CN107099055B - 一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法 - Google Patents
一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法。包括以下步骤：凹凸棒土/三氧化钨的制备，凹凸棒土/三氧化钨/聚吡咯的制备，凹凸棒土/三氧化钨/聚吡咯/石墨烯的制备，三氧化钨/聚吡咯/石墨烯的制备。本发明的有益效果是凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法新颖独特。
Description
技术领域
本发明涉及一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，属于材料合成领域。
技术背景
近年来，石墨烯与导电高分子及过渡金属氧化物复合材料已经引起了研究工作者越来越多的关注，已经成为电化学研究的前言领域之一。三氧化钨是稳定的n型半导体材料，已经被广泛的应用在气体传感器和电化学催化等方面。近几年已经有部分研究将三氧化钨应用在电化学储能方面，研究表明三氧化钨与石墨烯气凝胶复合材料能表现出极好的电容性能。聚吡咯具有较高的导电性和生物相容性，环境友好，稳定性好。石墨烯是从石墨材料中剥离出来的并且由碳原子组成的只有一层原子厚度的二维晶体，石墨烯既是最薄的材料，也是最强韧的材料，同时它还具有很好的弹性。每个碳原子均为sp2杂化，并贡献剩余一个p轨道上的电子形成大π键，π电子可以自由移动，赋予石墨烯良好的导电性。凹凸棒土又称坡缕石或坡缕缟石，是一种具链层状结构的含水富镁硅酸盐粘土矿物。凹凸棒石形态呈毛发状或纤维状，通常为毛毯状或土状集合体。模板法制备的材料具有良好的形貌结构。因此，通过凹凸棒土为模板通过逐步合成的方法合成三氧化钨/聚吡咯/石墨烯复合材料。
发明内容
本发明的目的是在于提供一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法。
本发明所述一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，包括以下步骤：
a、凹凸棒土/三氧化钨的制备：称取凹凸棒土超声分散在20mL溶有磷钨酸的乙醇中，在室温下干燥完全后在空气条件下煅烧4h，将煅烧后的样品二次分散在20mL溶有1g磷钨酸的乙醇中，在室温下干燥完全后在空气条件下二次煅烧4h；
b、凹凸棒土/三氧化钨/聚吡咯的制备：将1g步骤a中所制备的凹凸棒土/三氧化钨超声分散在50mL 20％的乙醇溶液中，加入吡咯单体，然后迅速加入50mL 20％的乙醇，紧接着加入六水氯化铁溶液，室温搅拌，最后将生成物离心，洗涤，冷冻干燥；
c、凹凸棒土/三氧化钨/聚吡咯/石墨烯的制备：将1g步骤b中所制备的凹凸棒土/三氧化钨/聚吡咯超声分散在50mL 1mg mL-1的氧化石墨烯的分散液中，加入4.5mL的浓盐酸，然后加入锌粉超声30min，紧接着加入5mL浓盐酸除去过量的锌粉，最后将生成物离心，洗涤，冷冻干燥；
d、三氧化钨/聚吡咯/石墨烯的制备：将步骤c中所制备凹凸棒土/三氧化钨/聚吡咯/石墨烯复合物分散到40％的氢氟酸中，搅拌48h，最后将生成物离心，洗涤，冷冻干燥。
进一步，所述步骤a中凹凸棒土的量为1～5g，磷钨酸的量为1～5g，首次煅烧温度为200～500℃，二次煅烧温度为400～800℃。
进一步，所述步骤b中吡咯单体的量为0.05～0.3g，六水氯化铁的量1～5g，搅拌时间为10～20h。
进一步，所述步骤c中加入锌粉的量为200～500mg。
本发明的有益效果是：凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法新颖独特。
具体实施方式
现在结合具体实施例对本发明做进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例一：
凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，包括以下步骤：
(1)称取4g凹凸棒土超声分散在20mL溶有2g磷钨酸的乙醇中，在室温下干燥完全后在空气条件下350℃煅烧4h，将煅烧后的样品二次分散在20mL溶有1g磷钨酸的乙醇中，在室温下干燥完全后在空气条件下550℃二次煅烧4h。
(2)将1g步骤(1)中所制备的凹凸棒土/三氧化钨超声分散在50mL 20％的乙醇溶液中，加入0.1g吡咯单体，然后迅速加入50mL 20％的乙醇，紧接着加入3g六水氯化铁溶液，室温搅拌，最后将生成物离心，洗涤，冷冻干燥。
(3)将1g步骤(2)中所制备的凹凸棒土/三氧化钨/聚吡咯超声分散在50mL 1mgmL-1的氧化石墨烯的分散液中，加入4.5mL的浓盐酸，然后加入400mg锌粉超声30min，紧接着加入5mL浓盐酸除去过量的锌粉，最后将生成物离心，洗涤，冷冻干燥。
(4)将步骤(3)中所制备凹凸棒土/三氧化钨/聚吡咯/石墨烯复合物分散到40％的氢氟酸中，搅拌48h，最后将生成物离心，洗涤，冷冻干燥。
Claims (4)
1.一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，其特征在于：步骤如下：
a、凹凸棒土/三氧化钨的制备：称取凹凸棒土超声分散在20mL溶有磷钨酸的乙醇中，在室温下干燥完全后在空气条件下煅烧4h，将煅烧后的样品二次分散在20mL溶有1g磷钨酸的乙醇中，在室温下干燥完全后在空气条件下二次煅烧4h；
b、凹凸棒土/三氧化钨/聚吡咯的制备：将1g步骤a中所制备的凹凸棒土/三氧化钨超声分散在50mL 20％的乙醇溶液中，加入吡咯单体，然后迅速加入50mL 20％的乙醇，紧接着加入六水氯化铁溶液，室温搅拌，最后将生成物离心，洗涤，冷冻干燥；
c、凹凸棒土/三氧化钨/聚吡咯/石墨烯的制备：将1g步骤b中所制备的凹凸棒土/三氧化钨/聚吡咯超声分散在50mL 1mg mL-1的氧化石墨烯的分散液中，加入4.5mL的浓盐酸，然后加入锌粉超声30min，紧接着加入5mL浓盐酸除去过量的锌粉，最后将生成物离心，洗涤，冷冻干燥；
d、三氧化钨/聚吡咯/石墨烯的制备：将步骤c中所制备凹凸棒土/三氧化钨/聚吡咯/石墨烯复合物分散到40％的氢氟酸中，搅拌48h，最后将生成物离心，洗涤，冷冻干燥。
2.根据权利要求1所述一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，其特征是：所述步骤a中凹凸棒土的量为1～5g，磷钨酸的量为1～5g，首次煅烧温度为200～500℃，二次煅烧温度为400～800℃。
3.根据权利要求1所述一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，其特征是：所述步骤b中吡咯单体的量为0.05～0.3g，六水氯化铁的量1～5g，搅拌时间为10～20h。
4.根据权利要求1所述一种以凹凸棒土为模板的三氧化钨/聚吡咯/石墨烯复合材料的制备方法，其特征是：所述步骤c中加入锌粉的量为200～500mg。
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| Synthesis and characterization of secondary doped polypyrrole/organic Modified Attapulgite Conductive Composites;Huxia Feng et.al;《Journal of Applied Polymer Science》;20140908;第132卷(第5期);第1-8页 * |
| 导电高分子聚吡咯纳米复合材料的研究进展;汪菊英等;《塑料》;20051231;第34卷(第6期);第84-91页 * |
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