单电子转移活性自由基聚合法制备丙烯酰胺类聚合物
发布时间：2018-10-26 21:17
【摘要】： 本实验以一种新的聚合方法—单电子转移活性自由基聚合法(SET-LRP)来聚合丙烯酰胺(AM)单体,在水溶液中合成了AM的均聚物和共聚物,在离子液体中合成了AM的均聚物,并且考察了各实验因素对聚合的影响,具体内容如下: 1.以金属铜和三(2-氨甲基乙基)胺(Me6-TREN)为催化剂,2-氯丙酰胺为引发剂,采用SET-LRP方法在水溶液中成功合成了AM的均聚物。通过改变反应时间、单体浓度、反应温度、引发剂和配体的用量等实验条件,考察了不同反应条件对聚合物分子量的影响。在单因素实验基础上,根据Central Composite Design(CCD)实验设计原理,采用三因素三水平的响应面法(RSM)对聚合反应的最佳工艺条件进行了初步探索,得出的最佳工艺条件是:引发剂用量为1.0mmol,单体质量分数为26%,反应时间为40min。 2.介绍了配体Me6-TREN和五甲基二乙三胺的合成方法,并分别与催化剂Cu(0)作为催化体系,采用SET-LRP方法在水溶液中成功合成了AM的均聚物。通过考察配体种类、配体用量和反应时间对聚合反应的影响,结果表明Me6-TREN为更适宜配体。 3.以Cu(0)和Me6-TREN为催化剂,2-氯丙酰胺为引发剂,采用SET-LRP方法在水溶液中分别合成了AM与甲基丙烯酸二甲氨基乙酯(DM)、AM与甲基丙烯酰氧乙基三甲基氯化铵(DMC)的共聚物。考察了共聚反应的实验条件,即反应温度、反应时间、聚合单体的用量及两种单体物质的量之比对共聚物的转化率和分子量大小的影响,对反应的工艺条件进行了探索。 4.以离子液体为溶剂,Cu(0)和Me6-TREN为催化剂,2-氯丙酰胺为引发剂,用SET-LRP方法合成了AM的均聚物。通过改变反应时间、单体浓度、引发剂和催化剂的用量等,考察了不同反应条件对聚合物分子量的影响。 5.在水溶液中采用SET-LRP方法,以Me6-TREN为配体合成的AM均聚物为研究对象,考察其水溶液浓度、温度、剪切速率、NaCl和CaCl2用量对聚合物水溶液表观粘度的影响。结果表明采用SET-LRP方法合成的聚丙烯酰胺在水溶液中具有较高的粘度。
[Abstract]:In this experiment, a new polymerization method, single electron transfer active radical polymerization (SET-LRP), was used to polymerize acrylamide (AM) monomer. Homopolymer and copolymer of AM were synthesized in aqueous solution and homopolymer of AM were synthesized in ionic liquid. The effects of various experimental factors on polymerization are also investigated. The specific contents are as follows: 1. The homopolymer of AM was successfully synthesized in aqueous solution with copper metal and tris (2-aminomethyethyl) amine (Me6-TREN) as catalyst and 2-chloropropanamide as initiator by SET-LRP method. The effects of different reaction conditions on the molecular weight of the polymer were investigated by changing the reaction time, monomer concentration, reaction temperature and the amount of initiator and ligand. On the basis of single factor experiment, according to the principle of Central Composite Design (CCD) experimental design, the optimum process conditions of polymerization were preliminarily explored by using three factors and three levels of response surface method (RSM). The optimum technological conditions are as follows: the amount of initiator is 1.0 mmol, the mass fraction of monomer is 26, and the reaction time is 40 min. 2. The synthesis methods of ligand Me6-TREN and pentamethylenetriamine were introduced. The homopolymer of AM was successfully synthesized by SET-LRP method with the catalyst Cu (0) as the catalytic system. The effects of ligand type, amount of ligand and reaction time on polymerization were investigated. The results showed that Me6-TREN was a more suitable ligand. 3. Using Cu (0) and Me6-TREN as catalysts and 2-chloropropionamide as initiator, AM and dimethylaminoethyl methacrylate (DM), were synthesized in aqueous solution by SET-LRP method, respectively. Copolymer of AM with methacryloxy ethyl trimethylammonium chloride (DMC). The experimental conditions of copolymerization, such as reaction temperature, reaction time, amount of polymeric monomer and the ratio of the two monomers to the amount of the copolymers, were investigated, and the reaction conditions were explored. 4. The homopolymer of AM was synthesized by SET-LRP method using ionic liquid as solvent, Cu (_ 0) and Me6-TREN as catalyst and 2-chloropropanamide as initiator. The effects of different reaction conditions on the molecular weight of the polymer were investigated by changing the reaction time, monomer concentration, initiator and the amount of catalyst. 5. The effects of aqueous solution concentration, temperature, shear rate, NaCl and CaCl2 content on the apparent viscosity of aqueous solution of AM homopolymer synthesized with Me6-TREN as ligand were investigated by SET-LRP method in aqueous solution. The results show that polyacrylamide synthesized by SET-LRP method has high viscosity in aqueous solution.
【学位授予单位】：大庆石油学院
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：TQ316.322
本文编号：2296969
[Abstract]:In this experiment, a new polymerization method, single electron transfer active radical polymerization (SET-LRP), was used to polymerize acrylamide (AM) monomer. Homopolymer and copolymer of AM were synthesized in aqueous solution and homopolymer of AM were synthesized in ionic liquid. The effects of various experimental factors on polymerization are also investigated. The specific contents are as follows: 1. The homopolymer of AM was successfully synthesized in aqueous solution with copper metal and tris (2-aminomethyethyl) amine (Me6-TREN) as catalyst and 2-chloropropanamide as initiator by SET-LRP method. The effects of different reaction conditions on the molecular weight of the polymer were investigated by changing the reaction time, monomer concentration, reaction temperature and the amount of initiator and ligand. On the basis of single factor experiment, according to the principle of Central Composite Design (CCD) experimental design, the optimum process conditions of polymerization were preliminarily explored by using three factors and three levels of response surface method (RSM). The optimum technological conditions are as follows: the amount of initiator is 1.0 mmol, the mass fraction of monomer is 26, and the reaction time is 40 min. 2. The synthesis methods of ligand Me6-TREN and pentamethylenetriamine were introduced. The homopolymer of AM was successfully synthesized by SET-LRP method with the catalyst Cu (0) as the catalytic system. The effects of ligand type, amount of ligand and reaction time on polymerization were investigated. The results showed that Me6-TREN was a more suitable ligand. 3. Using Cu (0) and Me6-TREN as catalysts and 2-chloropropionamide as initiator, AM and dimethylaminoethyl methacrylate (DM), were synthesized in aqueous solution by SET-LRP method, respectively. Copolymer of AM with methacryloxy ethyl trimethylammonium chloride (DMC). The experimental conditions of copolymerization, such as reaction temperature, reaction time, amount of polymeric monomer and the ratio of the two monomers to the amount of the copolymers, were investigated, and the reaction conditions were explored. 4. The homopolymer of AM was synthesized by SET-LRP method using ionic liquid as solvent, Cu (_ 0) and Me6-TREN as catalyst and 2-chloropropanamide as initiator. The effects of different reaction conditions on the molecular weight of the polymer were investigated by changing the reaction time, monomer concentration, initiator and the amount of catalyst. 5. The effects of aqueous solution concentration, temperature, shear rate, NaCl and CaCl2 content on the apparent viscosity of aqueous solution of AM homopolymer synthesized with Me6-TREN as ligand were investigated by SET-LRP method in aqueous solution. The results show that polyacrylamide synthesized by SET-LRP method has high viscosity in aqueous solution.
【学位授予单位】：大庆石油学院
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：TQ316.322
【引证文献】
相关期刊论文 前2条
1 丁伟;孙颖;吕崇福;魏继军;于涛;;单电子转移活性自由基聚合的现状及展望[J];应用化学;2011年03期
2 丁伟;吕崇福;孙颖;景慧;魏继军;栾和鑫;于涛;曲广淼;;苯乙烯的单电子转移活性自由基聚合[J];应用化学;2011年09期
相关硕士学位论文 前3条
1 吕崇福;基于SET-LRP法合成四臂星形PMA、PSt及P（MA-co-St）[D];东北石油大学;2011年
2 孙颖;单电子转移活性自由基聚合法制备水溶性聚合物[D];东北石油大学;2011年
3 刘小军;系列可聚合离子液体表面活性剂的合成及聚合研究[D];东北石油大学;2012年
，本文编号：2296969
本文链接：https://www.wllwen.com/shekelunwen/minzhuminquanlunwen/2296969.html
