钒电池用杂萘联苯聚芳醚酮阴离子交换膜研究
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摘要
全钒氧化还原液流电池(VRB,简称钒电池)是一种新型储能电池,它的电池功率与容量独立,具有可深度放电、长寿命、维护简便等优点,是太阳能、风能等可再生能源发电及智能电网削峰填谷的理想储能装置。离子交换膜为钒电池的关键部件。全氟磺酸型的Nafion膜因其优良的电化学性能和稳定性而广泛地被用作钒电池隔膜,但是Nafion膜阻钒性能欠佳,价格昂贵,限制了钒电池的推广应用。因此有必要开发替代膜,开展相关的膜材料研究。杂萘联苯聚醚酮(PPEK)和杂萘联笨聚醚酮酮(PPEKK)是高性能高分子材料,具有机械强度高、化学稳定性好等特点。与全氟磺酸膜材料相比,杂萘联苯聚芳醚酮类膜材料具有显著的低成本优势。
分别用浓硫酸、硝基苯为溶剂对PPEKK进行氯甲基化改性制备氯甲基化杂萘联苯聚醚酮酮(CMPPEKK)。系统研究了PPEKK的氯甲基化改性工艺,考察了反应因素对产物氯甲基化程度的影响。对产物进行了红外光谱、核磁氢谱表征,结果表明氯甲基被成功地引入到聚合物中。CMPPEKK的氯甲基含量介于0.9～1.9mmol/g之间。CMPPEKK基膜经三甲胺胺化制备季铵化杂萘联苯聚醚酮酮(QAPPEKK)阴离子交换膜,详细考察了胺化条件对QAPPEKK膜性能的影响,制备出离子交换容量(IEC)介于0.99～1.56mmol/g之间的QAPPEKK膜。对膜进行了红外光谱、热性能分析；测试了膜的基本性能及其应用于钒电池的单电池性能。单电池性能测试结果表明,在相同电流密度下(20～80mA/cm2),QAPPEKK膜(IEC=1.56mmol/g)的单电池电流效率高于Nafionl17膜,而两者的能量效率相当。考察了QAPPEKK (?)膜在五价钒溶液中的稳定性和在钒电池中连续运行的稳定性,结果表明QAPPEKK膜具有较好的稳定性。
以吡啶为胺化试剂对CMPPEKK基膜进行胺化,制备吡啶型杂茶联苯聚醚酮酮阴离子交换膜(PyPPEKK)。通过考察吡啶的稀释剂对膜性能的影响,优选出吡啶水溶液为胺化溶液。研究了胺化工艺对膜性能的影响,并对工艺条件进行优化。制备出IEC介于0.96～1.55mmol/g之间的PyPPEKK膜。对膜进行了红外光谱分析,结果表明吡啶基团被成功引入到膜中。测试了膜的基本性能及其应用于钒电池时的单电池性能。在电流密度为80mA/cm2时,单电池的电流效率可达99.2%,能量效率可达83.6%,高于相同测试条件下采用Nafionl17膜的单电池(电流效率和能量效率分别为96.8%和80.7%)。测试了PyPPEKK膜在五价钒溶液中的稳定性,考察了膜在钒电池中的连续运行稳定性,结果表明PyPPEKK膜具有较好的稳定性。
从分子结构设计出发,将甲基引入到聚合物中,利用溶液缩聚法制备二甲基杂荼联苯聚醚酮(DMPPEK)。对DMPPEK进行了红外光谱、核磁氢谱分析,结果表明制备出一系列不同甲基含量的DMPPEK。对DMPPEK进行溴化改性制备溴化二甲基杂萘联苯聚醚酮(BPPEK)。考察了溴化工艺对产物溴化结果的影响,并对工艺进行了优化。对溴化产物进行了红外光谱、核磁共振谱分析,结果表明通过溴化将甲基部分转化为单溴甲基,BPPEK的单溴甲基转化率达到50%左右,满足制备阴离子交换膜的要求。BPPEK经溶液铸膜法制备出基膜,分别采用三甲胺、毗啶对基膜进行胺化制备季铵化杂萘联苯聚醚酮(QBPPEK)、吡啶型杂萘联苯聚醚酮(PyBPPEK)阴离子交换膜。对‘膜进行了红外光谱、热性能分析。测试了膜的基本性能及其应用于钒电池的单电池性能。单电池性能测试结果表明,相同电流密度下(20～80mA/cm2), QBPPEK(IEC-1.53mmol/g)、PyBPPEK(IEC=1.50mmol/g)膜的单电池电流效率、能量效率均高于Nafionl17膜。
用溶液缩聚方法制备二甲基杂萘联苯聚醚酮酮(DMPPEKK),对DMPPEKK进行了红外光谱、核磁氢谱分析,结果表明制备出一系列具有不同甲基含量的DMPPEKK。对DMPPEKK进行溴化改性制备溴化二甲基杂萘联苯聚醚酮酮(BPPEKK)。对溴化产物进行了红外光谱、核磁共振谱分析,结果表明通过溴化制备出满足制备阴离子交换膜要求的BPPEKK。分别用三甲胺、吡啶对BPPEKK基膜胺化制备季铵化杂萘联苯聚醚酮酮(QBPPEKK)和吡啶型杂萘联苯聚醚酮酮(PyBPPEKK)阴离子交换膜。对膜进行了红外光谱分析。测试了膜的基本性能及其应用于钒电池的单电池性能。单电池性能测试结果表明,QBPPEKK(1.51mmol/g)、PyBPPEKK(1.45mmol/g)(?)膜在相同电流密度下,(20～80mA/cm2)单电池的电流效率高于Nafionl17(?)膜,而能量效率与Nafionl17膜相当。
比较研究了基于氯甲基化聚芳醚酮的阴离子交换膜与基于溴化聚芳醚酮的刚离r交换膜的结构与性能关系。结果表明,季铵化杂荼联苯聚芳醚酮阴离子交换膜与吡啶型杂萘联苯聚芳醚酮阴离子交换膜的含水率和溶胀率均随着离子交换容量的增加而增加,主链结构和甲基对膜的含水率和溶胀率影响较小。季铵化杂荼联苯聚芳醚酮阴离子交换膜比吡啶型杂萘联苯聚芳醚酮阴离子交换膜有较高的含水率和较大的溶胀率。杂茶联苯聚芳醚酮阴离子交换膜应用于单电池时的电压效率、能量效率主要受离子交换容量的影响。
Vanadium redox flow battery (VRB) is a new battery for energy storage. The power and capacity of VRB are divided. It has the advantage of deep discharge capacity, long cycle life, and maintenance convenient. The VRB is an ideal large energy storage device for renewable energy sources such as solar energy, wind energy and smart grid for load shifting. Ion exchange membrane is key component for VRB. Nafion has been used as separator for its good chemical stability and high conductivity; however, it suffers from high cost and the crossover of vanadium ions. Therefore, study on alternative membranes and related membrane materials are necessary. Poly(phthalazinone ether ketone)(PPEK) and poly(phthalazinone ether ketone ketone)(PPEKK) are high performance polymers. They have high mechanical strength and good chemical stability. The poly(phthalazinone ether ketone)s membrane materials have lower cost than that of perfluorinated sulfonic acid materials.
Chloromethyl poly(phthalazinone ether ketone ketone)(CMPPEKK) were prepared from PPEKK with sulfuric acid and nitrobenzene as solvents, respectively. The effects of reaction conditions on chloromethyl degree were studied. The resulting polymer were analysed by using FTIR and NMR. The resluts confirmed that chloromethyl groups were intrduced into polymer. The chloromethyl degree of CMPPEKK was in a range of0.9-1.9mmol/g. CMPPEKK membranes were aminated to prepare quaternized poly(phthalazinone ether ketone ketone)(QAPPEKK) anion exchange membranes. The ion exchange capacity (IEC) of QAPPEKK membranes was in a range of0.99-1.56mmol/g. Under the same current density (20-80mA/cm2), the current efficiency of VRB cell with QAPPEKK (IEC=1.56mmol/g) was higher than that of Nafion117, and the energy efficiency of both cells was comparable. QAPPEKK membranes showed good stability in VO2+solution and VRB.
Poly(phthalazinone ether ketone ketone) anion exchange membranes with pyridinium groups (PyPPEKK) were prepared from CMPPEKK and pyridine. The amimation conditions were studied and optimized. The IEC of PyPPEKK was in a range of0.96-1.55mmol/g. FTIR confirmed that pyridinium groups were introduced into membranes. At80mA/cm2, the cell with PyPPEKK (IEC=1.55mmol/g) membrane showed a current efficiency of99.2%and energy efficiency of83.6%higher than that of cell with Nafionl17(current efficiency and energy efficiency were96.8%and80.7%, respectively). The stability test in VO2+solution (?)nd cell cycling test showed that PyPPEKK membranes had good stability.
By designing the molecular structure of the polymer, the methyl groups were introduced into polymer to obtain poly(phthalazinone ether ketone) with methyl groups (DMPPEK). FTIR and NMR were used to characterize the structure of DMPPEK, the results indicated that DMPPEK were obtained. DMPPEK were brominated to prepare poly(phthalazinone ether ketone) with bromomethylated groups (BPPEK). The conversation ratio of bromomethyl groups was about50%. BPPEK was adequate to meet the requirement of preparation of anion exchange membrane. Quaternized poly(phthalazinone ether ketone)(QBPPEK) anion exchange membranes and poly(phthalazinone ether ketone) anion exchange membranes with pyridinium groups (PyBPPEK) were prepared from BPPEK with trimethylamine and pyridine, respectively. The IEC was in a range of0.82-1.53mmol/g for QBPPEK and0.85-1.50mmol/g for PyPPEK membranes, respectively. At the same current density (20-80mA/cm2), the current efficiency and energy efficiency of cells with QBPPEK (IEC=1.53mmol/g) and PyBPPEK (IEC=1.50mmol/g) were higher than those of cell with Nafionl17.
Poly(phthalazinonc ether ketone ketone) with dimethyl groups (DMPPEKK) were prepared from polycondcnsation method. Poly(phthalazinone ether ketone ketone) with bromomethylated groups (BPPEKK) was prepared from bromination of DMPPEKK. Quaternized poly(phthalazinone ketone ketone)(QBPPEKK) anion exchange membranes and poly(phthalazinone ketone ketone) with pyridinium groups (PyBPPEKK) anion exchange membranes were prepared from BPPEKK with trimethylamine and pyridine as the amination reagents, respectively. At the same current density (20-80mA/cm2), the current efficiency of cells with QBPPEK (1.51mmol/g) and PyBPPEK (1.45mmol/g) was higher than that of cell with Nafionl17, and the energy efficiencies of cells were comparable.
The relationships of structure-property of anion exchange membranes made from chloromethyl poly(phthalazinone ether ketone) and brominated poly(phthalazinone ether ketone) with dimethyl groups were investigated. The water content and swelling ratio of quaternizated poly(phthalazinone ether ketone) membranes and poly(phthalazinone ether ketone) anion exchange membranes with pyridinium groups were increased with the increasing IEC of membranes. The water content and swelling ratio of membranes with quaternary ammonium groups were higher than those of membranes with pyridinium groups. The voltage efficiency and energy efficiency of cells with poly(phthalazinone ether ketone)s membranes were mainly affected by the ion exchange capacity of membranes.
分别用浓硫酸、硝基苯为溶剂对PPEKK进行氯甲基化改性制备氯甲基化杂萘联苯聚醚酮酮(CMPPEKK)。系统研究了PPEKK的氯甲基化改性工艺,考察了反应因素对产物氯甲基化程度的影响。对产物进行了红外光谱、核磁氢谱表征,结果表明氯甲基被成功地引入到聚合物中。CMPPEKK的氯甲基含量介于0.9～1.9mmol/g之间。CMPPEKK基膜经三甲胺胺化制备季铵化杂萘联苯聚醚酮酮(QAPPEKK)阴离子交换膜,详细考察了胺化条件对QAPPEKK膜性能的影响,制备出离子交换容量(IEC)介于0.99～1.56mmol/g之间的QAPPEKK膜。对膜进行了红外光谱、热性能分析；测试了膜的基本性能及其应用于钒电池的单电池性能。单电池性能测试结果表明,在相同电流密度下(20～80mA/cm2),QAPPEKK膜(IEC=1.56mmol/g)的单电池电流效率高于Nafionl17膜,而两者的能量效率相当。考察了QAPPEKK (?)膜在五价钒溶液中的稳定性和在钒电池中连续运行的稳定性,结果表明QAPPEKK膜具有较好的稳定性。
以吡啶为胺化试剂对CMPPEKK基膜进行胺化,制备吡啶型杂茶联苯聚醚酮酮阴离子交换膜(PyPPEKK)。通过考察吡啶的稀释剂对膜性能的影响,优选出吡啶水溶液为胺化溶液。研究了胺化工艺对膜性能的影响,并对工艺条件进行优化。制备出IEC介于0.96～1.55mmol/g之间的PyPPEKK膜。对膜进行了红外光谱分析,结果表明吡啶基团被成功引入到膜中。测试了膜的基本性能及其应用于钒电池时的单电池性能。在电流密度为80mA/cm2时,单电池的电流效率可达99.2%,能量效率可达83.6%,高于相同测试条件下采用Nafionl17膜的单电池(电流效率和能量效率分别为96.8%和80.7%)。测试了PyPPEKK膜在五价钒溶液中的稳定性,考察了膜在钒电池中的连续运行稳定性,结果表明PyPPEKK膜具有较好的稳定性。
从分子结构设计出发,将甲基引入到聚合物中,利用溶液缩聚法制备二甲基杂荼联苯聚醚酮(DMPPEK)。对DMPPEK进行了红外光谱、核磁氢谱分析,结果表明制备出一系列不同甲基含量的DMPPEK。对DMPPEK进行溴化改性制备溴化二甲基杂萘联苯聚醚酮(BPPEK)。考察了溴化工艺对产物溴化结果的影响,并对工艺进行了优化。对溴化产物进行了红外光谱、核磁共振谱分析,结果表明通过溴化将甲基部分转化为单溴甲基,BPPEK的单溴甲基转化率达到50%左右,满足制备阴离子交换膜的要求。BPPEK经溶液铸膜法制备出基膜,分别采用三甲胺、毗啶对基膜进行胺化制备季铵化杂萘联苯聚醚酮(QBPPEK)、吡啶型杂萘联苯聚醚酮(PyBPPEK)阴离子交换膜。对‘膜进行了红外光谱、热性能分析。测试了膜的基本性能及其应用于钒电池的单电池性能。单电池性能测试结果表明,相同电流密度下(20～80mA/cm2), QBPPEK(IEC-1.53mmol/g)、PyBPPEK(IEC=1.50mmol/g)膜的单电池电流效率、能量效率均高于Nafionl17膜。
用溶液缩聚方法制备二甲基杂萘联苯聚醚酮酮(DMPPEKK),对DMPPEKK进行了红外光谱、核磁氢谱分析,结果表明制备出一系列具有不同甲基含量的DMPPEKK。对DMPPEKK进行溴化改性制备溴化二甲基杂萘联苯聚醚酮酮(BPPEKK)。对溴化产物进行了红外光谱、核磁共振谱分析,结果表明通过溴化制备出满足制备阴离子交换膜要求的BPPEKK。分别用三甲胺、吡啶对BPPEKK基膜胺化制备季铵化杂萘联苯聚醚酮酮(QBPPEKK)和吡啶型杂萘联苯聚醚酮酮(PyBPPEKK)阴离子交换膜。对膜进行了红外光谱分析。测试了膜的基本性能及其应用于钒电池的单电池性能。单电池性能测试结果表明,QBPPEKK(1.51mmol/g)、PyBPPEKK(1.45mmol/g)(?)膜在相同电流密度下,(20～80mA/cm2)单电池的电流效率高于Nafionl17(?)膜,而能量效率与Nafionl17膜相当。
比较研究了基于氯甲基化聚芳醚酮的阴离子交换膜与基于溴化聚芳醚酮的刚离r交换膜的结构与性能关系。结果表明,季铵化杂荼联苯聚芳醚酮阴离子交换膜与吡啶型杂萘联苯聚芳醚酮阴离子交换膜的含水率和溶胀率均随着离子交换容量的增加而增加,主链结构和甲基对膜的含水率和溶胀率影响较小。季铵化杂荼联苯聚芳醚酮阴离子交换膜比吡啶型杂萘联苯聚芳醚酮阴离子交换膜有较高的含水率和较大的溶胀率。杂茶联苯聚芳醚酮阴离子交换膜应用于单电池时的电压效率、能量效率主要受离子交换容量的影响。
Vanadium redox flow battery (VRB) is a new battery for energy storage. The power and capacity of VRB are divided. It has the advantage of deep discharge capacity, long cycle life, and maintenance convenient. The VRB is an ideal large energy storage device for renewable energy sources such as solar energy, wind energy and smart grid for load shifting. Ion exchange membrane is key component for VRB. Nafion has been used as separator for its good chemical stability and high conductivity; however, it suffers from high cost and the crossover of vanadium ions. Therefore, study on alternative membranes and related membrane materials are necessary. Poly(phthalazinone ether ketone)(PPEK) and poly(phthalazinone ether ketone ketone)(PPEKK) are high performance polymers. They have high mechanical strength and good chemical stability. The poly(phthalazinone ether ketone)s membrane materials have lower cost than that of perfluorinated sulfonic acid materials.
Chloromethyl poly(phthalazinone ether ketone ketone)(CMPPEKK) were prepared from PPEKK with sulfuric acid and nitrobenzene as solvents, respectively. The effects of reaction conditions on chloromethyl degree were studied. The resulting polymer were analysed by using FTIR and NMR. The resluts confirmed that chloromethyl groups were intrduced into polymer. The chloromethyl degree of CMPPEKK was in a range of0.9-1.9mmol/g. CMPPEKK membranes were aminated to prepare quaternized poly(phthalazinone ether ketone ketone)(QAPPEKK) anion exchange membranes. The ion exchange capacity (IEC) of QAPPEKK membranes was in a range of0.99-1.56mmol/g. Under the same current density (20-80mA/cm2), the current efficiency of VRB cell with QAPPEKK (IEC=1.56mmol/g) was higher than that of Nafion117, and the energy efficiency of both cells was comparable. QAPPEKK membranes showed good stability in VO2+solution and VRB.
Poly(phthalazinone ether ketone ketone) anion exchange membranes with pyridinium groups (PyPPEKK) were prepared from CMPPEKK and pyridine. The amimation conditions were studied and optimized. The IEC of PyPPEKK was in a range of0.96-1.55mmol/g. FTIR confirmed that pyridinium groups were introduced into membranes. At80mA/cm2, the cell with PyPPEKK (IEC=1.55mmol/g) membrane showed a current efficiency of99.2%and energy efficiency of83.6%higher than that of cell with Nafionl17(current efficiency and energy efficiency were96.8%and80.7%, respectively). The stability test in VO2+solution (?)nd cell cycling test showed that PyPPEKK membranes had good stability.
By designing the molecular structure of the polymer, the methyl groups were introduced into polymer to obtain poly(phthalazinone ether ketone) with methyl groups (DMPPEK). FTIR and NMR were used to characterize the structure of DMPPEK, the results indicated that DMPPEK were obtained. DMPPEK were brominated to prepare poly(phthalazinone ether ketone) with bromomethylated groups (BPPEK). The conversation ratio of bromomethyl groups was about50%. BPPEK was adequate to meet the requirement of preparation of anion exchange membrane. Quaternized poly(phthalazinone ether ketone)(QBPPEK) anion exchange membranes and poly(phthalazinone ether ketone) anion exchange membranes with pyridinium groups (PyBPPEK) were prepared from BPPEK with trimethylamine and pyridine, respectively. The IEC was in a range of0.82-1.53mmol/g for QBPPEK and0.85-1.50mmol/g for PyPPEK membranes, respectively. At the same current density (20-80mA/cm2), the current efficiency and energy efficiency of cells with QBPPEK (IEC=1.53mmol/g) and PyBPPEK (IEC=1.50mmol/g) were higher than those of cell with Nafionl17.
Poly(phthalazinonc ether ketone ketone) with dimethyl groups (DMPPEKK) were prepared from polycondcnsation method. Poly(phthalazinone ether ketone ketone) with bromomethylated groups (BPPEKK) was prepared from bromination of DMPPEKK. Quaternized poly(phthalazinone ketone ketone)(QBPPEKK) anion exchange membranes and poly(phthalazinone ketone ketone) with pyridinium groups (PyBPPEKK) anion exchange membranes were prepared from BPPEKK with trimethylamine and pyridine as the amination reagents, respectively. At the same current density (20-80mA/cm2), the current efficiency of cells with QBPPEK (1.51mmol/g) and PyBPPEK (1.45mmol/g) was higher than that of cell with Nafionl17, and the energy efficiencies of cells were comparable.
The relationships of structure-property of anion exchange membranes made from chloromethyl poly(phthalazinone ether ketone) and brominated poly(phthalazinone ether ketone) with dimethyl groups were investigated. The water content and swelling ratio of quaternizated poly(phthalazinone ether ketone) membranes and poly(phthalazinone ether ketone) anion exchange membranes with pyridinium groups were increased with the increasing IEC of membranes. The water content and swelling ratio of membranes with quaternary ammonium groups were higher than those of membranes with pyridinium groups. The voltage efficiency and energy efficiency of cells with poly(phthalazinone ether ketone)s membranes were mainly affected by the ion exchange capacity of membranes.
引文
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