AM/DAC的反相乳液聚合及絮凝性能评价
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摘要
论文采用反相乳液聚合法,以丙烯酰胺(AM)和丙烯酰氧乙基三甲基氯化铵(DAC)作为单体,Span80-Tween80为复合乳化剂,液体石蜡为连续相制备污泥脱水剂阳离子型聚丙烯酰胺(CPAM)。实验考察了油水体积比、乳化剂用量和配比、单体用量和配比、引发剂种类和用量、温度、聚合时间、通氮气时间和搅拌对聚合物特性黏度和稳定性的影响。研究结果表明:在油水体积比为1:1.6、乳化剂用量为30%(占液体石蜡的质量分数)、乳化剂Span80与Tween80质量比为3:5、单体用量为30%(占水相质量分数)、单体AM与DAC摩尔比为2:3、引发剂用量为0.15%(占单体的质量分数)、聚合温度为40℃,通入普通氮气30min,聚合时间为5h的条件下,得到特性黏度为897 mL·g-1,阳离子度为60%的阳离子聚丙烯酰胺。
对制得的产品进行脱乳和干燥,干燥的优化条件是在真空度为1000Pa,温度为60℃～70℃范围内干燥10h左右,所得产物效果较好。通过红外光谱和差热分析对自制的CPAM进行了结构表征。结果显示:通过红外光谱分析证明自制的CPAM结构与理论产物结构相符,通过差热分析内表明自制CPAM在265.54℃时发生化学分解。
将自制的阳离子聚丙烯酰胺用于重庆市鸡冠石污水处理厂浓缩池的污泥处理,实验研究表明阳离子聚丙烯酰胺用于污泥脱水,其脱水效果与阳离子聚丙烯酰胺的特性黏度、阳离子度、投加量和搅拌速度等因素有关。在阳离子聚丙烯酰胺特性黏度为897 mL·g-1,质量分数为0.05‰,投加量为25mL的情况下进行絮凝实验研究结果表明:污泥的透光率可达96.9%,滤液浊度可达11.2,滤饼含水率可达62.05%。此外,论文还研究了阳离子聚丙烯酰胺的特性黏度、投加量、阳离子度对污泥脱水效果的影响。研究结果表明:就目前实验室制备的阳离子聚丙烯酰胺的情况下,投加量和阳离子度对污泥脱水效果的影响有一个最佳范围,特性黏度越高絮凝性能越好,但是这仅限于目前实验室合成产物的特性黏度。除此之外,温度,搅拌速度等也对污泥脱水有一定的影响。
The cationic polyacrylamide (CPAM) was synthesized by inverse emulsion polymerization using acrylamide (AM) and acryloyloxyethyltrimethyl ammonium chloride (DAC) as monomers, Span80-Tween80 as compound emulsifier, liquid paraffin as continuous phase. The influences factors to the viscosity of product and the stability of the system were discussed, such as the volume ratio of oil to water, the ratio and concentration of Span80 to Tween80, the ratio and concentration of AM to DAC, the type and concentration of initiator, the initial reaction temperature, reaction time, inlet time of N2, whisk speed, the drying and granulation. The optimum conditions of copolymerization were obtained as follows:the volume ratio of oil to water was 1:1.6, the emulsifier dosage was 30%, the mass ratio of Span80 to Tween80 was 3:5, the concentration of monomer was 30%, the mol distribution ratio of AM to DAC was 2:3, initiating temperature was 40℃, inlet time of N2 was 30min and reaction time was 5 hours. The cationic polyacrylamide with viscosity 897 mL·g-1 and cationic degree being about 60% was obtained.
Using acetone and the ethanol to demulsify the product, then dry it. The optimum conditions of deemulsification and drying were obtained as follows: then at the Vacuum Degree of 1000MPa, the drying temperature was 70℃, drying time was 10h. Using the differential thermal analysis and infrared spectroscopy characterize the self-made CPAM. The infrared spectroscopy result shows that self-made CPAM was consentaneous with the theory. The differential thermal analysis result shows that the self-made CPAM was decomposed at 265.54℃.
Use the self-made CPAM to flocculation the sludge in condenses pool of a sewage plant in the city of Chongqing, China. The experiment shows that the performance of self-made CPAM has related with the viscosity of CPAM, the cationic degree, the adding quality of CPAM, the mixing speed, etc. With the viscosity of CPAM was 897 mL·g-1, the dosage was 25mL, cationic degree was 60%, CPAM has the better treatment effects. Under the optimum conditions, the transmittance removal for upper clean liquid was up to 96.9%, filtrate turbidity was decreasing to 11.2, the water content for press cake was decreasing to 62.05%. In addition, the paper also researched the effects of viscosity of CPAM, the dosage and the cationic degree. The result shows that the dosage and the cationic degree have optimum scope. It means sludge dewatering was not better even with excessive cationic degree and dosage. In addition to that, the temperature and mixing speed also have effect to sludge dewatering
对制得的产品进行脱乳和干燥,干燥的优化条件是在真空度为1000Pa,温度为60℃～70℃范围内干燥10h左右,所得产物效果较好。通过红外光谱和差热分析对自制的CPAM进行了结构表征。结果显示:通过红外光谱分析证明自制的CPAM结构与理论产物结构相符,通过差热分析内表明自制CPAM在265.54℃时发生化学分解。
将自制的阳离子聚丙烯酰胺用于重庆市鸡冠石污水处理厂浓缩池的污泥处理,实验研究表明阳离子聚丙烯酰胺用于污泥脱水,其脱水效果与阳离子聚丙烯酰胺的特性黏度、阳离子度、投加量和搅拌速度等因素有关。在阳离子聚丙烯酰胺特性黏度为897 mL·g-1,质量分数为0.05‰,投加量为25mL的情况下进行絮凝实验研究结果表明:污泥的透光率可达96.9%,滤液浊度可达11.2,滤饼含水率可达62.05%。此外,论文还研究了阳离子聚丙烯酰胺的特性黏度、投加量、阳离子度对污泥脱水效果的影响。研究结果表明:就目前实验室制备的阳离子聚丙烯酰胺的情况下,投加量和阳离子度对污泥脱水效果的影响有一个最佳范围,特性黏度越高絮凝性能越好,但是这仅限于目前实验室合成产物的特性黏度。除此之外,温度,搅拌速度等也对污泥脱水有一定的影响。
The cationic polyacrylamide (CPAM) was synthesized by inverse emulsion polymerization using acrylamide (AM) and acryloyloxyethyltrimethyl ammonium chloride (DAC) as monomers, Span80-Tween80 as compound emulsifier, liquid paraffin as continuous phase. The influences factors to the viscosity of product and the stability of the system were discussed, such as the volume ratio of oil to water, the ratio and concentration of Span80 to Tween80, the ratio and concentration of AM to DAC, the type and concentration of initiator, the initial reaction temperature, reaction time, inlet time of N2, whisk speed, the drying and granulation. The optimum conditions of copolymerization were obtained as follows:the volume ratio of oil to water was 1:1.6, the emulsifier dosage was 30%, the mass ratio of Span80 to Tween80 was 3:5, the concentration of monomer was 30%, the mol distribution ratio of AM to DAC was 2:3, initiating temperature was 40℃, inlet time of N2 was 30min and reaction time was 5 hours. The cationic polyacrylamide with viscosity 897 mL·g-1 and cationic degree being about 60% was obtained.
Using acetone and the ethanol to demulsify the product, then dry it. The optimum conditions of deemulsification and drying were obtained as follows: then at the Vacuum Degree of 1000MPa, the drying temperature was 70℃, drying time was 10h. Using the differential thermal analysis and infrared spectroscopy characterize the self-made CPAM. The infrared spectroscopy result shows that self-made CPAM was consentaneous with the theory. The differential thermal analysis result shows that the self-made CPAM was decomposed at 265.54℃.
Use the self-made CPAM to flocculation the sludge in condenses pool of a sewage plant in the city of Chongqing, China. The experiment shows that the performance of self-made CPAM has related with the viscosity of CPAM, the cationic degree, the adding quality of CPAM, the mixing speed, etc. With the viscosity of CPAM was 897 mL·g-1, the dosage was 25mL, cationic degree was 60%, CPAM has the better treatment effects. Under the optimum conditions, the transmittance removal for upper clean liquid was up to 96.9%, filtrate turbidity was decreasing to 11.2, the water content for press cake was decreasing to 62.05%. In addition, the paper also researched the effects of viscosity of CPAM, the dosage and the cationic degree. The result shows that the dosage and the cationic degree have optimum scope. It means sludge dewatering was not better even with excessive cationic degree and dosage. In addition to that, the temperature and mixing speed also have effect to sludge dewatering
引文
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