及红橙光与植物的光合作用最为直接相关，而日光中的紫外光对农作物生长却有不利影响。特别地，在600～680nm波段的红橙光区被叶绿素吸收光合作用最强，可促进植物的果实生长。通过增加对植物的红橙光辐照程度，可以显著促进植物根系发达、茎叶生长，达到增产丰收的目的。太阳光中200nm～280nm的短波段紫外线(UVC波段)，在经过地球表面同温层时会被臭氧层吸收。能将日光中280～380nm的紫外光转换成蓝紫光及红橙光的农膜，可以改善光质，有效提高作物的光能利用率有益于作物生长并促进作物的早熟和增产。这类能将日光紫外线转化成蓝紫光或红橙光的转光材料称为转光剂，加有转光剂的农膜即是具有转光功能的农用转光膜。在现代高科技农业生产中，转光农膜越来越引起人们的关注，具有巨大发展空间。
含有稀土元素的无机或者无机-有机复合转光剂是转光剂的主要类型。目前含稀土转光剂的转光农膜多是采用掺杂稀土离子的金属氧化物或者无机盐的无机荧光粉型转光剂。而稀土金属有机化合物类转光剂品种相对较少。基于稀土氧化物或无机盐的无机荧光粉型转光剂，其分散性及与高分子基材相容性较差，转光膜制备工艺复杂，转光剂容易与树脂基质发生离析效应。另外，已有的稀土转光膜不管是采用稀土无机转光剂还是稀土有机配合物型转光剂，往往存在日光紫外光区的吸收谱带较窄，蓝紫或红橙光区的转光发射谱带也为窄隙谱带的不利状况，很难覆盖植物光合作用的光谱带宽，光能利用率不高。因此已有稀土转光膜在环境友好、制备工艺简便、光能的高效利用以及价格低廉等方面还存在不足。
发明内容
为了克服现有技术产品的缺点及不足，本发明的首要目的在于提供一种基于铕配合物转光剂的红橙光转光膜。
本发明的另一目的在于提供上述红橙光转光膜的制备方法。
本发明提供的铕配合物转光剂结构设计合理、合成方法简单，成本低廉。由本方法制备的红光转光膜，工艺过程简单，无污染，性能优异，易于工业化生产。
为实现上述发明目的，本发明的技术方案如下：
本发明提供的铕配合物转光剂分子式为[Eu(2-BIT)(phen)3]Cl3(分子结构如式I)，其中第一配体2-BIT为2-巯基苯并咪唑，第二配体phen为1，10-邻菲罗啉。
本发明提供以[Eu(2-BIT)(phen)3]Cl3为转光剂的红橙光转光膜的制备方法为：称取一定量的[Eu(2-BIT)(phen)3]Cl3，先用混合有机溶剂浸润，然后连同一定量的分散剂一起加入到基础农膜塑料颗粒中进行掺混均匀，热熔混炼，最后按2.0～3.0的吹胀比吹塑成薄膜即得到红橙光转光膜。
如上所述的红橙光转光膜制备方法，其特征在于：[Eu(2-BIT)(phen)3]Cl3在转光膜制备原料中的w％含量为0.5～2.5％。
如上所述的红橙光转光膜制备方法，其特征在于：所使用的混合有机溶剂由醇(乙醇或异丙醇或乙二醇)与白油和松节油中的一种按一定比例组成，优选的混合有机溶剂由乙醇与白油组成。
如上所述的红橙光转光膜制备方法，其特征在于：所使用的分散剂为PEG600和PEG800中的一种或二者的混合物。
如上所述的红橙光转光膜制备方法，其特征在于：分散剂在转光膜制备原料中w％含量为1.0～3.0％。
如上所述的红橙光转光膜制备方法，其特征在于：基础农膜塑料为低密度聚乙烯(LDPE)塑料、聚氯乙烯(PVC)及乙烯-聚醋酸乙烯共聚物(EVA)中的一种或者几种的混合物。
如上所述的红橙光转光膜制备方法，其特征在于：所使用的混合有机溶剂中白油或者松节油在转光膜制备原料中的w％含量为1.0～2.5％，乙醇或异丙醇或乙二醇在转光膜制备原料中的w％含量为1.0～3.5％。
本发明转光材料[Eu(2-BIT)(phen)3]Cl3的合成路线如下：
分别以2-巯基苯并咪唑和邻菲罗啉为第一和第二配体与三氯化铕按1∶3∶1摩尔比，在无水乙醇中加热回流反应制得转光剂[Eu(2-BIT)(phen)3]Cl3。
所述的红橙光转光膜可用于农业棚膜或地膜，使用于作物种植或者育苗等。
与现有技术相比，本发明的有益效果在于：
本发明铕有机配合物转光剂[Eu(2-BIT)(phen)3]Cl3为一种金属有机化合物，在农膜基础树脂材料中的分散性和相容性好，避免了传统稀土无机荧光粉型转光剂在树脂基材中分散性不好而造成的离析效应。
本发明是基于铕有机配合物转光剂的红橙光转光膜，其紫外吸收谱带更加宽广吸收强度更大，同时其红橙光转光发射谱带也更宽广强度更大，因此光能利用效率更高。
本发明红橙光转光膜所用的有机溶剂及分散剂等复配组分用量少且环境友好，红橙光转光谱带宽而强与作物光合作用中叶绿素在红橙光波段的吸收谱带匹配性更好，转光膜的制备工艺方法简便易于操作，生产成本低廉，非常有利于工业生产和农业生产的推广使用。
附图说明
图1是转光剂[Eu(2-BIT)(phen)3]Cl3与第一配体2-BIT的FT-IR光谱图。
图2是转光剂[Eu(2-BIT)(phen)3]Cl3的1H NMR谱图。
图3是转光剂[Eu(2-BIT)(phen)3]Cl3与配体的UV-Vis光谱图(1×10-5mol/L DMF溶液)。
图4是实施例1制得的转光膜在λ＝365nm光激发下的红橙光转光效果图。
具体实施方式
下面以实施例来进一步说明本发明，但本发明并不局限于这些实施例。
所用的主要原料、测试仪器及方法：线型低密度聚乙烯(LDPE-7042)，扬子石油化工股份有限公司；透明聚氯乙烯(PVC)，东莞市宏嘉塑胶原料有限公司；吹膜机，SJMZ-45×30，青岛顺德塑料机械有限公司；元素组成由德国Elementar公司的vario EL III型元素分析仪测定；FT-IR由Spectrum BX II型傅立叶变换红外光谱仪测定；UV-Vi s光谱经TU-1901型紫外分光光度计(北京普析通用仪器制造有限公司)测得；荧光光谱经LS55型荧光分光光度计(美国PerkinElmer公司)测得；1H NMR核磁波谱经AVANCE型核磁共振波谱仪(dmso-d6为溶剂，TMS为内标，瑞士Bruker公司)测得。配合物中Sm的含量通过EDTA络合滴定法测定。
实施例1
转光剂[Eu(2-BIT)(phen)3]Cl3的合成方法如下：所有原料先经烘干去除水分，称取0.751g(5mmol)2-巯基苯并咪唑，用10mL无水乙醇溶解，加入到100mL的三口瓶中，在磁力搅拌下，然后加入溶有1.291g(5mmol)EuCl3的15mL乙醇溶液，回流2h；称取2.703g(15mmol)邻菲罗啉，用15mL的无水乙醇溶解，逐滴加入到上述三口烧瓶中，滴加完毕，继续回流5h，冷却静置，有沉淀析出，抽滤，粗产品用无水乙醇重结晶，真空干燥得到粉末状产物3.26g。元素分析结果(理论/实测，w％)：C 54.36/54.31，N 11.80/11.76，H 3.16/3.21，S 3.37/3.39；铕的含量(理论/实测，w％)：16.01/15.97。FT-IR(KBr)，v/cm-1：从[Eu(2-BIT)(phen)3]Cl3与2-巯基苯并咪唑的红外对比图(图1)可以看出，位于3180cm-1附近的该配体的芳环C-H及N-H耦合伸缩振动吸收峰位移到了3400cm-1附近，这说明该配体中的N参与了配位；位于2500～2600cm-1处的S-H伸缩振动特征吸收峰在配合物中消失了，说明S原子参与了形成配位键；两种配体都应该有的位于1640cm-1附近的C＝N双键以及1580～1450cm-1附近的芳环骨架伸缩振动特征吸收峰在配合物中也都发生了明显变化。这些都表明两种配体与铕离子发生了配位作用。根据红外测试结果，并结合Eu3+的配位特性以及元素分析结果可以说明配体2-巯基苯并咪唑和邻菲罗啉都以二齿成键的形式分别与Eu3+发生配位，形成了稳定的三元配合物[Eu(2-BIT)(phen)3]Cl3。转光剂[Eu(2-BIT)(phen)3]Cl3的1H NMR(DMSO，400MHz，δ)，如图2：12.496(s，N-H)，9.110，9.102(d，phen-H)，8.512，8.488(q，phen-H)，8.002(s，Ar-H)，7.794-7.763(q，Ar-H)，7.157-7.100(s，phen-H，Ar-H)，与配体2-巯基苯并咪唑的核磁谱图相比，H原子的化学位移有明显变化，在转光剂配合物中-SH上的H原子峰消失，证明-SH参与了配位，这也佐证了所合成转光剂的分子结构式。图3是[Eu(2-BIT)(phen)3]Cl3与配体2-巯基苯并咪唑及邻菲罗啉的UV-Vi s光谱图，可见由于两种配体都具有大π共轭体系，中心铕离子又具有空轨道，形成的配合物容易发生分子内的电子迁移，从而使得所合成的稀土配合物转光剂与配体相比具有更宽更强的紫外吸收，吸收谱带基本覆盖了280～380nm的紫外波段。
实施例2
使用实施例1所合成的转光剂在制备红橙光转光膜方面的应用，该红橙光转光膜由如下重量百分比的原料制得：[Eu(2-BIT)(phen)3]Cl3 1.5％，无水乙醇2.0％，白油2.0％，分散剂PEG 800 2.5％，余量为低密度聚乙烯(LDPE)。
该红橙光转光膜的制备方法如下：按上述比例称取15g[Eu(2-BIT)(phen)3]Cl3先用20g无水乙醇和20g白油组成的混合溶剂浸润，然后连同25g PEG 800-同加入920g LDPE颗粒掺混均匀，加热熔融混炼，按2.5的吹胀比吹塑成薄膜即得红橙光转光膜。
所制得的转光膜对280～380nm紫外光具有良好的吸收性能。在365nm波长紫外光激发下转光膜的转光效果见图4，可见该转光膜可以发射出λem，max≈600nm的红橙光，且谱带为覆盖590～680nm范围的较强红橙光，转光效果非常良好。
实施例3
使用实施例1所合成的转光剂在制备红橙光转光膜方面的应用，该转光膜由如下重量百分比的原料复配制得：[Eu(2-BIT)(phen)3]Cl31.5％，异丙醇1.5％，松节油2.0％，分散剂PEG 6002.0％，余量为聚氯乙烯(PVC)。
该红橙光转光膜的制备方法如下：按上述比例称取15g[Eu(2-BIT)(phen)3]Cl3先用15g异丙醇和20g松节油组成的混合溶剂浸润，然后连同20g PEG 600一同加入930g PVC颗粒掺混均匀，加热熔融混炼，按2.0的吹胀比吹塑成薄膜即得红光转光膜。
所制得的转光膜对280～380nm紫外光同样具有良好吸收性能，在365nm波长紫外光激发下转光膜的转光效果同样优异，可以发射出谱带覆盖590～680nm宽而强λem，max≈600nm的红橙光。
Claims (6)
1.一种铕配合物红橙光转光剂[Eu(2-BIT)(phen)3]Cl3，其特征在于，其分子结构式为
2.一种基于铕配合物转光剂的红橙光转光膜，其特征在于，所述的红橙光转光膜制备原料由转光剂[Eu(2-HBI)(phen)3]Cl30.5～2.5％、混合有机溶剂2.0～6.0％、分散剂1.0～3.0％及余量的基础农膜树脂组成，其中比例皆为重量百分比。
3.如权利要求2所述的一种基于铕配合物转光剂的红橙光转光膜，其特征在于，所使用的混合有机溶剂由醇(乙醇或异丙醇或乙二醇)与白油和松节油中的一种按一定用量组成，优选的混合有机溶剂由乙醇与白油组成。
4.如权利要求2所述的一种基于铕配合物转光剂的红橙光转光膜，其特征在于，所使用的混合有机溶剂中白油或者松节油在转光膜制备原料中w％含量为1.0～2.5％，乙醇或异丙醇或乙二醇在转光膜制备原料中w％含量为1.0～3.5％。
5.如权利要求2所述的一种基于铕配合物转光剂的红橙光转光膜，其特征在于，所述的分散剂为PEG600及PEG800中的一种或二者的混合物。
6.如权利要求2所述的一种基于铕配合物转光剂的红橙光转光膜的制备方法为：按转光膜原料重量百分组成，称取一定量的[Eu(2-HBI)(phen)3]Cl3，先用混合有机溶剂浸润，然后与分散剂一起加入到基础农膜树脂颗粒中掺混均匀，热熔混炼，最后按2.0～3.0的吹胀比吹塑成膜即制得所述的红橙光转光膜。
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