Determination of Pore Size Distribution of Nafion/Sulfated β-Cyclodextrin Composite Membranes as Studied by 1H Solid-State NMR Cryoporometry

Jae-Deok Jeon, B. Lee, S. Kwak
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Abstract

Nafion/sb-CD membranes were prepared by mixing 5 wt% Nafion solution with H-form sulfated β-cyclodextrin (sb-CD), and their water uptake, ion exchange capacity (IEC), and ionic cluster size distribution were measured. The water uptake and IEC of the membrane increased with an increase in the sb-CD content. The SAXS experiments confirmed that an increase in the sb-CD content of the membranes shifted the maximum SAXS peaks to lower angles, indicating an increase in the cluster correlation peak. NMR cryoporometry is based on the theory of the melting point depression of a liquid confined within a pore, which is dependent on the pore diameter. The intensity-temperature (IT) curves showed that the cluster size distribution gradually became broader with an increase in the sb-CD content due to the increased water content, indicating an increase in the ionic cluster size. This result indicates that the presence of sb-CD results in increases in the cluster size as well as in the water uptake and the IEC.
1H固体核磁共振冻孔法测定钠离子/硫酸化β-环糊精复合膜的孔径分布
采用5 wt%的Nafion溶液与h型硫酸化β-环糊精(sb-CD)混合制备了Nafion/sb-CD膜,并测定了其吸水性、离子交换容量(IEC)和离子簇大小分布。膜的吸水性和IEC随硒镉含量的增加而增加。SAXS实验证实,随着膜中sb-CD含量的增加,SAXS最大峰向低角度移动,表明簇相关峰增加。核磁共振冻孔法是基于液体在孔内的熔点下降理论,而熔点下降取决于孔的直径。强度-温度(IT)曲线显示,随着水含量的增加,离子簇尺寸分布逐渐变宽,表明离子簇尺寸增大。这一结果表明,sb-CD的存在导致簇大小的增加以及水的吸收和IEC。
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