Page 64 - 精细化工2019年第12期

·2392· 精细化工 FINE CHEMICALS
2.8 粒径分析
最佳工艺下合成的 CSM 粒径及其分布如图 11
所示。
图 11 CSM 的粒径及其分布曲线
Fig. 11 Particle size and particle size distribution of CSM
由图 11 可知，CSM 粒径分布中只显示一个峰，
质量距体积平均粒径〔D (4,3) 〕为 13.98 μm，平均粒
径（D 50 ，即中位径）为 13.79 μm，累积分布为 98%
时的最大颗粒的等效直径（D 98 ）为 31.11 μm，跨度
是 1.58，粒径分布均匀集中，服从正态分布。此外，
还发现通过粒度仪测定出的微球粒径与 SEM 图中
微球粒径大小不一致，这可能是由于 CSM 是一种不
溶水、不溶油的物质，在分散介质中不能均匀分散，
仍有微球粘连，导致测出的微球粒径偏大。
3 结论
（1）以 HA 和 St 为原料，K 2 S 2 O 8 /NaHSO 3 为复
合引发剂，MBAA 为交联剂合成了腐植酸/淀粉复合
微球，通过单因素和响应曲面设计得到最佳工艺：
以质量为 1.5 g 的 St 为基准，取 HA 2.265 g、K 2 S 2 O 8 /
NaHSO 3 0.6 g/0.6 g、MBAA 0.6 g、复合乳化剂 1.2 g、
液体石蜡 90 mL，反应温度为 50 ℃、反应时间 3 h。
（2）通过 FTIR、SEM、XRD、TGA 和激光粒
度分布仪对 CSM 的结构、形貌和性能进行了表征和
测定，发现最佳工艺条件下合成的 CSM 形状规则，
表面粗糙，粒径分布均匀，平均粒径为 13.79 μm，
其热稳定性良好，结晶度相对 St 降低；在 CSM 用
量为 5 g/L、pH=1、温度 25 ℃，振荡 3 h 条件下，
对水中 Cr(Ⅵ)(10 mg/L)去除率可达到 99.91%，吸附
量为 1.9980 mg/g。相较于 HA〔当 HA 用量 5 g/L、
pH=1、温度 25 ℃、振荡 3 h 时，对 Cr(Ⅵ)(10 mg/L)
去除率为 94.99%〕和累托石/腐植酸微球
球用量 20 g/L、pH=1、温度 30 ℃、振荡 2.5 h 时，
对 Cr(Ⅵ)(10 mg/L)去除率为 98.39%〕有显著提高，
表明 CSM 是一种性能优良的重金属离子吸附剂。
第 36 卷
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