磺化聚苯醚基复合高温质子交换膜的制备及性能研究
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摘要
质子交换膜燃料电池(PEMFC)是以氢气或甲醇作为燃料,将燃料的化学能直接转变成电能,具有能量转换率高、无污染等特点,是一种很有前途的高效绿色能源动力源。质子交换膜(Proton Exchange Membrane,PEM)是PEMFC中的关键材料之一,对其研究开发具有非常重要的意义。虽然杜邦公司生产的Nafion膜在PEMFC中已成功应用,但其工作温度受限、费用昂贵等不足限制了它更为广泛的应用。而高温(120-200°C)下质子交换膜燃料电池的运行具有更多有利之处,如提高Pt催化剂对CO的耐受性;简化水、热管理;提高电化学反应速度以提高电池性能等,因此,开发高效、低成本的新型质子交换膜,特别是耐高温、能在低湿度环境运行的非氟质子交换膜便成为燃料电池技术亟待解决的关键问题。
由于芳香族聚合物具有良好的热稳定性和较高的强度,因此,其磺化产品是制备质子交换摸的理想材料。本文采用热性能、电性能等综合性能优良的工程塑料聚苯醚(PPO)为原料,以氯磺酸为磺化剂制备磺化聚苯醚(SPPO),并通过红外和核磁共振对结构进行了验证。通过探讨磺化剂用量与产物磺化度(Degree of Sulfonation,DS)的关系,并测试磺化度不同对SPPO溶解性、电导率、拉伸强度、含水率和溶胀度等的影响,得到优选的磺化度值为35%。将此磺化度的SPPO与咪唑(Im)共混,以DMF为溶剂,采用溶液浇铸法制备了Br?nsted酸-碱型磺化聚苯醚-咪唑复合质子交换膜。并分析了不同咪唑掺杂量对最终薄膜电导率、热稳定性、微观结构、机械性能等的影响:所制备的SPPO-xIm系列膜具有良好的热稳定性,可满足高温质子交换膜工作温度的要求;呈现低的溶胀度和适中的含水率;SPPO-xIm膜的电导率随着温度增加而增加,最佳掺杂量x (Im/SPPO单元的摩尔比) = 2,200°C、33%相对湿度时SPPO-2Im膜的电导率可达6.92×10-3S/cm,电导率与温度间符合Arrhenius方程,在高温、低湿度条件下,主要遵循的是Grotthuss机理;DMA结果显示SPPO-2Im是一种硬而韧的材料。
研究了Br?nsted碱的碱性对复合电解质膜电导率的影响:以咪唑、吡唑、苯并咪唑、1-甲基咪唑、4-甲基咪唑五种Br?nsted碱掺杂制备了五种以SPPO为基底的Br?nsted acid-base复合膜,其质子电导率相差一个数量级,说明对于掺杂的Br?nsted碱来说,不但要考虑pKa的大小,更要考虑Br?nsted碱的分子体积、基团空间位置对构型重排(质子传导)的影响。
以离子浸渍-沉淀法在SPPO-2Im膜的基础上制备了无机-有机复合质子交换膜SPPO/Im/nano-ZrP(zirconium phosphate, ZrP),该复合膜具有良好的热稳定性;形态分析显示生成的磷酸锆颗粒的尺寸在纳米级别范围;XRD显示生成了α-ZrP;与SPPO-2Im膜相比,SPPO/Im/ZrP复合膜的含水率和溶胀度有不同程度的提高。确定了优化反应条件:反应温度在80°C、与氯氧化锆溶液作用时间在6 h、与磷酸溶液作用时间在12 h、反应物浓度C Zr4+:C H3PO4为1:1时,所制备复合膜的质子电导率较高,120-200°C、35% RH时可以达到10-2 S/cm。
尝试了咪唑在复合膜中的固定化研究:通过亲核取代反应将咪唑环接枝到烷氧基硅烷上,生成2- (三乙氧基硅丙基)硫基-咪唑,与磺化聚苯醚共混成膜后,放入H2O+ NH3 + EtOH + TEOS的混合体系中,水解、缩合以固定咪唑基团,所制备的接枝有咪唑基团的改性聚硅氧烷/磺化聚苯醚复合膜的质子电导率较低,为10-6 S/cm。虽然需要进一步改进,但较单纯以小分子修饰易造成掺杂物流失的局面,提供了接枝固定的新思路,如果调整咪唑接枝碳链的长短,有可能提高其质子电导率。
对于膜电极和PEMFC单电池测试,相关的实验尚待进一步展开,但以上的初步探索表明,SPPO-2Im、SPPO/Im/ZrP复合膜有可能运用于120-200°C温度区域的PEMFC。
Proton exchange membrane fuel cells (PEMFC) are attracting people’s attention as clean power sources for vehicular transportation and their potential applications in electrochemical devices. PEMFC has been considered as a promising energy source because of their high efficiency at low temperatures, easily constructed and environment friendly. As one of key components for the PEMFC system, the study of PEM is very important in the development of PEMFC. The commercially available Nafion membranes produced by DuPont have been extensively employed in PEMFC. However, there are still many shortcomings will bind their wider application in PEMFC, including limited operation temperatures, high methanol permeability and high cost. However, a number of advantages were reported for PEMFC to be operated at high temperature (120-200°C), such as improved CO tolerance of the platinum electrode, simplified water and heat managements, and increased the energy efficiency. Thus the preparation of new PEMs which providing a good performance at high temperature and low relative humidity is still one of the critical challenges in the area of fuel cell technologies.
Due to its good thermal stabilities and high performance, aromatic polymers have been widely employed as PEMFC materials. In this paper, sulfonated poly(phenylene oxide) (SPPO) was prepared through sulfonating poly(phenylene oxide) with chlorosulfonic acid, and its comprehensive properties were investigated. The structure of SPPO was confirmed by FTIR and 1HNMR, and the influences of the factors affecting the sulfonation reaction were studied. In addition, series SPPO membranes with different degree of sulfonation (DS), was also investigated, and the optimum of DS, 35%, was obtained. SPPO-xIm composite membranes with different content of imidazole (Im) from 0.25 to 4 in SPPO (35%DS) polymer matrix were prepared by solution cast film. The relation between doping ratio x (x is the molar ratio of Im to SPPO repeat unit) and membranes properties were studied by means of thermogravimetric-differential thermal analysis (TG-DTA), X-ray diffraction (XRD), dynamic mechanical analysis (DMA), and scanning electronic microscope (SEM); and the investigation of conductivity activation energies of the SPPO-xIm at different relative humidity was also performed. TG-DTA curves reveal that these SPPO-xIm composite materials had a high thermal stability, and all these membranes show a lower swelling degree and moderate uptake. The proton conductivity of SPPO-xIm composite material increased with the temperature, and the maximum proton conductivity of SPPO-xIm composite materials was found to be 6.92×10-3 S/cm at 200°C, 33%RH and x = 2. Under high temperature and low relative humidity condition, the proton conduction was mainly in accordance with“Grotthuss mechanism”. Measurement results of DMA showed that the SPPO-2Im composite membranes possess excellent rigidity and tenacity.
In this study, the effect of Br?nsted basicity on the proton conductivity of composite PEMs was also discussed. Five acid-base composite materials with different basicity were prepared by doping of SPPO of 35% DS with different Br?nsted bases, such as imidazole (Im), pyrazole (Py), benzimidazole (BnIm), 1-methylimidazole (1-MeIm) and 4-methylimidazole (4-MeIm) respectively. The resulting proton conductivities of the SPPO-heterocyclic composite membranes showed differences at approximately one order of magnitude at a high temperature and 33%RH condition, which reveals that the proton conductivities were related with not only dissociation constant (pKa), but also the molecular structure of basic heterocyclic.
Based on SPPO-2Im, SPPO/2Im/nano-23wt%ZrP (zirconium phosphate) organic-inorganic composite membranes were prepared by method of ion impregnation-precipitation. TG-DTA analysis showed that SPPO/2Im/nano-23wt%ZrP has a high thermal stability. SEM pictures showed that the ZrP particles uniformly dispersed in the SPPO matrix and the size of ZrP particles reached nanometer level. XRD spectra showed thatα-ZrP was generated. Water uptake and swelling degree of SPPO/2Im/nano-23wt%ZrP was higher than that of SPPO-2Im membrane. This SPPO/2Im/nano-23wt%ZrP membrane provided proton conductivity as high as 10-2 S/cm at 120-200°C and 33%RH conduction. The optimized preparation ways were obtained: the reaction temperature was 80°C, the concentration ratio of C Zr4+/C H3PO4was 1, and the reaction time with zirconyl chloride and phosphoric acid was 6h and 12h respectively.
The fixation of imidazole in composite membrane was also attempted. Imidazole ring were grafted on alkoxysilane with a nucleophilic reaction to synthesis 2-((3-triethoxysilylpropyl) thio)-imidazole, which was mixed with SPPO to form hybrid composite membranes with fixed imidazole rings by cross linkage. The hybrid composite membranes exhibited a low proton conductivity of approximately 10-6 S/cm. Although it needs further improvement, by comparing with the situation that imidazole dopant gets lost from membrane, it provide new idea of immobilization of imidazole.
The above primary exploration indicate that SPPO-2Im、SPPO/Im/ZrP composite membranes can be applied on PEMFC at 120-200°C.
由于芳香族聚合物具有良好的热稳定性和较高的强度,因此,其磺化产品是制备质子交换摸的理想材料。本文采用热性能、电性能等综合性能优良的工程塑料聚苯醚(PPO)为原料,以氯磺酸为磺化剂制备磺化聚苯醚(SPPO),并通过红外和核磁共振对结构进行了验证。通过探讨磺化剂用量与产物磺化度(Degree of Sulfonation,DS)的关系,并测试磺化度不同对SPPO溶解性、电导率、拉伸强度、含水率和溶胀度等的影响,得到优选的磺化度值为35%。将此磺化度的SPPO与咪唑(Im)共混,以DMF为溶剂,采用溶液浇铸法制备了Br?nsted酸-碱型磺化聚苯醚-咪唑复合质子交换膜。并分析了不同咪唑掺杂量对最终薄膜电导率、热稳定性、微观结构、机械性能等的影响:所制备的SPPO-xIm系列膜具有良好的热稳定性,可满足高温质子交换膜工作温度的要求;呈现低的溶胀度和适中的含水率;SPPO-xIm膜的电导率随着温度增加而增加,最佳掺杂量x (Im/SPPO单元的摩尔比) = 2,200°C、33%相对湿度时SPPO-2Im膜的电导率可达6.92×10-3S/cm,电导率与温度间符合Arrhenius方程,在高温、低湿度条件下,主要遵循的是Grotthuss机理;DMA结果显示SPPO-2Im是一种硬而韧的材料。
研究了Br?nsted碱的碱性对复合电解质膜电导率的影响:以咪唑、吡唑、苯并咪唑、1-甲基咪唑、4-甲基咪唑五种Br?nsted碱掺杂制备了五种以SPPO为基底的Br?nsted acid-base复合膜,其质子电导率相差一个数量级,说明对于掺杂的Br?nsted碱来说,不但要考虑pKa的大小,更要考虑Br?nsted碱的分子体积、基团空间位置对构型重排(质子传导)的影响。
以离子浸渍-沉淀法在SPPO-2Im膜的基础上制备了无机-有机复合质子交换膜SPPO/Im/nano-ZrP(zirconium phosphate, ZrP),该复合膜具有良好的热稳定性;形态分析显示生成的磷酸锆颗粒的尺寸在纳米级别范围;XRD显示生成了α-ZrP;与SPPO-2Im膜相比,SPPO/Im/ZrP复合膜的含水率和溶胀度有不同程度的提高。确定了优化反应条件:反应温度在80°C、与氯氧化锆溶液作用时间在6 h、与磷酸溶液作用时间在12 h、反应物浓度C Zr4+:C H3PO4为1:1时,所制备复合膜的质子电导率较高,120-200°C、35% RH时可以达到10-2 S/cm。
尝试了咪唑在复合膜中的固定化研究:通过亲核取代反应将咪唑环接枝到烷氧基硅烷上,生成2- (三乙氧基硅丙基)硫基-咪唑,与磺化聚苯醚共混成膜后,放入H2O+ NH3 + EtOH + TEOS的混合体系中,水解、缩合以固定咪唑基团,所制备的接枝有咪唑基团的改性聚硅氧烷/磺化聚苯醚复合膜的质子电导率较低,为10-6 S/cm。虽然需要进一步改进,但较单纯以小分子修饰易造成掺杂物流失的局面,提供了接枝固定的新思路,如果调整咪唑接枝碳链的长短,有可能提高其质子电导率。
对于膜电极和PEMFC单电池测试,相关的实验尚待进一步展开,但以上的初步探索表明,SPPO-2Im、SPPO/Im/ZrP复合膜有可能运用于120-200°C温度区域的PEMFC。
Proton exchange membrane fuel cells (PEMFC) are attracting people’s attention as clean power sources for vehicular transportation and their potential applications in electrochemical devices. PEMFC has been considered as a promising energy source because of their high efficiency at low temperatures, easily constructed and environment friendly. As one of key components for the PEMFC system, the study of PEM is very important in the development of PEMFC. The commercially available Nafion membranes produced by DuPont have been extensively employed in PEMFC. However, there are still many shortcomings will bind their wider application in PEMFC, including limited operation temperatures, high methanol permeability and high cost. However, a number of advantages were reported for PEMFC to be operated at high temperature (120-200°C), such as improved CO tolerance of the platinum electrode, simplified water and heat managements, and increased the energy efficiency. Thus the preparation of new PEMs which providing a good performance at high temperature and low relative humidity is still one of the critical challenges in the area of fuel cell technologies.
Due to its good thermal stabilities and high performance, aromatic polymers have been widely employed as PEMFC materials. In this paper, sulfonated poly(phenylene oxide) (SPPO) was prepared through sulfonating poly(phenylene oxide) with chlorosulfonic acid, and its comprehensive properties were investigated. The structure of SPPO was confirmed by FTIR and 1HNMR, and the influences of the factors affecting the sulfonation reaction were studied. In addition, series SPPO membranes with different degree of sulfonation (DS), was also investigated, and the optimum of DS, 35%, was obtained. SPPO-xIm composite membranes with different content of imidazole (Im) from 0.25 to 4 in SPPO (35%DS) polymer matrix were prepared by solution cast film. The relation between doping ratio x (x is the molar ratio of Im to SPPO repeat unit) and membranes properties were studied by means of thermogravimetric-differential thermal analysis (TG-DTA), X-ray diffraction (XRD), dynamic mechanical analysis (DMA), and scanning electronic microscope (SEM); and the investigation of conductivity activation energies of the SPPO-xIm at different relative humidity was also performed. TG-DTA curves reveal that these SPPO-xIm composite materials had a high thermal stability, and all these membranes show a lower swelling degree and moderate uptake. The proton conductivity of SPPO-xIm composite material increased with the temperature, and the maximum proton conductivity of SPPO-xIm composite materials was found to be 6.92×10-3 S/cm at 200°C, 33%RH and x = 2. Under high temperature and low relative humidity condition, the proton conduction was mainly in accordance with“Grotthuss mechanism”. Measurement results of DMA showed that the SPPO-2Im composite membranes possess excellent rigidity and tenacity.
In this study, the effect of Br?nsted basicity on the proton conductivity of composite PEMs was also discussed. Five acid-base composite materials with different basicity were prepared by doping of SPPO of 35% DS with different Br?nsted bases, such as imidazole (Im), pyrazole (Py), benzimidazole (BnIm), 1-methylimidazole (1-MeIm) and 4-methylimidazole (4-MeIm) respectively. The resulting proton conductivities of the SPPO-heterocyclic composite membranes showed differences at approximately one order of magnitude at a high temperature and 33%RH condition, which reveals that the proton conductivities were related with not only dissociation constant (pKa), but also the molecular structure of basic heterocyclic.
Based on SPPO-2Im, SPPO/2Im/nano-23wt%ZrP (zirconium phosphate) organic-inorganic composite membranes were prepared by method of ion impregnation-precipitation. TG-DTA analysis showed that SPPO/2Im/nano-23wt%ZrP has a high thermal stability. SEM pictures showed that the ZrP particles uniformly dispersed in the SPPO matrix and the size of ZrP particles reached nanometer level. XRD spectra showed thatα-ZrP was generated. Water uptake and swelling degree of SPPO/2Im/nano-23wt%ZrP was higher than that of SPPO-2Im membrane. This SPPO/2Im/nano-23wt%ZrP membrane provided proton conductivity as high as 10-2 S/cm at 120-200°C and 33%RH conduction. The optimized preparation ways were obtained: the reaction temperature was 80°C, the concentration ratio of C Zr4+/C H3PO4was 1, and the reaction time with zirconyl chloride and phosphoric acid was 6h and 12h respectively.
The fixation of imidazole in composite membrane was also attempted. Imidazole ring were grafted on alkoxysilane with a nucleophilic reaction to synthesis 2-((3-triethoxysilylpropyl) thio)-imidazole, which was mixed with SPPO to form hybrid composite membranes with fixed imidazole rings by cross linkage. The hybrid composite membranes exhibited a low proton conductivity of approximately 10-6 S/cm. Although it needs further improvement, by comparing with the situation that imidazole dopant gets lost from membrane, it provide new idea of immobilization of imidazole.
The above primary exploration indicate that SPPO-2Im、SPPO/Im/ZrP composite membranes can be applied on PEMFC at 120-200°C.
引文
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