SET-LRP法制備星型疏水締合水溶性聚合物及其性能研究
發(fā)布時(shí)間:2018-03-01 13:09
本文關(guān)鍵詞: 單電子轉(zhuǎn)移活性自由基聚合 星型疏水締合水溶性聚合物 N-叔丁基丙烯酰胺 性能 出處:《東北石油大學(xué)》2017年碩士論文 論文類型:學(xué)位論文
【摘要】:本文采用單電子轉(zhuǎn)移活性自由基聚合方法(SET-LRP),以“先核法”手段先后合成了三種不同的星型疏水締合水溶性聚合物,同時(shí)對(duì)聚合物的反應(yīng)因素和溶液性能做出了研究,主要的研究?jī)?nèi)容如下:1.實(shí)驗(yàn)以三(2-氨乙基)胺(TREN)、甲酸和甲醛等為原料合成了實(shí)驗(yàn)所用配體三(2-甲氨基乙基)胺(Me_6-TREN),通過(guò)紅外光譜(FT-IR)和核磁共振(1H NMR)分析證明所得產(chǎn)物為目標(biāo)產(chǎn)物。2.以季戊四醇、四氫呋喃及三乙胺等為原料,經(jīng)過(guò)2-溴異丁酰溴的;铣闪诵切痛蠓肿右l(fā)劑2-溴異丁酸季戊四醇四酯(PT-Br),通過(guò)FT-IR和1H NMR證明所得產(chǎn)物為目標(biāo)產(chǎn)物。3.采用SET-LRP方法,先后以四氯化碳(CCl_4)、2-溴異丁酸季戊四醇四酯(PT-Br)為引發(fā)劑,Cu0粉/Me_6-TREN為催化體系,在水溶液中分別合成出了二元星型疏水締合水溶性聚合物P(AM-co-NtBA)和三元星型疏水締合水溶性聚合物P(AM/NtBA/NaAMPS)。采用FT-IR和1H NMR分析所得產(chǎn)物為目標(biāo)產(chǎn)物。通過(guò)控制變量法分別考察了各反應(yīng)因素對(duì)聚合物相對(duì)分子質(zhì)量的影響,確定了星型疏水締合水溶性聚合物合成的最佳工藝條件,其中以CCl_4和PT-Br為核的P(AM-co-NtBA)最高相對(duì)分子質(zhì)量分別為189萬(wàn)和214萬(wàn),而以PT-Br為核的P(AM/Nt BA/NaAMPS)的相對(duì)分子質(zhì)量可達(dá)到223萬(wàn)。同時(shí),考察了聚合反應(yīng)條件的變化對(duì)聚合反應(yīng)動(dòng)力學(xué)產(chǎn)生的影響,結(jié)果表明,ln([M]0/[M])隨聚合反應(yīng)時(shí)間的增大呈線性增大,表現(xiàn)為一級(jí)動(dòng)力學(xué)關(guān)系,反映出了活性自由基聚合應(yīng)具有的特點(diǎn)。4.通過(guò)測(cè)定在不同溫度和鹽濃度下聚合物溶液的表觀粘度,研究了星型疏水締合水溶性聚合物的耐溫抗鹽性能,實(shí)驗(yàn)結(jié)果表明,星型聚合物的溶液性能與線型化聚合物相似,但從表觀粘度上看,隨著溫度的升高和鹽濃度的增加,兩種形態(tài)的聚合物溶液表觀粘度呈現(xiàn)下降趨勢(shì),且星型聚合物的耐溫抗鹽性要略優(yōu)于其線型化聚合物,并且在相同鹽濃度下CaCl_2對(duì)聚合物表觀粘度的影響比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.
【學(xué)位授予單位】:東北石油大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:TQ316.322
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本文編號(hào):1552063
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