CN113181896B - 一种柔性生物质基压电材料的制备方法及应用 - Google Patents
一种柔性生物质基压电材料的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种柔性生物质基压电材料的制备方法及应用，该方法包括：使用生物质基柔性材料(棉花，果皮，秸秆等)，利用水热法共沉淀法制备压电材料并使其负载在生物质基体上，通过调节反应参数来实现对生物质基体上上氧化锌纳米材料的形貌调控。本发明提出的这种制备生物质纳米材料的方法，可以使纳米材料与生物质之间形成强烈的结合，多次循环之后仍能保持较高的催化活性，对有机污染物(RhB，四环素)显示出了出色的降解能力，并且易于回收利用，合成方法简单。
Description
【技术领域】
本发明属于催化材料技术领域，涉及一种柔性生物质基压电材料的制备方法及应用。生物质经过活化处理后会得到具有超高比表面积和空洞纤维状材料，与压电材料相复合，兼具有生物材料的稳定性和高压电相应能力，尤其设计是在界面催化反应及水质净化领域的应用，属于新型功能材料的制备。
【背景技术】
使用可再生资源满足人们日益增长的物质与生活需要，是目前人类所面临的一个新的现实问题。在地球这个充满有机生命体的星球上，存在最广泛的，数量最多的无疑是生物体及其衍生物，称其为生物质或生物质衍生物。如果能以生物质为原材料将其转变为功能材料，不仅可以解决环境污染问题，也可以获得高活性的生物质碳基材料。
目前压电催化材料机械能收集效率低，回收性差，极大地限制了其进一步的应用。此外，当前压电材料催化活性的激发多以超声或搅拌，通过外界输入电能然后转变为机械能，在材料表面产生低频震动，使得具有压电特性的材料产生形变产生电荷迁移，继而释放出催化活性。
基于此，我们研发了柔性生物质基压电材料，通过在生物质基础上负载具有高压电相应能力的材料并将其制作为纳米薄片，使其既具有压电材料的出色的压电响应能力，又有生物质材料较高的比表面积和多空的结构。
目前，压电催化方法在解决环境问题上具有广阔的应用前景。近年来，压电催化降解有机染料的研究取得了显著进展，相较于光催化压电催化可以在暗环境下进行操作，对环境条件要求更为宽松，应用前景更为广泛。
专利CN111871405A公开了一种利用光协同压电催化高效降解染料废水的方法，在BaTiO3，粉体表面包覆BiVO4纳米颗粒，BaTiO3粉体在振动环境下由于压电效应表面会产生力生电荷，BiVO4纳米颗粒在可见光下可以诱导出光生电荷；BaTiO3/BiVO4压电/半导体复合材料在协同可见光和超声振动作用下，会产生增强的催化活性可加快染料废水的降解，在60min内降解效率高达98％。但是必须需要可见光于其协同才能发挥作用，在暗环境下难以进行。
专利CN108411406B公开了一种通过静电纺丝技术，将压电陶瓷前驱体与可纺聚合物复合，通过高温煅烧减少复合材料之间的阻抗，从而提高材料的压电性能。可以得到高密度的裸露在纤维表面的压电材料与光催化剂结合的界面，充分利用压电材料与光催化剂界面的内电场作用，有效驱动光生电子和空穴的分离，从而高效提高光催化反应效率。然而，在机械力作用下压电催化材料的活性位点会逐渐被破坏，催化活性会逐渐降低，研究表明将压电催化材料固定在PVDF可以提高材料的稳定性，但10个循环后，催化活性只维持了80％。
【发明内容】
[要解决的技术问题]
本发明目的是解决发明目的是解决压电催化领域分析出现在压电材料收到循环次数的制约，这样柔性材料可以克服这一缺点，从而提高材料的稳定性和催化性能。同时还能利用生物质的多表面官能团增加活性位点，提高材料的压电催化活性。
[技术方案]
本发明所述的一种生物质基压电材料的制备及应用方法，其技术方案及步骤如下：
(1)以脱脂棉，果皮，秸秆为原料，先进性预处理，通过使用乙醇去离子水进行清洗除去表面的污渍和杂质，然后在干燥箱中进行干燥，温度60～80℃，6～12h，除去表面所吸附的水分。
(2)通过使用水热法按照摩尔比1:(2～16)制备氧化锌前驱体，按钼和硫原子比为1:(4～20)制备二硫化钼前驱体；共沉淀法，按铋和铁原子比按1:(1～4)制备铁酸铋前驱体。
(3)将前驱体进行洗涤干燥，进一步纯净产物。其中棉花做载体的需要进行水热反应温度100～180℃，时间6～18h；其余载体的只需通过使用球磨催化剂颗粒进行负载，在转速为500～1500rpm/min条件下，球磨3～5h。
(4)将(3)中所收集到的材料放置到干燥箱中在60～80℃下进一步干燥。
(5)将前驱体置于管式加热炉中，在N2气氛下于300～500℃下活化2h，并自然冷却至室温收集所得产物。
(6)收集冷却后的产品，得到生物质基压电催化剂产品。
(7)称取质量为0.05～0.3g的生物质基压电催化剂固体，至于压电催化体系中，测试其压电催化性能，具体操作为：称取质量为0.05～0.3g的生物质基压电催化剂固体，加入到体积为20～50mL的污染物水样，引入超声激发压电催化反应5～60min，离心取上层清液测定目标污染物的浓度。
所述的压电材料前驱体可以为棉花、柳絮、果皮、秸秆纤维等其中的任意一种。
所属的压电催化反应体系应用的机械力引发方法可以为超声法、搅拌法、水流法等的一种或多种符合提供机械力的方法。
生物质是一直以来所备受关注的碳材料，具有较大的比表面积，孔道和稳定性等优点，是优异的催化剂载体。与现有技术相比，本发明的优点和有益效果：
(1)本发明技术中的生物质具有较高的比表面积、化学惰性、高机械强度大大提高了催化剂的稳定性。
(2)本发明合成生物质基压电催化催化剂操作流程简单，成本低廉，易于批量化生产。
(3)本发明制备的压电催化材料同时具有高寿命和高催化活性，能满足环境工程的应用需求。
(4)本发明制备的压电材料可重复性好，多次循环之后仍能保持较高的压电相应能力。
【附图说明】
图1为实施方案后制备的生物质基氧化锌材料表面SEM图(10μm)。
图2为实施方案后制备的生物质基氧化锌材料表面SEM图(1μm)。
图3为负载氧化锌的生物质XRD图。
【具体实施方式】
实施例1：
(1)准确称量0.5g棉花放置到乙酸锌溶液(10ml)中浸泡，然后按乙酸锌，氢氧化钠的摩尔比为1:4准确移取乙酸锌溶液和氢氧化钠溶液至锥形瓶，加入磁子在转速为600rpm/min条件下，搅拌30min，得到前驱体。
(2)将步骤(1)得到的前驱体放置到聚四氟乙烯内胆的反应釜中，转移至真空干燥箱中在100～180℃下进行水热反应，反应时间14h，反应完成后取出后自然冷却至室温。
(3)将步骤(2)得到的材料放置到聚四氟乙烯内胆的反应釜中，转移至真空干燥箱中在100～180℃下进行水热反应，反应时间6～18h后取出后自然冷却至室温。
(4)将前驱体放置到培养皿中在80℃下干燥12h，使其充分干燥。
(5)将干燥完成后置于管式加热炉中，在N2气氛下于300～500℃下活化2h，并自然冷却至室温。
(6)收集冷却后的产物品，得到生物质基压电催化剂材料，其投射电镜表征结果见说明书附图。
(7)量取4份25ml含有25mg/L的罗丹明B水样，编号分别为1、2、3和4，分别在四组样品中加入0.1g的生物质基材料，其中1号体系在50kHz下超声5min，2号体系在50kHz下超声10min，3号体系在50kHz下超声20min，4号体系在50kHz下超声60min，离心取上层清液测定罗丹明B的浓度。
(8)附图1的投射电镜可以证明成功的制备处理生物质基氧化锌复合材料，具有纤维状结构，氧化锌颗粒在上面附着均匀，有着纳米花状的结构。
实施例2：
(1)将收集的猕猴桃皮用去离子水和乙醇多次清洗，洗去上面的污渍和杂质，然后将其放置在80℃的干燥箱中进行6h干燥，除去水分，冷却至室温后取出留作备用。
(2)使用粉碎机将其粉碎，过200目筛后即得到预处理的原料。
(3)使用二水钼酸钠和硫脲分别最为钼源和硫源，按照二水钼酸钠和硫脲原子比为Mo:S＝1:4制备溶液，溶解在70mL的水中，在剧烈搅拌下形成均相溶液。
(4)在转速500rpm/min下搅拌30min，后将溶液转移至100ml聚四氟乙烯内胆高压反应釜中，在180℃下反应48h，自然冷却至室温。
(5)将(4)所制备的固体产物进行离心收集，用去离子水和无水乙醇清洗3次以上，在水中进行超声后经冷冻干燥。
(6)称取质量为0.5g的生物质粉末，按照生物质与二硫化钼的质量比为1:2混合均匀。
(7)将(6)得到的混合粉末加入到聚四氟球磨釜中，按照物料与氧化锆球的质量比为1:100～500的质量比加入氧化锆球，在转速为500～1500rpm/min条件下，球磨3～5h，得到生物质基压电催化材料前驱体粉末。
(8)将前驱体粉末至于管式炉中，在N2气氛下，于500℃活化2h，自然冷却至室温。
(9)量取4份25ml含有25mg/L的四环素水样，编号分别为1、2、3和4，分别在四组样品中加入0.1g的生物质基材料，其中1号体系在50kHz下超声5min，2号体系在50kHz下超声10min，3号体系在50kHz下超声20min，4号体系在50kHz下超声60min，离心取上层清液测定四环素的浓度。
(10)附图2的投射电镜可以证明成功的制备处理生物质基压电复合材料，有着纳米花状的结构。
实施例3：
(1)称取等摩尔量的Bi(NO3)3和Fe(NO3)3溶于2mol/L的硝酸溶液中，再加入25ml的2mol/L的氢氧化钠溶液进行沉淀，在室温下，转速600rpm/min搅拌15min。
(2)将所得的沉淀物用蒸馏水清洗三次后，放到干燥箱中在40℃下干燥5天，再将干燥后的物质进行研磨，得到BiFeO3粉体的前驱体。
(3)将小麦秸秆用去离子水和乙醇多次清洗，洗去上面的污渍和杂质，然后将其放置在80℃的干燥箱中进行6h干燥，除去水分，冷却至室温。
(4)使用粉碎机将其粉碎，过200目筛后即得到预处理的原料。
(5)称取质量为0.5g的生物质粉末，按照生物质与铁酸铋的质量比1:2混合均匀。
(6)将(5)得到的混合粉末加入到聚四氟球磨釜中，按照物料与氧化镐球的质量比为1:100～500的质量比加入氧化锆球，在转速为500～1500rpm/min条件下，球磨3～5h，得到生物质基压电催化材料前驱体粉末。
(8)将前驱体粉末至于管式炉中，在N2气氛下，于600℃烧结2h，自然冷却至室温。
(9)量取4份25ml含有25mg/L的罗丹明B水样，编号分别为1、2、3和4，分别在四组样品中加入0.1g的生物质基材料，其中1号体系在30kHz下超声5min，2号体系在30kHz下超声10min，3号体系在30kHz下超声20min，4号体系在30kHz下超声60min，离心取上层清液测定罗丹明B的浓度。
Claims (1)
1.一种柔性生物质基压电材料的应用，其特征在，具体步骤如下：
1）准确称量0.5 g棉花放置到乙酸锌溶液10 mL中浸泡，然后按乙酸锌，氢氧化钠的摩尔比为1：4准确移取乙酸锌溶液和氢氧化钠溶液至锥形瓶，加入磁子在转速为600 rpm/min条件下，搅拌30 min，得到前驱体；
2）将步骤1）得到的前驱体放置到聚四氟乙烯内胆的反应釜中，转移至真空干燥箱中在100-180 ℃下进行水热反应，反应时间14 h，反应完成后取出后自然冷却至室温；
3）将步骤2）得到的材料放置到聚四氟乙烯内胆的反应釜中，转移至真空干燥箱中在100-180 ℃下进行水热反应，反应时间6-18 h后取出后自然冷却至室温；
4）将反应后前驱体放置到培养皿中在80 ℃下干燥12 h，使其充分干燥;
5）将干燥完成后的材料置于管式加热炉中，在N2气氛下于300-500 ℃活化2 h，并自然冷却至室温；
6）收集冷却后的产物，得到生物质基压电催化剂材料;
7）量取4份25 mL 含有25 mg/L的罗丹明B水样，编号分别为1、2、3和4，分别在四组样品中加入0.1 g的生物质基材料，其中1号体系在50 kHz下超声5分钟，2号体系在50 kHz下超声10分钟，3号体系在50 kHz下超声20分钟，4号体系在50 kHz下超声60分钟，离心取上层清液测定罗丹明B的浓度。
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