SET-LRP法制备星型疏水缔合水溶性聚合物及其性能研究

发布时间：2018-03-01 13:09

  本文关键词： 单电子转移活性自由基聚合 星型疏水缔合水溶性聚合物 N-叔丁基丙烯酰胺 性能　出处：《东北石油大学》2017年硕士论文　论文类型：学位论文

【摘要】：本文采用单电子转移活性自由基聚合方法(SET-LRP),以“先核法”手段先后合成了三种不同的星型疏水缔合水溶性聚合物,同时对聚合物的反应因素和溶液性能做出了研究,主要的研究内容如下:1.实验以三(2-氨乙基)胺(TREN)、甲酸和甲醛等为原料合成了实验所用配体三(2-甲氨基乙基)胺(Me_6-TREN),通过红外光谱(FT-IR)和核磁共振(1H NMR)分析证明所得产物为目标产物。2.以季戊四醇、四氢呋喃及三乙胺等为原料,经过2-溴异丁酰溴的酰化合成了星型大分子引发剂2-溴异丁酸季戊四醇四酯(PT-Br),通过FT-IR和1H NMR证明所得产物为目标产物。3.采用SET-LRP方法,先后以四氯化碳(CCl_4)、2-溴异丁酸季戊四醇四酯(PT-Br)为引发剂,Cu0粉/Me_6-TREN为催化体系,在水溶液中分别合成出了二元星型疏水缔合水溶性聚合物P(AM-co-NtBA)和三元星型疏水缔合水溶性聚合物P(AM/NtBA/NaAMPS)。采用FT-IR和1H NMR分析所得产物为目标产物。通过控制变量法分别考察了各反应因素对聚合物相对分子质量的影响,确定了星型疏水缔合水溶性聚合物合成的最佳工艺条件,其中以CCl_4和PT-Br为核的P(AM-co-NtBA)最高相对分子质量分别为189万和214万,而以PT-Br为核的P(AM/Nt BA/NaAMPS)的相对分子质量可达到223万。同时,考察了聚合反应条件的变化对聚合反应动力学产生的影响,结果表明,ln([M]0/[M])随聚合反应时间的增大呈线性增大,表现为一级动力学关系,反映出了活性自由基聚合应具有的特点。4.通过测定在不同温度和盐浓度下聚合物溶液的表观粘度,研究了星型疏水缔合水溶性聚合物的耐温抗盐性能,实验结果表明,星型聚合物的溶液性能与线型化聚合物相似,但从表观粘度上看,随着温度的升高和盐浓度的增加,两种形态的聚合物溶液表观粘度呈现下降趋势,且星型聚合物的耐温抗盐性要略优于其线型化聚合物,并且在相同盐浓度下CaCl_2对聚合物表观粘度的影响比NaCl大。
[Abstract]:In this paper, three different star hydrophobically associating water-soluble polymers have been synthesized by means of "first nucleation method" by means of single electron transfer active radical polymerization. The reaction factors and solution properties of the polymers have also been studied. The main contents of this study are as follows: 1. The ligand triamethylaminoethyl) triamethylamine Me6-TRENN was synthesized from triamethylaminoethyl triamine, formic acid and formaldehyde. The results of FTIR and 1H NMRs showed that the product was obtained by means of FT-IR and 1H NMRs. With pentaerythritol, Tetrahydrofuran and triethylamine were synthesized by acylation of 2-bromoisobutylol bromide. The star macromolecular initiator 2-pentaerythritol 2-bromoisobutyrate tetraester PT-Brine was synthesized. The product was proved to be the target product by FT-IR and 1H NMR. SET-LRP method was used. Carbon tetrachloride (CCl4) 2-pentaerythritol tetraester (PT-Br) was used as the initiator, and the Cu0 powder / Me6-TREN was used as the catalytic system. The binary star hydrophobically associating water-soluble polymer (PIAM-co-NtBA) and the ternary star hydrophobically associating water-soluble polymer (PIAM-co-NtBA) were synthesized in aqueous solution respectively. The products obtained by FT-IR and 1H NMR analysis were used as the target products. The influence of various reaction factors on the relative molecular weight of polymer was observed. The optimum conditions for the synthesis of star-type hydrophobically associating water-soluble polymers were determined. The maximum relative molecular weight of CCl_4 and PT-Br were 189 million and 2.14 million, respectively, while that of PT-Br was 2.23 million. The effect of the reaction conditions on the kinetics of the polymerization was investigated. The results showed that the polymerization time increased linearly with the increase of polymerization time, and showed a first-order kinetic relationship. The characteristics of active radical polymerization. 4. By measuring the apparent viscosity of polymer solution at different temperature and salt concentration, the temperature resistance and salt resistance of star hydrophobically associating water-soluble polymer were studied. The solution properties of star-shaped polymers are similar to those of linear polymers, but the apparent viscosity of the two kinds of polymer solutions decreases with the increase of temperature and salt concentration. The temperature and salt resistance of star polymer is slightly better than that of linear polymer, and the effect of CaCl_2 on the apparent viscosity of the polymer is greater than that of NaCl at the same salt concentration.
【学位授予单位】：东北石油大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ316.322
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本文编号：1552063