單電子轉(zhuǎn)移活性自由基聚合法制備丙烯酰胺類聚合物
發(fā)布時(shí)間：2018-10-26 21:17
【摘要】： 本實(shí)驗(yàn)以一種新的聚合方法—單電子轉(zhuǎn)移活性自由基聚合法(SET-LRP)來(lái)聚合丙烯酰胺(AM)單體,在水溶液中合成了AM的均聚物和共聚物,在離子液體中合成了AM的均聚物,并且考察了各實(shí)驗(yàn)因素對(duì)聚合的影響,具體內(nèi)容如下: 1.以金屬銅和三(2-氨甲基乙基)胺(Me6-TREN)為催化劑,2-氯丙酰胺為引發(fā)劑,采用SET-LRP方法在水溶液中成功合成了AM的均聚物。通過(guò)改變反應(yīng)時(shí)間、單體濃度、反應(yīng)溫度、引發(fā)劑和配體的用量等實(shí)驗(yàn)條件,考察了不同反應(yīng)條件對(duì)聚合物分子量的影響。在單因素實(shí)驗(yàn)基礎(chǔ)上,根據(jù)Central Composite Design(CCD)實(shí)驗(yàn)設(shè)計(jì)原理,采用三因素三水平的響應(yīng)面法(RSM)對(duì)聚合反應(yīng)的最佳工藝條件進(jìn)行了初步探索,得出的最佳工藝條件是:引發(fā)劑用量為1.0mmol,單體質(zhì)量分?jǐn)?shù)為26%,反應(yīng)時(shí)間為40min。 2.介紹了配體Me6-TREN和五甲基二乙三胺的合成方法,并分別與催化劑Cu(0)作為催化體系,采用SET-LRP方法在水溶液中成功合成了AM的均聚物。通過(guò)考察配體種類、配體用量和反應(yīng)時(shí)間對(duì)聚合反應(yīng)的影響,結(jié)果表明Me6-TREN為更適宜配體。 3.以Cu(0)和Me6-TREN為催化劑,2-氯丙酰胺為引發(fā)劑,采用SET-LRP方法在水溶液中分別合成了AM與甲基丙烯酸二甲氨基乙酯(DM)、AM與甲基丙烯酰氧乙基三甲基氯化銨(DMC)的共聚物�？疾炝斯簿鄯磻�(yīng)的實(shí)驗(yàn)條件,即反應(yīng)溫度、反應(yīng)時(shí)間、聚合單體的用量及兩種單體物質(zhì)的量之比對(duì)共聚物的轉(zhuǎn)化率和分子量大小的影響,對(duì)反應(yīng)的工藝條件進(jìn)行了探索。 4.以離子液體為溶劑,Cu(0)和Me6-TREN為催化劑,2-氯丙酰胺為引發(fā)劑,用SET-LRP方法合成了AM的均聚物。通過(guò)改變反應(yīng)時(shí)間、單體濃度、引發(fā)劑和催化劑的用量等,考察了不同反應(yīng)條件對(duì)聚合物分子量的影響。 5.在水溶液中采用SET-LRP方法,以Me6-TREN為配體合成的AM均聚物為研究對(duì)象,考察其水溶液濃度、溫度、剪切速率、NaCl和CaCl2用量對(duì)聚合物水溶液表觀粘度的影響。結(jié)果表明采用SET-LRP方法合成的聚丙烯酰胺在水溶液中具有較高的粘度。
[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.
【學(xué)位授予單位】：大慶石油學(xué)院
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2010
【分類號(hào)】：TQ316.322
本文編號(hào)：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.
【學(xué)位授予單位】：大慶石油學(xué)院
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2010
【分類號(hào)】：TQ316.322
【引證文獻(xiàn)】
相關(guān)期刊論文 前2條
1 丁偉;孫穎;呂崇福;魏繼軍;于濤;;單電子轉(zhuǎn)移活性自由基聚合的現(xiàn)狀及展望[J];應(yīng)用化學(xué);2011年03期
2 丁偉;呂崇福;孫穎;景慧;魏繼軍;欒和鑫;于濤;曲廣淼;;苯乙烯的單電子轉(zhuǎn)移活性自由基聚合[J];應(yīng)用化學(xué);2011年09期
相關(guān)碩士學(xué)位論文 前3條
1 呂崇福;基于SET-LRP法合成四臂星形PMA、PSt及P（MA-co-St）[D];東北石油大學(xué);2011年
2 孫穎;單電子轉(zhuǎn)移活性自由基聚合法制備水溶性聚合物[D];東北石油大學(xué);2011年
3 劉小軍;系列可聚合離子液體表面活性劑的合成及聚合研究[D];東北石油大學(xué);2012年
，本文編號(hào)：2296969
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