CN110128739B - 一种表面负载改性二氧化钛光催化剂的eva发泡材料及其制备方法 - Google Patents
一种表面负载改性二氧化钛光催化剂的eva发泡材料及其制备方法 Download PDFInfo
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- CN110128739B CN110128739B CN201910424908.8A CN201910424908A CN110128739B CN 110128739 B CN110128739 B CN 110128739B CN 201910424908 A CN201910424908 A CN 201910424908A CN 110128739 B CN110128739 B CN 110128739B
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Abstract
本发明公开了一种表面负载改性二氧化钛光催化剂的EVA发泡材料及其制备方法,属于高分子复合发泡材料领域。本发明使用水热法一步制备RGO/TiO2复合催化剂,并通过多巴胺具有自聚合成膜的特性及聚多巴胺的还原性,使其通过与RGO/TiO2间的氢键作用,将RGO/TiO2复合光催化剂自组装在EVA表面,制得表面负载RGO/TiO2的EVA发泡材料,其提高了发泡材料对有机大分子的降解能力,同时其制备方法操作简单,避免了后期涂膜与发泡材料的不相容,在实际应用中具有巨大的社会经济效益。
Description
技术领域
本发明属于高分子复合发泡材料领域,具体涉及一种表面负载改性二氧化钛光催化剂的EVA发泡材料及其制备方法。
背景技术
社会在高速发展,但资源与环境现状不断恶化。以室内环境为例,目前种类繁多的室内装修材料都含有超过健康标准的二甲苯、甲苯、甲醛CH2O和丙酮等VOC物质,对人体有长期的健康危害。作为应用最为广泛的有机泡沫材料之一,EVA泡沫产品自然被人们提出了更多的产品性能的要求,因此研究出一种具有光催化自清洁功能、使用范围广泛且健康无毒的EVA泡沫材料就显得十分重要。
二氧化钛因为具有氧化能力强、化学性质稳定无毒、催化效率高的特点,被认为是一种优良的半导体光催化材料。TiO2光催化反应过程中的界面氧化还原反应通常负责有机污染物的光降解。TiO2表面羟基在静电引力作用下将氧气吸附至表面而形成的导带电子-空穴对,会在电场作用下将其氧化为超氧阴离子自由基,H+与水或羟基离子会与电子-空穴对反应形成羟基自由基,这些自由基具有超强活化作用,遇到有机污染物时能使其发生链式降解,而被分解成水、CO2。但TiO2是一种宽带隙半导体,其只吸收在日光中占很少一部分的紫外光,这限制了其在室内的使用,同时其光生电子空穴对的复合率很高。为提高TiO2光催化效率,需对TiO2进行修饰改性,以缩短其带隙宽度,或者阻止电子空穴对的复合率,比如采用金属离子掺杂(Fe、Cu)、非金属掺杂(N、F)、表面染料敏化等方法来降低带隙宽带。近年来,学者发现将半导体光催化剂TiO2与不同形态、结构的炭材料(如CNT、CB、EG、GO等)复合是一种有效提高TiO2光催化活性的途径之一。
常用的涂层剂或者涂膜,例如聚氟乙烯PVF涂层剂、聚氨酯PU膜,与EVA相容性很差,无论是通过涂膜机还是流延机尾段高温高压下复合,干燥后均容易脱落,导致无法实现有效的EVA发泡材料的表面改性。多巴胺DPA可聚合形成聚多巴胺,聚多巴胺是一种新型的仿生聚合物,其与海洋贻贝的胶粘分泌物具有相似的特性。在水体中,均能粘附在不经任何预处理的基体表面,易于沉积在无机和有机基体上,包括超疏水表面,且具有持久性。因此多巴胺为不同基体的表面改性提供了一种新方法。
发明内容
本发明的目的在于提供一种表面负载改性二氧化钛光催化剂的EVA发泡材料及其制备方法。本发明配方科学合理,工艺流程简单实用,在实际应用中具有巨大的社会经济效益。
为实现上述目的,本发明采用如下技术方案:
一种表面负载改性二氧化钛光催化剂的EVA发泡材料,其制备方法包括以下步骤:
1)将EVA、发泡剂AC、交联剂DCP、氧化锌、硬脂酸和硬脂酸锌混合均匀后置于转矩流变仪中,于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min,得到EVA发泡材料;将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
2)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5,得到多巴胺DPA溶液;将步骤1)所得EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃真空干燥箱中烘干5h,得到DPA负载的EVA泡沫片材;
3)称取一定质量的RGO/TiO2置于去离子水和乙醇混合溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液;将步骤2)得到的EVA泡沫片材浸没到该分散液中,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载RGO/TiO2的EVA发泡材料。
步骤1)中所用各原料的重量份为:EVA 80-100份、发泡剂AC 3.2份、交联剂DCP1.2份,氧化锌1.2份、硬脂酸0.8份、硬脂酸锌1份。
步骤3)中所述RGO/TiO2是以钛酸四丁酯为钛源,对苯二胺PPD为还原剂,通过一步水热法制得。其具体制备方法为:
a)将100mg氧化石墨烯GO室温下加入到40mL去离子水中搅拌2h,加入溶解有600mg对苯二胺PPD的20mL乙醇溶液,继续搅拌30min;
b)将100mg钛酸四丁酯和5mg氯化铵室温下加入到10mL去离子水中;
c)将步骤a)、b)所得溶液混合,在反应釜中经140℃水热反应8h,将获得的产物过滤并洗涤干净,然后置于真空烘箱中干燥,即得所述RGO/TiO2。
步骤3)所述混合溶液中乙醇与水的体积比为1:2。
步骤3)所得复合物分散液的浓度为2g~10g/L。
本发明利用还原氧化石墨烯对二氧化钛进行改性,并通过聚多巴胺将其组装在EVA发泡材料表面,得到一种可光降解有机物的功能发泡材料。
本发明的有益效果在于:
1、本发明采用一步水热法制备RGO-TiO2光催化剂。在水热条件下,对苯二胺的还原性大大提高,同时不同于RGO和TiO2的简单混合,在还原过程中保留下来的GO与TiO2表面的羟基可相互作用形成Ti-O-C键,以增强RGO和TiO2之间的电子传输作用。
2、本发明中RGO的使用提高了光吸收强度和光吸收范围,从而增强了TiO2的光催化降解效果,且其优异的导电性增大了光生电子的转移速率,从而抑制了光激发TiO2产生的电子-空穴对的复合。
3、本发明利用多巴胺具有的自聚合成膜的特性,可以不经任何预处理粘附在EVA基体表面,且具有持久性。
4、本发明利用聚多巴胺薄膜的还原性,及其与RGO-TiO2间的氢键作用,将光催化剂自组装在EVA表面,避免了大分子涂料或薄膜与EVA不相容、干燥后容易脱落的情况,且操作简单。
附图说明
图1为GO和RGO-TiO2的红外光谱图。
图2为石墨、GO、RGO和RGO-TiO2的X射线衍射谱图。
图3为EVA泡沫(a)和负载RGO-TiO2的泡沫(b)的SEM图片。
图4为RGO-TiO2和不同负载的EVA发泡材料在可见光照下光催化降解RhB的降解曲线。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是本发明不仅限于此。
实施例1
一种制备表面负载改性二氧化钛光催化剂的EVA发泡材料的方法,具体步骤为:
1)将100mg氧化石墨烯GO室温下加入到40mL去离子水中搅拌2h,加入溶解有600mg对苯二胺PPD的20mL乙醇溶液,继续搅拌30min;
2)将100mg钛酸四丁酯和5mg氯化铵室温下加入到10mL去离子水中;
3)将步骤1)、2)所得溶液混合,在140℃的反应釜中水热反应8h,将获得的产物过滤并洗涤干净,然后置于真空烘箱中干燥,得到RGO/TiO2;
4)将EVA 100重量份、发泡剂AC 3.2重量份、交联剂DCP 1.2重量份、氧化锌1.2重量份、硬脂酸0.8重量份和硬脂酸锌1重量份混合均匀后置于转矩流变仪中,于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min得到EVA发泡材料,将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
5)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5左右,得到多巴胺DPA溶液;将制得的EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃下真空干燥箱烘干5h,得到DPA负载的EVA泡沫片材;
6)称取0.2g的RGO/TiO2置于100mL去离子水和乙醇(2:1,v/v)溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液,将步骤5)得到的EVA泡沫片材浸没到该分散液下,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载RGO/TiO2的EVA发泡材料。
实施例2
一种制备表面负载改性二氧化钛光催化剂的EVA发泡材料的方法,具体步骤为:
1)将100mg氧化石墨烯GO室温下加入到40mL去离子水中搅拌2h,加入溶解有600mg对苯二胺PPD的20mL乙醇溶液,继续搅拌30min;
2)将100mg钛酸四丁酯和5mg氯化铵室温下加入到10mL去离子水中;
3)将步骤1)、2)所得溶液混合,在140℃的反应釜中水热反应8h,将获得的产物过滤并洗涤干净,然后置于真空烘箱中干燥,得到RGO/TiO2;
4)将EVA 100重量份、发泡剂AC 3.2重量份、交联剂DCP 1.2重量份、氧化锌1.2重量份、硬脂酸0.8重量份和硬脂酸锌1重量份混合均匀后置于转矩流变仪中,于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min得到EVA发泡材料,将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
5)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5左右,得到多巴胺DPA溶液;将制得的EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃下真空干燥箱烘干5h,得到DPA负载的EVA泡沫片材;
6)称取0.4g的RGO/TiO2置于100mL去离子水和乙醇(2:1,v/v)溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液,将步骤5)得到的EVA泡沫片材浸没到该分散液下,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载RGO/TiO2的EVA发泡材料。
实施例3
一种制备表面负载改性二氧化钛光催化剂的EVA发泡材料的方法,具体步骤为:
1)将100mg氧化石墨烯GO室温下加入到40mL去离子水中搅拌2h,加入溶解有600mg对苯二胺PPD的20mL乙醇溶液,继续搅拌30min;
2)将100mg钛酸四丁酯和5mg氯化铵室温下加入到10mL去离子水中;
3)将步骤1)、2)所得溶液混合,在140℃的反应釜中水热反应8h,将获得的产物过滤并洗涤干净,然后置于真空烘箱中干燥,得到RGO/TiO2;
4)将EVA 100重量份、发泡剂AC 3.2重量份、交联剂DCP 1.2重量份、氧化锌1.2重量份、硬脂酸0.8重量份和硬脂酸锌1重量份混合均匀后置于转矩流变仪中,于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min得到EVA发泡材料,将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
5)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5左右,得到多巴胺DPA溶液;将制得的EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃下真空干燥箱烘干5h,得到DPA负载的EVA泡沫片材;
6)称取0.6g的RGO/TiO2置于100mL去离子水和乙醇(2:1,v/v)溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液,将步骤5)得到的EVA泡沫片材浸没到该分散液下,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载RGO/TiO2的EVA发泡材料。
实施例4
一种制备表面负载改性二氧化钛光催化剂的EVA发泡材料的方法,具体步骤为:
1)将100mg氧化石墨烯GO室温下加入到40mL去离子水中搅拌2h,加入溶解有600mg对苯二胺PPD的20mL乙醇溶液,继续搅拌30min;
2)将100mg钛酸四丁酯和5mg氯化铵室温下加入到10mL去离子水中;
3)将步骤1)、2)所得溶液混合,在140℃的反应釜中水热反应8h,将获得的产物过滤并洗涤干净,然后置于真空烘箱中干燥,得到RGO/TiO2;
4)将EVA 100重量份、发泡剂AC 3.2重量份、交联剂DCP 1.2重量份、氧化锌1.2重量份、硬脂酸0.8重量份和硬脂酸锌1重量份混合均匀后置于转矩流变仪中,于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min得到EVA发泡材料,将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
5)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5左右,得到多巴胺DPA溶液;将制得的EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃下真空干燥箱烘干5h,得到DPA负载的EVA泡沫片材;
6)称取0.8g的RGO/TiO2置于100mL去离子水和乙醇(2:1,v/v)溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液,将步骤5)得到的EVA泡沫片材浸没到该分散液下,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载RGO/TiO2的EVA发泡材料。
对比例1
一种制备表面负载二氧化钛光催化剂的EVA发泡材料的方法,具体步骤为:
1)将EVA 100重量份、发泡剂AC 3.2重量份、交联剂DCP 1.2重量份、氧化锌1.2重量份、硬脂酸0.8重量份和硬脂酸锌1重量份混合均匀后置于转矩流变仪中,于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min得到EVA发泡材料,将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
2)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5左右,得到多巴胺DPA溶液;将制得的EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃下真空干燥箱烘干5h,得到DPA负载的EVA泡沫片材;
3)称取0.2g的TiO2置于100mL去离子水和乙醇(2:1,v/v)溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液,将步骤2)得到的EVA泡沫片材浸没到该分散液下,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载TiO2的EVA发泡材料。
图1为GO和RGO-TiO2的红外光谱图。由图1可以看出,RGO-TiO2 1716cm-1(C=O键)和1052cm-1~1384cm-1区间(C-O键与O-H键)的吸收峰减弱,说明经过PPD的还原处理后,GO成功被还原成石墨烯,而1630cm-1(C=C键)的吸收峰还在,说明材料保留了GO的碳骨架。同时很容易可以看到,RGO-TiO2谱线在低于1000cm-1出现新的低频峰带(Ti-O-C的骨架振动),其存在这证实了复合材料中RGO和TiO2间存在紧密的化学联系。
图2为石墨、GO、RGO和RGO-TiO2的X射线衍射谱图。由图2中RGO的曲线可以看出,其在2θ=24.5°处出现了一个宽化的强峰,证实了RGO的形成,其层间距略高于良好有序的石墨,表明在RGO中存在一些残留的含氧官能团,破坏了原来石墨晶体结构的规整度。由RGO-TiO2的曲线可以看出,在2θ为25.6°、37.7°、48.4°、54.4°、62.6°、68.5°、75.4°处出现的主要衍射峰分别指向了锐钛矿的101、004、200、105、204、116、215晶面,而RGO在24.5°处的衍射峰被TiO2在25.6°处的衍射峰所屏蔽,因此在复合物中没有能够发现RGO峰。
图3为EVA泡沫(a)和负载RGO-TiO2的泡沫(b)的SEM图片。由图3可见,未负载催化剂的EVA泡沫材料表面比较平整,负载后材料表面存在一些未团聚的RGO-TiO2催化剂,这是由于聚多巴胺和RGO-TiO2之间的氢键作用,使复合催化剂能够组装在泡沫材料的表面。
性能测试
以RhB为目标反应物,称取一定量的光催化剂或EVA泡沫片材,置于80mL、1.8×10- 5mol/L的RhB溶液中,盖上玻璃防止挥发。黑暗中搅拌30~60min,在可见光照射下每隔20min取3mL RhB溶液测定吸光度的变化。C0取溶液在黑暗中30-60min而达到吸附平衡时的浓度,C为可见光照射下的剩余溶液浓度。
表1 不同发泡材料在不同时间段对RhB染料的降解率
由表1可见,RGO/TiO2用量为8g/L制得的实施例4发泡材料对RhB的降解效果最佳。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (4)
1.一种表面负载改性二氧化钛光催化剂的EVA发泡材料的制备方法,其特征在于:包括以下步骤:
1)将EVA、发泡剂AC、交联剂DCP、氧化锌、硬脂酸和硬脂酸锌混合均匀后于110℃、转速15rpm条件下挤出混炼10min,所得混合物迅速转移到开炼机中,95℃下混炼10-20min,后将物料压制成薄片,置于预热好的平板硫化机模腔内,在10MPa、170℃下模压发泡6min,得到EVA发泡材料;将其剪切成一定的形状,浸没于去离子水中超声20min,干燥4h备用;
2)称取0.3g三羟甲基氨基甲烷,溶于250mL去离子水中作为缓冲溶液;在所得缓冲溶液中加入0.5g多巴胺盐酸盐,调节pH=8.5,得到多巴胺DPA溶液;将步骤1)所得EVA发泡材料浸没于多巴胺DPA溶液中,室温下磁力搅拌24h,反应结束后将EVA发泡材料取出,用去离子水多次冲洗干净,70℃真空干燥箱中烘干5h,得到DPA负载的EVA泡沫片材;
3)称取一定质量的RGO/TiO2置于去离子水和乙醇混合溶液中,室温下磁力搅拌1h,得到均匀的复合物分散液;将步骤2)得到的EVA泡沫片材浸没到该分散液中,30℃下超声震荡3h后将泡沫片材取出,用去离子水水洗多次后置于真空干燥箱内,70℃烘干5h,得到表面负载RGO/TiO2的EVA发泡材料;
步骤1)中所用各原料的重量份为:EVA 80-100份、发泡剂AC 3.2份、交联剂DCP 1.2份,氧化锌1.2份、硬脂酸0.8份、硬脂酸锌1份;
步骤3)中所述RGO/TiO2是以钛酸四丁酯为钛源,对苯二胺PPD为还原剂,通过一步水热法制得,其具体制备方法为:
a)将100mg氧化石墨烯GO室温下加入到40mL去离子水中搅拌2h,加入溶解有600mg对苯二胺PPD的20mL乙醇溶液,继续搅拌30min;
b)将100mg钛酸四丁酯和5mg氯化铵室温下加入到10mL去离子水中;
c)将步骤a)、b)所得溶液混合,在反应釜中经140℃水热反应8h,将获得的产物过滤并洗涤干净,然后置于真空烘箱中干燥,即得所述RGO/TiO2。
2.根据权利要求1所述的表面负载改性二氧化钛光催化剂的EVA发泡材料的制备方法,其特征在于:步骤3)所述混合溶液中乙醇与水的体积比为1:2。
3.根据权利要求1所述的表面负载改性二氧化钛光催化剂的EVA发泡材料的制备方法,其特征在于:步骤3)所得复合物分散液的浓度为2g~10g/L。
4.一种如权利要求1所述方法制得的表面负载改性二氧化钛光催化剂的EVA发泡材料。
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