两种引发体系下30%阳离子度PDA制备工艺初步研究
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摘要
本文研究了合成30%阳离子度PDA的聚合工艺。以工业一步法单体二甲基二烯丙基氯化铵(DMDAAC)和工业丙烯酰胺(AM)为原料,过硫酸铵(APS)-亚硫酸氢钠(RH)或过硫酸铵-偶氮二异丁腈(AIBN)为引发剂,采用水溶液聚合方式,对聚合工艺进行了研究。
在已有文献基础上选用未经精制的工业单体,通过对引发剂用量、单体起始总含量、聚合反应温度3个因素的初步优化得到基础工艺,在此工艺基础上加入助剂Na_4EDTA,通过对上述3个因素及Na_4EDTA用量的正交优化,得到了特征黏度为8.65 dL·g~(-1),总残余双键含量为25.65%的产物及其相应的聚合工艺。
探索了APS-AIBN复合引发体系下的聚合工艺。通过APS引发剂用量、Na_4EDTA用量、单体起始总含量和聚合反应温度4个因素的正交优化及熟化温度,AIBN用量,熟化时间3个因素的单因素实验,得到了特征黏度为8.98 dL·g~(-1),总残余双键含量为26.50%的产物及其相应的聚合工艺。
结果表明,通过加入Na_4EDTA,可使反应体系中引发剂用量、单体起始总含量、聚合反应温度在原有基础上上调,有利于在保持产物特征黏度基础上降低总残余双键含量,同时Na_4EDTA的加入也提高了采用APS-RH引发体系制备所得产物性质的稳定性。使用油溶性引发剂AIBN与APS的复合引发体系可以使熟化温度提高,促使二次引发,进而缩短反应所需时间,使产物的特征黏度值在原有APS工艺基础上略为提高。上述研究结果对于30%阳离子度PDA的进一步研究具有一定的参考作用。
The process of preparing the poly dimethyl diallyl ammonium chloride (DMDAAC) -acrylamide(AM) with cationicity of 30% was studied in this paper. Using monomer DMDAAC and AM as raw material, ammonium persulfate(APS)/sodium bisulfate(RH) redox complex or ammonium persulfate /azobisisobutyronitrile(AIBN) complex as initiators respectively, the polymerization was carried out in the aqueous solution.
Based on the present research results of preparing PDA with 30% cationicity, a primary optimization of three factors(initiator concentration, monomer concentration, reaction temperature) was conducted first, while APS/RH was used as initiator, DMDAAC without simply refining was used as raw material. Through a series of orthonormal experiments based on using Na_4EDTA as additive, a products with intrinsic viscosity 8.65 dL·g~(-1), the percent of the residual double bond 25.65% and its preparation condition were obtained.
At the same time, a primary study of preparing PDA with 30% cationicity was made on the basis of using ammonium persulfate/ azobisisobutyronitrile complex as initiator. Through a series of orthonormal experiments in the first stage and the single factor experiments in the second stage, a product with intrinsic viscosity 8.98 dL·g~(-1) and percent of the residual double bond 26.5%, and its preparation condition were obtained.
The result showed that the percent of the residual double bond could be reduced effectively by using Na_4EDTA as additive and the preparation processes stability was increased. The percent of the residual double bond could be reduced and the intrinsic viscosity could be increased also, by using APS-AIBN complex as initiator. The results in this paper would have a guiding function on the preparation of PDA with cationicity of 30% in the future.
在已有文献基础上选用未经精制的工业单体,通过对引发剂用量、单体起始总含量、聚合反应温度3个因素的初步优化得到基础工艺,在此工艺基础上加入助剂Na_4EDTA,通过对上述3个因素及Na_4EDTA用量的正交优化,得到了特征黏度为8.65 dL·g~(-1),总残余双键含量为25.65%的产物及其相应的聚合工艺。
探索了APS-AIBN复合引发体系下的聚合工艺。通过APS引发剂用量、Na_4EDTA用量、单体起始总含量和聚合反应温度4个因素的正交优化及熟化温度,AIBN用量,熟化时间3个因素的单因素实验,得到了特征黏度为8.98 dL·g~(-1),总残余双键含量为26.50%的产物及其相应的聚合工艺。
结果表明,通过加入Na_4EDTA,可使反应体系中引发剂用量、单体起始总含量、聚合反应温度在原有基础上上调,有利于在保持产物特征黏度基础上降低总残余双键含量,同时Na_4EDTA的加入也提高了采用APS-RH引发体系制备所得产物性质的稳定性。使用油溶性引发剂AIBN与APS的复合引发体系可以使熟化温度提高,促使二次引发,进而缩短反应所需时间,使产物的特征黏度值在原有APS工艺基础上略为提高。上述研究结果对于30%阳离子度PDA的进一步研究具有一定的参考作用。
The process of preparing the poly dimethyl diallyl ammonium chloride (DMDAAC) -acrylamide(AM) with cationicity of 30% was studied in this paper. Using monomer DMDAAC and AM as raw material, ammonium persulfate(APS)/sodium bisulfate(RH) redox complex or ammonium persulfate /azobisisobutyronitrile(AIBN) complex as initiators respectively, the polymerization was carried out in the aqueous solution.
Based on the present research results of preparing PDA with 30% cationicity, a primary optimization of three factors(initiator concentration, monomer concentration, reaction temperature) was conducted first, while APS/RH was used as initiator, DMDAAC without simply refining was used as raw material. Through a series of orthonormal experiments based on using Na_4EDTA as additive, a products with intrinsic viscosity 8.65 dL·g~(-1), the percent of the residual double bond 25.65% and its preparation condition were obtained.
At the same time, a primary study of preparing PDA with 30% cationicity was made on the basis of using ammonium persulfate/ azobisisobutyronitrile complex as initiator. Through a series of orthonormal experiments in the first stage and the single factor experiments in the second stage, a product with intrinsic viscosity 8.98 dL·g~(-1) and percent of the residual double bond 26.5%, and its preparation condition were obtained.
The result showed that the percent of the residual double bond could be reduced effectively by using Na_4EDTA as additive and the preparation processes stability was increased. The percent of the residual double bond could be reduced and the intrinsic viscosity could be increased also, by using APS-AIBN complex as initiator. The results in this paper would have a guiding function on the preparation of PDA with cationicity of 30% in the future.
引文
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[18]Dano N;Hisaoka T;Asano Si,etl.Ink-jet printing sheet with undercoat layer and ink receiving layer.JP:2006212885,2006-08-17
[19]Ikeda,O.,Yoshinaga,K,Lei.J.Nitric Oxide Detection with Glassy Carbon Electrodes Coated with Charge-different Polymer Films.Sensors 2005,5,161-170
[20]赵华章,高宝玉,岳钦艳.二甲基二烯丙基氯化铵(DMDAAC)聚合物的研究进展.工业水处理,1999,19(6):1-4
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[28]Wandrey C,Jaegar W,Reinish G.Determination of the relative molecular weight of poly(dimethyldiallyl ammonium chloride)by viscosimetry of solutions.Acta Polym,1982,33(2):156-158
[29]Gartner H A.Production of high molecular weight copolymers of diallylammonium monomers and acrylamide monomers in an aqueous dispersed phase.US:5171 783,1992-12-15
[30]岳钦艳,李勇,高宝玉,等.PDMDAAC-AM共聚物的反相乳液聚合研究.山东大学学报(理学版),2004,39(6):86-89
[31]吴建军,马喜平,郑锟,等.反相乳液聚合合成AM/DMDAAC阳离子共聚物.石油化工,2005,34(2):140-143
[32]冯薇,葛艳蕊,张林雅.高吸水性树脂的合成、性能及应用.2006,23(6):364-366
[33]唐善法.DMDAAC/AM絮凝剂的合成与性能评价.精细石油化工进展.2003,4(2):26-28
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