反相悬浮聚合制备单宁螯合树脂及吸附机理研究
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摘要
本文应用反相悬浮聚合法将黑荆树单宁与多聚甲醛在液体石蜡中发生聚合反应,制备球状单宁螯合树脂。通过试验得出最佳制备条件:颗粒粒径分布集中在20目、搅拌转速为450 r/min、单宁与多聚甲醛的质量比12:1、反应温度67℃、反应时间3.5h、石蜡体积65mL;最佳静态吸附条件为:吸附平衡时间9h,吸附温度为25℃,模拟废水初始浓度取为100mg/L,树脂投加量为0.1g,溶液pH不变;最佳脱附条件为:脱附剂为无水乙醇,脱附温度为45℃,解吸效率可达95%以上,具有较好的可再生性能。
利用FIR、XRD、SEM、热力学、动力学等方法对单宁螯合树脂结构与性能变化进行研究,表明对铬、铜离子的吸附符合Freudlich吸附,为放热过程,而且是自发进行的。对其吸附机理的研究表明,其对高浓度的铬溶液以氢键吸附为主,对低浓度的铬溶液以配位吸附为主,而对铜溶液的吸附基本属于配位吸附。吸附速率由颗粒内扩散和膜扩散联合控速,但以颗粒内扩散为主。
通过单宁与多聚甲醛、水和二乙烯三胺制备单宁胺基螯合树脂为单宁螯合树脂增加功能基团;以重铬酸钾为模拟废水测定其对金属离子的吸附、脱附能力。
Based on reviewing the present researches of chelating resin and the functional polymers of plant tannins,using black wattle tannins and paraform aldehyde in fluid-wax as organic dispersant, a spherical tannin chelating resins was prepared through inverse-suspension polymerization. The condition of reaction was determined by means of orthognonal experiment.The optimal condition of synthesis was: The distributing of particle size 20mm;milling rotate speed 450r/min;m (tannins): m (paraform aldehyde) =12:1; reaction temperature 67℃; reaction time 3.5 h; fluid-wax volume 65 mL;The best static state adsorption condition of tannins chelating resins: the time is 9h, the incipient concentration is 100mg/L, the adsorption temperature is 25℃, the adding quantity of resins is 0.1g, the pH is invariability;The best desorption experimental condition:the desorption agent is ethanol, the desorption temperature is 45℃, the adsorption rate is above 95%.
The experiment studied adsorption effect of tannins chelating resins towards Cr~(6+)、Cu~(2+)and the results indicate that tannins chelating resins has better adsorption effect towards Cu~(2+) than Cr~(6+), which may be contributed to the phenolic hydroxyl group of the adsorbent. In addition, easily desorption of tannins chelating resins was showed in experiments and exhibits excellent reuseability.
The structure of adsorption products was characterized by FIR, XRD, TG, DSC and SEM. The studies on the thermodynamics and the kinetics showed that the adsorption of Cr6+、Cu2+ onto tannins chelating resins is the endothermic sorption process and occurs automatically. Freundlich isotherm is suggested as the propriate type for this procedure. Furthermore, the adsorption propelling force was mainly the coordination-bonding interaction between Cr6+、Cu2+ and the–OH of tannin chelating resins. The studies on the kinetics and reaction activation energy showed that both film diffusion and particle diffusion are the rate-controlling process in the adsorption system tested. But particle diffusion is more predominant.
利用FIR、XRD、SEM、热力学、动力学等方法对单宁螯合树脂结构与性能变化进行研究,表明对铬、铜离子的吸附符合Freudlich吸附,为放热过程,而且是自发进行的。对其吸附机理的研究表明,其对高浓度的铬溶液以氢键吸附为主,对低浓度的铬溶液以配位吸附为主,而对铜溶液的吸附基本属于配位吸附。吸附速率由颗粒内扩散和膜扩散联合控速,但以颗粒内扩散为主。
通过单宁与多聚甲醛、水和二乙烯三胺制备单宁胺基螯合树脂为单宁螯合树脂增加功能基团;以重铬酸钾为模拟废水测定其对金属离子的吸附、脱附能力。
Based on reviewing the present researches of chelating resin and the functional polymers of plant tannins,using black wattle tannins and paraform aldehyde in fluid-wax as organic dispersant, a spherical tannin chelating resins was prepared through inverse-suspension polymerization. The condition of reaction was determined by means of orthognonal experiment.The optimal condition of synthesis was: The distributing of particle size 20mm;milling rotate speed 450r/min;m (tannins): m (paraform aldehyde) =12:1; reaction temperature 67℃; reaction time 3.5 h; fluid-wax volume 65 mL;The best static state adsorption condition of tannins chelating resins: the time is 9h, the incipient concentration is 100mg/L, the adsorption temperature is 25℃, the adding quantity of resins is 0.1g, the pH is invariability;The best desorption experimental condition:the desorption agent is ethanol, the desorption temperature is 45℃, the adsorption rate is above 95%.
The experiment studied adsorption effect of tannins chelating resins towards Cr~(6+)、Cu~(2+)and the results indicate that tannins chelating resins has better adsorption effect towards Cu~(2+) than Cr~(6+), which may be contributed to the phenolic hydroxyl group of the adsorbent. In addition, easily desorption of tannins chelating resins was showed in experiments and exhibits excellent reuseability.
The structure of adsorption products was characterized by FIR, XRD, TG, DSC and SEM. The studies on the thermodynamics and the kinetics showed that the adsorption of Cr6+、Cu2+ onto tannins chelating resins is the endothermic sorption process and occurs automatically. Freundlich isotherm is suggested as the propriate type for this procedure. Furthermore, the adsorption propelling force was mainly the coordination-bonding interaction between Cr6+、Cu2+ and the–OH of tannin chelating resins. The studies on the kinetics and reaction activation energy showed that both film diffusion and particle diffusion are the rate-controlling process in the adsorption system tested. But particle diffusion is more predominant.
引文
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