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石墨烯基双金属(氢)氧化物/聚苯胺复合材料的制备及热稳定性
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/9/4 8:02:51  

摘要:聚苯胺(PANI)因具有高储能、低成本、合成简单等良好的物理化学性质,而在催化、吸附、传感器、和超级电容器等领域有广泛的应用。然而,其热稳定性较差,容易导致设备失效甚至火灾发生。更重要的是,PANI在高温下会发生热分解,释放出大量的热和有毒气体,对人类的健康和生命财产安全构成巨大威胁。本文通过在聚苯胺中引入金属(氢)氧化物(MFe2O4和LDH)(M为Zn或Ni)和石墨烯载体,对聚苯胺进行改性,制备了金属(氢)氧化物/聚苯胺/还原氧化石墨烯复合材料(MFe2O4 (LDH)/PANI/RGO)。通过研究复合物制备条件(盐酸浓度以及氧化程度)、组分配比等对复合物热稳定的影响,改善复合物的热稳定性,提高复合物在实际应用中的安全性能。主要研究内容如下:

(1)   以苯胺、盐酸和过硫酸铵为原料,通过原位聚合法成功制备了不同浓度盐酸掺杂的PANI,以及不同氧化程度的PANI。通过X-射线衍射(XRD)和傅立叶变换红外光谱(FT-IR)对复合材料的结构进行了表征。并通过热重分析仪测试了聚苯胺复合材料的热稳定性,对实验条件进行优化的结果显示,酸掺杂浓度为c(HCl)=1 M,氧化程度为n(An) : n(APS)=1制备的复合物热稳定性最佳。

(2)   以苯胺、盐酸、过硫酸铵、氧化石墨、硝酸镍以及硝酸铁为原料,通过原位聚合法结合水热法成功制备了NiFe2O4/PANI/RGO复合材料。通过X-射线衍射(XRD)、傅立叶变换红外光谱(FT-IR)、场发射扫描电镜(FESEM)、透射电子显微镜(TEM)、能谱仪(EDS)和元素映射(Mapping)等对复合材料的结构和形貌进行了表征。表征结果显示NiFe2O4包裹在PANI内,复合材料呈中空结构,NiFe2O4纳米颗粒和RGO的负载增加了PANI的尺寸。热分析结果表明,当NiFe2O4的含量为2 wt%,RGO的含量为1 wt%时,三元复合材料NiFe2O4/PANI/RGO的热稳定性达到最佳。与PANI相比,其初始分解温度提高了126 °C,说明NiFe2O4和RGO的引入,极大地改善了PANI的热稳定性。与文献相比,本文所制备的NiFe2O4/PANI/RGO复合材料具有更高的热稳定性。此外,还探究了不同升温速率(5 °C/min、10 °C/min、15 °C/min和20 °C/min)和不同气氛(空气和氮气)对NiFe2O4/PANI/RGO热稳定性的影响。

(3)   以苯胺、盐酸、过硫酸铵、氧化石墨、硝酸镍以及硝酸铝为原料,采用两步法(原位聚合法和水热法)成功制备了NiAl LDH/PANI/RGO复合材料。通过XRD、FT-IR、FESEM、TEM、EDS和Mapping等对复合材料的结构和形貌进行了表征,结果显示NiAl LDH纳米片包裹在PANI内,NiAl LDH纳米片和RGO的负载增加了PANI的尺寸。热分析结果表明,当NiAl LDH的含量为10 wt%,RGO的含量为10 wt%时,三元复合材料NiAl LDH/PANI/RGO的热稳定性最佳。与PANI相比,其开始分解温度提高了132 °C,这说明了NiAl LDH和RGO的引入,极大地改善了PANI的热稳定性。与文献相比,本文所制备的NiAl LDH/PANI/RGO复合材料具有更好的热稳定性。此外,还探究了不同升温速率和气氛对NiAl LDH/PANI/RGO热稳定性的影响。

(4)   以苯胺、盐酸、过硫酸铵、氧化石墨、硝酸锌以及硝酸铁为原料,利用原位聚合法制备了ZnFe2O4/PANI复合材料,再通过水热法成功制备了ZnFe2O4/PANI/RGO复合材料。通过XRD、FT-IR、FESEM、TEM、EDS和Mapping等对复合材料的结构和形貌进行了表征,表征结果显示,ZnFe2O4包裹在PANI内,复合材料呈中空结构,ZnFe2O4纳米颗粒和RGO的负载增加了PANI的尺寸。热分析结果表明,当ZnFe2O4的含量为4 wt%复合材料,RGO的含量为5 wt%时,三元复合材料ZnFe2O4/PANI/RGO的热稳定性最佳。与PANI相比,其开始分解温度提高了77 °C,这说明了ZnFe2O4和RGO的引入,极大地改善了PANI的热稳定性。此外,还探究了不同升温速率和气氛对ZnFe2O4/PANI/RGO热稳定性的影响。值得一提的是,ZnFe2O4/PANI/RGO复合材料的制备过程中没有使用任何有毒的化学还原剂,因此用该方法制备ZnFe2O4/PANI/RGO复合材料,与文献报道的相比,更加绿色环保。

Polyaniline (PANI) has been widely used in catalysis, adsorption, sensors, supercapacitors and other fields due to its high energy storage, low cost and simple synthesis. However, its thermal stability is poor, which can easily lead to equipment failure or even fire. More importantly, PANI will undergo thermal decomposition at high temperature, releasing a large number of heat and toxic gases, which poses a great threat to human health, life and property safety. In this paper, polyaniline was modified by introducing doubled metal (hydro) oxide (MFe2O4 and LDH) (M is Zn or Ni) and graphene carrier into polyaniline. Doubled metal (hydro) oxide/polyaniline/reduced graphene oxide composite (MFe2O4 (LDH)/PANI/RGO) was prepared. The effects of preparation conditions (concentration of hydrochloric acid and degree of oxidation) and composition ratio on the thermal stability of the composite were studied to improve the thermal stability of the composite and the safety performance of the composite in practical application. The main research contents are as follows:

(1) PANI doped with different concentrations of hydrochloric acid and PANI with different degrees of oxidation were successfully prepared by in situ polymerization from aniline, hydrochloric acid and ammonium persulfate. The structure of the composites was characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The thermal stability of polyaniline composites was tested by thermogravimetric analyzer. The experimental conditions were optimized. The results showed that the composites prepared with acid doping concentration c(HCl)=1 M and oxidation degree n(An): n(APS)=1 had the best thermal stability.

(2) NiFe2O4/PANI/RGO composites were successfully prepared from aniline, hydrochloric acid, ammonium persulfate, graphite oxide, nickel nitrate and ferric nitrate by in situ polymerization and hydrothermal method. The structure and morphology of the composites were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy dispersive spectrometer (EDS) and element mapping (Mapping). The characterization results showed that NiFe2O4 was encapsulated in PANI, and the composite was hollow. The size of PANI was increased by the loading of NiFe2O4 nanoparticles and RGO. The results of thermal analysis show that the thermal stability of ternary composite NiFe2O4/PANI/RGO is the best when the content of NiFe2O4 is 2 wt% and the content of RGO is 1 wt%. Compared with PANI, the initial decomposition temperature of PANI is increased by 126 °C, which indicates that the introduction of NiFe2O4 and RGO greatly improves the thermal stability of PANI. Compared with the literature, the NiFe2O4/PANI/RGO composites prepared in this paper have higher thermal stability. In addition, the effects of different heating rates (5 °C/min, 10 °C/min, 15 °C/min and 20 °C/min) and different atmospheres (air and nitrogen) on the thermal stability of NiFe2O4/PANI/RGO were investigated;

(3) NiAl LDH/PANI/RGO composites were successfully prepared from aniline, hydrochloric acid, ammonium persulfate, graphite oxide, nickel nitrate and aluminium nitrate by two-step method (in situ polymerization and hydrothermal method). The structure and morphology of the composites were characterized by XRD, FT-IR, FESEM, TEM, EDS and Mapping. The results showed that NiAl LDH nanosheets were encapsulated in PANI, and the loading of NiAl LDH nanosheets and RGO increased the size of PANI. Thermal analysis results show that the ternary composite NiAl LDH/PANI/RGO has the best thermal stability when the content of NiAl LDH is 10 wt% and RGO is 10 wt%. Compared with PANI, the initial decomposition temperature of PANI is increased by 132 °C, which indicates that the introduction of NiAl LDH and RGO greatly improves the thermal stability of PANI.

关键词:聚苯胺;热稳定性;双金属(氢)氧化物;石墨烯

Polyaniline; Thermal stability; Doubled metal (hydro) oxide; Graphene

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