反相乳液聚合法制备HACC及其絮凝性能

Synthesis of HACC by Inverse Emulsion and Study on its Flocculating Properties

以壳聚糖(CTS)和2,3-环氧丙基三甲基氯化铵(GTA)为原料,用反相乳液聚合法合成了壳聚糖季铵盐(HACC)。并采用FTIR、1HNMR、ESEM和XRD对其结构和形貌进行了表征。考察了反相乳液体系中复合乳化剂的HLB值、V(油)∶V(水)、引发剂用量、时间、温度和m(GTA)∶m(CTS)对反应取代度及产率的影响。结果表明:合成HACC的最佳工艺条件为:复合乳化剂的HLB=6.0、V(油)∶V(水)=1.0∶1、w(引发剂)(占单体质量的百分数)=1.5%,反应时间为5 h,温度为60℃,m(GTA)∶m(CTS)=3.0∶1。在此条件下,产物的取代度和产率均达最大值,分别为1.331和81.16%。用原料CTS、自制HACC和市售絮凝剂阳离子聚丙烯酰胺(CPAM)对高岭土模拟废水进行了絮凝实验。考察了絮凝体系p H、絮凝剂投加量对絮凝效果的影响。结果表明:CPAM、CTS和HACC对高岭土模拟废水都具有絮凝效果,HACC适宜的絮凝p H为6,絮凝剂的最佳投加量为1 mg/L。在此条件下,HACC、CTA、CPAM处理模拟废水的剩余浊度分别为3.98、10.81、25.67 NTU。

Chitosan quaternary ammonium salt （HACC） was synthesized by the reaction of chitosan （CTS） with 2, 3-trimethyl ammonium chloride （GTA） via inverse emulsion polymerization. The structure and morphology of HACC were characterized by Fourier transform infrared spectroscopy （FI＇IR）, nuclear magnetic resonance hydrogen spectroscopy （（1HNMR ）, environmental scanning electron microscope （ESEM） and X-ray diffraction （XRD）. In addition, the effects of compound emulsifier HLB value, volume ratio of oil to water, initiator amount, reaction time, reaction temperature and mass radio of GTA and CTS on degree of substitution （DS） and yield （P） of HACC were investigated. And the optimal conditions were obtained. When the compound emulsifier HLB value is 6. 0,volume ratio of oil to water is 1.0：1 ,initiator amount is 1.5% （based on mass of GTA） ,reaction time is 5 h, reaction temperature is 60 ~C and mass radio of GTA and CTS is 3.0, the degree of substitution and yield of the product reach the maximum,they are 1. 331 and 81.16% ,respectively. Moreover, the flocculating experiment of kaolin suspension as simulated wastewater was employed using CTS,cationic polyacrylamide （CPAM） and HACC as flocculants, the effects of pH of simulated wastewater and flocculant dosage were investigated. The results indicate that CPAM, CTS and HACC have good flocculating properties. The appropriate floeculation parameters of HACC are that theoptimum flocculation pH is 6 and the best flocculant dosage is 1 mg/L. And under these conditions, HACC,CTS and CPAM treated simulated wastewater, the residual turbidity were 3.98,10. 81 and 25.67 NTU. The results indicated that the flocculation effect was HACC 〉 CTS 〉 CPAM.