AM-DMC共聚物的合成与表征
发布时间：2018-10-16 09:59
【摘要】：水污染是人类21世纪面临的重大问题之一,废水治理是解决水污染及水资源短缺的有效途径,研究开发高效、多功能阳离子絮凝剂对处理高浊废水具有重要的理论意义和应用价值。双水相聚合法具有过程温和、可控条件多、易于操作和放大生产,在分离提纯以及机理解释中可借助传统溶剂萃取理论和经验等特点。阳离子型聚丙烯酰胺系列是目前我国水处理剂中用量最大的试剂之一,丙烯酰胺(AM)-甲基丙烯酰氧乙基三甲基氯化铵(DMC)共聚物(P(AM-DMC))便是阳离子型聚丙烯酰胺中的一种,具有电荷度可控,电荷分布均匀,水处理中用量小,絮凝澄清速度快,产生污泥量少,处理效率高,使用后易被环境中微生物所降解等特点,被广泛应用于各种工业和生活废水的处理。本文通过大量的文献阅读,在国内外已有研究的基础上,以丙烯酰胺、甲基丙烯酰氧乙基三甲基氯化铵为共聚单体,过硫酸铵-亚硫酸氢钠氧化还原体系为自由基引发剂,双水相共聚法制备P(AM-DMC)阳离子聚丙烯酰胺絮凝剂。研究共聚反应工艺条件的优化,双水相共聚相关理论,对共聚反应及共聚产物的结构与性能进行表征,并将所得共聚产物用于模拟废水的治理,获得了有意义的结论。(1)采用单因素试验探索聚合反应条件,并考察单体总量、引发剂用量、单体配比、pH值、反应时间、PEG用量等因素对共聚反应产物粘均分子量和阳离子度的影响。设计4因素3水平正交实验,探究制备较高粘均分子量和较大阳离子度的阳离子聚丙烯酰胺的最佳工艺条件。(2)研究了AM-DMC二元共聚反应的共聚物组成与单体组成之间的关系(二元共聚物微分方程),按照K-T法、F-R法、FBR法计算出单体AM和DMC在共聚反应过程中的竞聚率,研究共聚过程的聚合类型以及利用单体竞聚率绘制单体组成与共聚物组成F-f图。(3)探究绘制了双水相聚合体系液/液边界图,研究双水相体系分相时两高聚物质量分数关系,绘制分相图,同时对AM-DMC共聚反应动力学进行了研究,得出聚合反应动力学曲线。(4)将最终合成产物在模拟和实际污水处理中进行实际应用,研究最终合成产物的性能及相关特性指标。从单因素实验可知,共聚产物阳离子度与粘均分子量有如下结论:随着pH值增大先增后下降,pH控制在6.0左右最为合适;随着单体总量的增加均为增加;其中阳离子度随单体总量变化影响不大。随着反应时间增加均为增加趋势。但反应时间在165min时,反应接近停止,反应时间不要超过180min为宜。随着引发剂用量大于2.5ml时,两个指标都有明显的下降趋势;随着PEG含量的增加,聚合物的粘均分子量先增加后减小,在8%存在峰值。而阳离子度先减小后增加。由正交试验可知:在总单体质量分数为4%,质量比m(AM):m(DMC)=3:1,pH=9,引发剂用量为1.5mL,反应温度为35℃的最优条件下,合成的P(AM-DMC)的粘均分子量最大可达1.6*106,在总单体质量分数为8%,AM与DMC配比m(AM):m(DMC)=3:1,pH=5,引发剂用量为2.5mL,反应温度为35℃的最优条件下,合成的P(AM-DMC)的阳离子度最大可达13.8%。在最佳工艺条件下,所得的P(AM-DMC)也具有良好的絮凝效果。模拟高岭土悬浊液、PVSK悬浊液和AgI悬浊液三种废水的去浊实验,浊度去浊率均能达到70%以上。通过竞聚率设计实验测得DMC的竞聚率r1=2.041,AM的竞聚率r2=0.315。并且绘制出共聚反应F-f曲线图、共聚反应动力学曲线图以及PCAM-PEG双水相相图。
[Abstract]:Water pollution is one of the major problems facing mankind in the 21st century. Wastewater treatment is an effective way to solve water pollution and shortage of water resources. The double-water phase-gathering method has the characteristics of mild process, multiple controllable conditions, easy operation and amplification production, and can be used in separation and purification as well as mechanism interpretation with the aid of traditional solvent extraction theory and experience. The cationic polylactide series is one of the most used reagents in the water treatment agent in China, and the poly (AM)-methylpropenoate (DMC) copolymer (P (AM-DMC)) is one of the cationic polyacetal resins, and has the advantages of controllable charge degree, uniform charge distribution, in that wat treatment, the dosage is small, the flocculation clarification speed is high, the sludge amount is low, the treatment efficiency is high, the microorganism in the environment is easy to degrade after use and the like, and is widely applied to the treatment of various industrial and domestic wastewater. In this paper, a lot of literature reading, based on the existing research at home and abroad, is taken as the free radical initiator through the oxidation reduction system of poly (ethylene glycol)-sodium bisulfite as comonomer, methyl propylene and ethyl trimethylamine as comonomer. P (AM-DMC) cationic polyacrylate flocculant was prepared by double-aqueous phase copolymerization. The structure and properties of copolymerization reaction and copolymerization product were characterized by the optimization of the process conditions of copolymerization reaction and the theory of double water phase copolymerization, and the obtained copolymer was used to simulate the treatment of wastewater. (1) Single factor test was used to explore the polymerization conditions, and the effects of monomer total amount, initiator dosage, monomer ratio, pH value, reaction time, PEG dosage and other factors on the viscosity average molecular weight and cationic degree of the copolymerization product were investigated. The optimum technological conditions for preparing cationic polylactide with higher viscosity average molecular weight and higher cationic degree were studied by designing 4 factors 3 level orthogonal experiment. (2) The relationship between copolymer composition and monomer composition of AM-DMC binary copolymerization is studied (binary copolymer differential equation), and the reactivity of monomer AM and DMC in copolymerization reaction is calculated according to K-T method, F-R method and FBR method. The polymerization type of the copolymerization process and the monomer composition and the copolymer composition F-f were studied by using the monomer reactivity ratio. (3) The liquid/ liquid boundary map of the double-aqueous phase polymerization system was studied, the relationship between the mass fraction of the two polymers was studied, the phase diagram was drawn, and the kinetics of the copolymerization of AM-DMC was studied, and the kinetics curve of polymerization was obtained. (4) carrying out practical application on the final synthesis product in the simulation and the actual sewage treatment to study the performance and the related characteristic indexes of the final synthesis product. It can be seen from the single factor experiment that the cationic degree and the viscosity average molecular weight of the copolymer are as follows: with the increase of the pH value, the pH control is most appropriate at about 6.0; with the increase of the total amount of monomer, the cationic degree is not much influenced by the total amount of monomer. As the reaction time increased, the trend was increased. but when the reaction time is 165min, the reaction is close to stop, and the reaction time is not more than 180min. With the increase of PEG content, the viscosity average molecular weight of polymer decreased first, and peak value was found in 8%. and the cationic degree is increased first. The average molecular weight of the synthesized P (AM-DMC) was 1. 6 * 106, the mass fraction of the total monomer was 8%, and the ratio of AM to DMC (AM): m (DMC) = 3: 1. The cationic degree of the synthesized P (AM-DMC) can reach 13. 8% under the optimal conditions of pH = 5, initiator dosage of 2.5mL and reaction temperature of 35 鈩，
本文编号：2274000
[Abstract]:Water pollution is one of the major problems facing mankind in the 21st century. Wastewater treatment is an effective way to solve water pollution and shortage of water resources. The double-water phase-gathering method has the characteristics of mild process, multiple controllable conditions, easy operation and amplification production, and can be used in separation and purification as well as mechanism interpretation with the aid of traditional solvent extraction theory and experience. The cationic polylactide series is one of the most used reagents in the water treatment agent in China, and the poly (AM)-methylpropenoate (DMC) copolymer (P (AM-DMC)) is one of the cationic polyacetal resins, and has the advantages of controllable charge degree, uniform charge distribution, in that wat treatment, the dosage is small, the flocculation clarification speed is high, the sludge amount is low, the treatment efficiency is high, the microorganism in the environment is easy to degrade after use and the like, and is widely applied to the treatment of various industrial and domestic wastewater. In this paper, a lot of literature reading, based on the existing research at home and abroad, is taken as the free radical initiator through the oxidation reduction system of poly (ethylene glycol)-sodium bisulfite as comonomer, methyl propylene and ethyl trimethylamine as comonomer. P (AM-DMC) cationic polyacrylate flocculant was prepared by double-aqueous phase copolymerization. The structure and properties of copolymerization reaction and copolymerization product were characterized by the optimization of the process conditions of copolymerization reaction and the theory of double water phase copolymerization, and the obtained copolymer was used to simulate the treatment of wastewater. (1) Single factor test was used to explore the polymerization conditions, and the effects of monomer total amount, initiator dosage, monomer ratio, pH value, reaction time, PEG dosage and other factors on the viscosity average molecular weight and cationic degree of the copolymerization product were investigated. The optimum technological conditions for preparing cationic polylactide with higher viscosity average molecular weight and higher cationic degree were studied by designing 4 factors 3 level orthogonal experiment. (2) The relationship between copolymer composition and monomer composition of AM-DMC binary copolymerization is studied (binary copolymer differential equation), and the reactivity of monomer AM and DMC in copolymerization reaction is calculated according to K-T method, F-R method and FBR method. The polymerization type of the copolymerization process and the monomer composition and the copolymer composition F-f were studied by using the monomer reactivity ratio. (3) The liquid/ liquid boundary map of the double-aqueous phase polymerization system was studied, the relationship between the mass fraction of the two polymers was studied, the phase diagram was drawn, and the kinetics of the copolymerization of AM-DMC was studied, and the kinetics curve of polymerization was obtained. (4) carrying out practical application on the final synthesis product in the simulation and the actual sewage treatment to study the performance and the related characteristic indexes of the final synthesis product. It can be seen from the single factor experiment that the cationic degree and the viscosity average molecular weight of the copolymer are as follows: with the increase of the pH value, the pH control is most appropriate at about 6.0; with the increase of the total amount of monomer, the cationic degree is not much influenced by the total amount of monomer. As the reaction time increased, the trend was increased. but when the reaction time is 165min, the reaction is close to stop, and the reaction time is not more than 180min. With the increase of PEG content, the viscosity average molecular weight of polymer decreased first, and peak value was found in 8%. and the cationic degree is increased first. The average molecular weight of the synthesized P (AM-DMC) was 1. 6 * 106, the mass fraction of the total monomer was 8%, and the ratio of AM to DMC (AM): m (DMC) = 3: 1. The cationic degree of the synthesized P (AM-DMC) can reach 13. 8% under the optimal conditions of pH = 5, initiator dosage of 2.5mL and reaction temperature of 35 鈩，
本文编号：2274000
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