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腐植酸/淀粉复合微球的制备及工艺优化 被引量:2

Preparation and Process Optimization of Humic Acid/Starch Composite Microspheres
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摘要 以腐植酸(HA)和可溶性淀粉(St)为原料,N,N’-亚甲基双丙烯酰胺(MBAA)为交联剂,过硫酸钾/亚硫酸氢钠(K2S2O8/Na HSO3)为复合引发剂,采用反相乳液聚合法合成了腐植酸/淀粉复合微球(CSM)。结合响应曲面设计,探讨了m(HA)∶m(St)、K2S2O8/Na HSO3用量、MBAA用量、复合乳化剂用量、反应温度等因素对CSM吸附Cr(Ⅵ)性能的影响。结果表明,合成CSM的最佳工艺条件为:m(HA)∶m(St)=1.51∶1.00、MBAA用量40%(以St质量为基准,下同)、K2S2O8/NaHSO3用量40%/40%、复合乳化剂〔m(Span-80):m(Tween-20)=3:1〕用量80%、反应温度50℃、反应时间3 h。在该条件下合成的CSM对Cr(Ⅵ)(10 mg/L)的去除率达到99.91%,吸附量为1.9980 mg/g。利用FTIR、SEM、激光粒度分布仪、XRD和TGA对CSM进行了结构表征和性能测试,结果显示HA和St成功反应,所得CSM形状规则,表面粗糙,粒径分布均匀,平均粒径为13.79μm,结晶度(相较于St)降低,具有较好的热稳定性。 Humic acid/starch composite microspheres(CSM) were prepared by reverse phase emulsion polymerization method using humic acid(HA) and soluble starch(St) as raw materials, N,N’-methylenebisacrylamide(MBAA) as cross-linking agent, potassium persulfate/sodium hydrogen sulfite(K2S2O8/Na HSO3) as initiator. Response surface methodology was used to investigated the effects of m(HA)∶m(St), K2S2O8/NaHSO3 dosage, MBAA dosage, composite emulsifier dosage and temperature on the adsorption properties of CSM. The results showed that the optimum conditions for the synthesis of CSM were obtained as follows: mass ratio of HA to St 1.51∶1.00, MBAA dosage 40%(based on the mass of St, the same below), K2S2O8/Na HSO3 dosage 40%/40%, composite emulsifier〔m(Span-80): m(Tween-20)=3:1〕dosage 80%, reaction temperature 50 ℃, and reaction time was 3 h. Under the above-mentioned conditions, the removal rate of CSM for Cr(Ⅵ)(10 mg/L) reached 99.91%, the adsorption capacity was 1.9980 mg/g. The CSM was characterized by FTIR, SEM, laser particle size distribution analyzer, XRD and TGA. It was found that HA and St reacted successfully, the CSM was regular in shape and rough in surface with a uniform particle size distribution. The average particle size was 13.79 μm. The crystallinity of CSM decreased compared with that of St. In addition, the CSM had good thermal stability.
作者 苏秀霞 胡金龙 张婧 晏春苗 徐佳 SU Xiu-xia;HU Jin-long;ZHANG Jing;YAN Chun-miao;XU Jia(Key Laboratory of Auxiliary Chemistry and Technology for Chemical Industry,Ministry of Education,Shaanxi University of Science&Technology,Xi'an 710021,Shaanxi,China;Xianyang Vocational Technical College,Xianyang 712000,Shaanxi,China)
出处 《精细化工》 EI CAS CSCD 北大核心 2019年第12期2385-2392,2430,共9页 Fine Chemicals
基金 陕西省科技厅科技计划项目(2014K10-20) 咸阳市科技计划项目(2018K02-49)
关键词 腐植酸 复合微球 反相乳液聚合 优化 吸附性能 功能材料 humic acid composite microspheres inverse emulsion polymeriztion optimization adsorption properties functional materials
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