速溶型阳离子聚丙烯酰胺制备工艺研究
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摘要
本文以丙烯酰胺(AM)、甲基丙烯酰氧乙基三甲基氯化铵(DMC)、丙烯酰氧乙基三甲基氯化铵(DAC)三种单体为原料,采用水溶液光辅助引发聚合法合成了P(DMC-AM)和P(DAC-AM)两种不同的阳离子聚丙烯酰胺,并对其絮凝性能进行了评价。另外,对DMC的均聚反应进行了初步研究。采用FT-IR技术对所得三种产物的结构进行了表征。
考察了不同引发方式对聚合反应的影响,研究了原料、单体浓度、引发温度、总引发剂浓度、溶液pH值、阳离子度、氧化还原引发体系、引发剂的配比、氧化还原剂用量、偶氮类引发剂用量、助溶剂用量、络合剂用量和稳定剂用量等因素对产物特性粘数和溶解性的影响。结果表明:加入络合剂及稳定剂并不能显著提高产物的特性粘数,但是稳定剂的加入可以提高聚合物的稳定性;随着助溶剂用量的增大,产物的特性粘数先增大后减小,而产物的溶解时间明显减少。在絮凝性能实验中,主要研究了絮凝剂特性粘数、用量及阳离子度等因素对其絮凝性能的影响。所得到的P(DMC-AM)的较佳合成工艺条件为:单体浓度30%,阳离子度为30%,氧化还原引发剂用量为0.0020%,氧化剂和还原剂的质量比为1:1,偶氮类引发剂用量为0.0030%,引发温度10℃,pH值为4.0,络合剂用量为0.0030%,助溶剂用量为0.4%,稳定剂用量为0.0040%,干燥温度60℃,干燥时间2h。在上述条件下,所得产物的特性粘数为11.81 dL·g-1,溶解时间45min。得到较佳的絮凝条件是:污泥pH值6.0,P(DMC-AM)特性粘数10.34dL·g-1,阳离子度30%,用量0.06%,离心速度在1200rpm,搅拌时间12min,在此条件下,所得上层清液的透光率达99.3%,絮凝率达77.8%,污泥的脱水率达到80.0%以上。
所得到的P(DAC-AM)的较佳合成工艺是:单体浓度40%,阳离子度50%,氧化还原引发剂用量0.0020%,偶氮类引发剂用量0.0020%,络合剂用量0.0030%,助溶剂用量1.5%,稳定剂用量0.0040%,pH=4,引发温度15℃,干燥温度60℃,干燥时间5h,在上述条件下,所得产物的特性粘数为16.40dL·g-1,溶解时间42min。得到较佳的絮凝试验条件为:P(DAC-AM)的阳离子度30%,特性粘数15.29 dL·g-1,用量0.06%,在此条件下,污水的透光率达99.9%、絮凝率达77.9%、脱水率达到81.4%以上。
PDMC的较佳合成工艺条件是:引发剂体系采用硫酸亚铁和过硫酸铵,引发剂用量0.0020%,氧化剂和还原剂的质量比为1:1,单体浓度75%,pH=4,引发温度10℃,络合剂用量0.0030%。在上述条件下,所得产物的特性粘数为8.4 dL·g-1以上,溶解时间在11min左右。
采用水溶液聚合法和光辅助引发技术,对上述聚合体系进行系统研究,目前未见文献报道。
Two different kinds of cationic polyacrylamide were prepared using acrylamide(AM),2-methylacryloyloxyethyltrimethyl ammonium chloride (DMC) and acryloyloxyethyltrimethyl ammonium chloride(DAC) as monomers in aqueous solution by assistance of photo-initiation. Their flocculating performances to wastewater were investigated. The polymerization of DMC was also studied.The structure of obtained products were characterized by FT-IR,
The influences of factors, such as way of initiation, raw materials, monomer concentration, initiation temperature, pH, cationic degree, oxidant–reductant initiator system , mass ratio of oxidizer to reductant, oxidant–reductant concentration, azo-compound concentration, solubilizing agent concentration, chelator concentration and stabilizer concentration, on the intrinsic viscosity and solubility of product were studied. The results showed that with increasing of chelator concentration and stabilizer concentration, there was no obvious improvement on the intrinsic viscosity of product, but the stability of product was improved due to using stabilizer; with increasing of solubilizing agent concentration, the intrinsic viscosity of product increased at first and then decreased, however the dissolving time of product decreaseed gradually. In flocculanting experiment, the effects of intrinsic viscosity, dosage of cationic flocculant and cationic degree on its flocculating performance were investigated.
The obtained optimum conditions for synthesis of P(DMC-AM) were monomer concentration 30%, cationic degree 30%,oxidant–reductant concentration 0.0020%, mass ratio of oxidizer to reductant 1.0:1.0, azo-compound concentration 0.0030%, initiation temperature 10℃, pH=4.0, chelator concentration 0.0030% , the concentration of solubilizing agent 0.4%, stabilizer concentration 0.0040%, drying temperature 60℃and drying time 2h. Under above conditions, the intrinsic viscosity of P(DMC-AM) was 11.81 dL·g-1 ,and the dissolving time was 45min.The obtained optimum flocculating conditions were pH of wastewater 6.0, the intrinsic viscosity of cationic polyacrylamide 10.34dL·g-1, cationic degree 30%, dosage of cationic polyacrylamide 0.06%, velocity of centrifuge 1200 rpm, stirring time 12min. Under above conditions, the transmittance of treated wastewater was 99.3%,the flocculating rate was 77.8% and dewatering rate was 80.0%.
The obtained optimum conditions for synthesis of P(DAC-AM) were monomer concentration 40%, cationic degree 50%, oxidant–reductant concentration 0.0020%, azo-compound concentration 0.0020%, chelator concentration 0.030% , concentration of solubilizing agent 1.5% and stabilizer concentration 0.0040%,initiation temperature 15℃, pH=4.0,drying temperature 60℃and drying time 5h. Under above conditions, the intrinsic viscosity of P(DAC-AM) was 16.40dL·g-1 , and the dissolving time was 42min. The obtained optimum flocculating conditions were pH of wastewater 6.0, the intrinsic viscosity of cationic polyacrylamide 15.29 dL·g-1, cationic degree 30%, dosage of cationic polyacrylamide 0.06%. Under above conditions, the transmittance of treated wastewater was 99.9%,the flocculating rate was 77.9% and dewatering rate was 81.4%.
The obtained optimum reaction conditions for synthesis of PDMC were initiater FeSO_4/(NH_3)2S_2O_4, initiater concentration 0.0020%, the mass ratio of oxidizer to reductant 1.0:1.0, monomer concentration 75%, pH=4, initiation temperature 10℃, chelator concentration 0.0030%. Under above conditions, the intrinsic viscosity of P(DMC) was 8.4 dL·g-1 , and the dissolving time was about 11min.
To our knowledge, there is no report in literature about the polymerization of above systems in aqueous solution by assistance of photo-initiation.
考察了不同引发方式对聚合反应的影响,研究了原料、单体浓度、引发温度、总引发剂浓度、溶液pH值、阳离子度、氧化还原引发体系、引发剂的配比、氧化还原剂用量、偶氮类引发剂用量、助溶剂用量、络合剂用量和稳定剂用量等因素对产物特性粘数和溶解性的影响。结果表明:加入络合剂及稳定剂并不能显著提高产物的特性粘数,但是稳定剂的加入可以提高聚合物的稳定性;随着助溶剂用量的增大,产物的特性粘数先增大后减小,而产物的溶解时间明显减少。在絮凝性能实验中,主要研究了絮凝剂特性粘数、用量及阳离子度等因素对其絮凝性能的影响。所得到的P(DMC-AM)的较佳合成工艺条件为:单体浓度30%,阳离子度为30%,氧化还原引发剂用量为0.0020%,氧化剂和还原剂的质量比为1:1,偶氮类引发剂用量为0.0030%,引发温度10℃,pH值为4.0,络合剂用量为0.0030%,助溶剂用量为0.4%,稳定剂用量为0.0040%,干燥温度60℃,干燥时间2h。在上述条件下,所得产物的特性粘数为11.81 dL·g-1,溶解时间45min。得到较佳的絮凝条件是:污泥pH值6.0,P(DMC-AM)特性粘数10.34dL·g-1,阳离子度30%,用量0.06%,离心速度在1200rpm,搅拌时间12min,在此条件下,所得上层清液的透光率达99.3%,絮凝率达77.8%,污泥的脱水率达到80.0%以上。
所得到的P(DAC-AM)的较佳合成工艺是:单体浓度40%,阳离子度50%,氧化还原引发剂用量0.0020%,偶氮类引发剂用量0.0020%,络合剂用量0.0030%,助溶剂用量1.5%,稳定剂用量0.0040%,pH=4,引发温度15℃,干燥温度60℃,干燥时间5h,在上述条件下,所得产物的特性粘数为16.40dL·g-1,溶解时间42min。得到较佳的絮凝试验条件为:P(DAC-AM)的阳离子度30%,特性粘数15.29 dL·g-1,用量0.06%,在此条件下,污水的透光率达99.9%、絮凝率达77.9%、脱水率达到81.4%以上。
PDMC的较佳合成工艺条件是:引发剂体系采用硫酸亚铁和过硫酸铵,引发剂用量0.0020%,氧化剂和还原剂的质量比为1:1,单体浓度75%,pH=4,引发温度10℃,络合剂用量0.0030%。在上述条件下,所得产物的特性粘数为8.4 dL·g-1以上,溶解时间在11min左右。
采用水溶液聚合法和光辅助引发技术,对上述聚合体系进行系统研究,目前未见文献报道。
Two different kinds of cationic polyacrylamide were prepared using acrylamide(AM),2-methylacryloyloxyethyltrimethyl ammonium chloride (DMC) and acryloyloxyethyltrimethyl ammonium chloride(DAC) as monomers in aqueous solution by assistance of photo-initiation. Their flocculating performances to wastewater were investigated. The polymerization of DMC was also studied.The structure of obtained products were characterized by FT-IR,
The influences of factors, such as way of initiation, raw materials, monomer concentration, initiation temperature, pH, cationic degree, oxidant–reductant initiator system , mass ratio of oxidizer to reductant, oxidant–reductant concentration, azo-compound concentration, solubilizing agent concentration, chelator concentration and stabilizer concentration, on the intrinsic viscosity and solubility of product were studied. The results showed that with increasing of chelator concentration and stabilizer concentration, there was no obvious improvement on the intrinsic viscosity of product, but the stability of product was improved due to using stabilizer; with increasing of solubilizing agent concentration, the intrinsic viscosity of product increased at first and then decreased, however the dissolving time of product decreaseed gradually. In flocculanting experiment, the effects of intrinsic viscosity, dosage of cationic flocculant and cationic degree on its flocculating performance were investigated.
The obtained optimum conditions for synthesis of P(DMC-AM) were monomer concentration 30%, cationic degree 30%,oxidant–reductant concentration 0.0020%, mass ratio of oxidizer to reductant 1.0:1.0, azo-compound concentration 0.0030%, initiation temperature 10℃, pH=4.0, chelator concentration 0.0030% , the concentration of solubilizing agent 0.4%, stabilizer concentration 0.0040%, drying temperature 60℃and drying time 2h. Under above conditions, the intrinsic viscosity of P(DMC-AM) was 11.81 dL·g-1 ,and the dissolving time was 45min.The obtained optimum flocculating conditions were pH of wastewater 6.0, the intrinsic viscosity of cationic polyacrylamide 10.34dL·g-1, cationic degree 30%, dosage of cationic polyacrylamide 0.06%, velocity of centrifuge 1200 rpm, stirring time 12min. Under above conditions, the transmittance of treated wastewater was 99.3%,the flocculating rate was 77.8% and dewatering rate was 80.0%.
The obtained optimum conditions for synthesis of P(DAC-AM) were monomer concentration 40%, cationic degree 50%, oxidant–reductant concentration 0.0020%, azo-compound concentration 0.0020%, chelator concentration 0.030% , concentration of solubilizing agent 1.5% and stabilizer concentration 0.0040%,initiation temperature 15℃, pH=4.0,drying temperature 60℃and drying time 5h. Under above conditions, the intrinsic viscosity of P(DAC-AM) was 16.40dL·g-1 , and the dissolving time was 42min. The obtained optimum flocculating conditions were pH of wastewater 6.0, the intrinsic viscosity of cationic polyacrylamide 15.29 dL·g-1, cationic degree 30%, dosage of cationic polyacrylamide 0.06%. Under above conditions, the transmittance of treated wastewater was 99.9%,the flocculating rate was 77.9% and dewatering rate was 81.4%.
The obtained optimum reaction conditions for synthesis of PDMC were initiater FeSO_4/(NH_3)2S_2O_4, initiater concentration 0.0020%, the mass ratio of oxidizer to reductant 1.0:1.0, monomer concentration 75%, pH=4, initiation temperature 10℃, chelator concentration 0.0030%. Under above conditions, the intrinsic viscosity of P(DMC) was 8.4 dL·g-1 , and the dissolving time was about 11min.
To our knowledge, there is no report in literature about the polymerization of above systems in aqueous solution by assistance of photo-initiation.
引文
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