两亲水溶性聚合物的合成、表征及性质研究
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摘要
两亲水溶性聚合物由于疏水基团在水溶液中的憎水作用而产生分子内缔合和分子间缔合,表现出较好的增粘性、耐温耐盐性和抗剪切稳定性。尤其是含有孪尾长链疏水烷基的疏水缔合聚合物,其疏水缔合作用较单尾型的疏水缔合聚合物要强很多,使其在低浓度下就易形成分子间缔合,耐温、抗盐性能突出。本文同时考虑了疏水缔合聚合物、两性聚合物的特性,将磺酸盐单体、两性单体与长链挛尾疏水单体分别进行共聚,合成了一系列新型两亲水溶性聚合物及其衍生物,并用激光光散射、透射电镜等方法考察了聚合物的疏水缔合、耐温抗盐等性能,研究了不同因素对聚合物溶液聚集行为的影响及聚合物结构与溶液性能的关系,并进行聚合物复配、富集铬离子等应用性能测试。主要开展的工作如下几方面：
1、用Al3+作为交联剂制备HPAM-AI的凝胶粒子,并将凝胶粒子与壳聚糖相互作用形成HPAM-chitosan复合凝胶粒子。研究了吸附时间、吸附剂用量、溶液pH、时间、温度和溶液离子浓度等对于凝胶粒子吸附性能的影响,结果表明,准二级动力学方程为复合凝胶粒子吸附动力学的最佳模型,Langmuir模型为其吸附等温线的最佳模型。同时提出了该类复合凝胶粒子吸附铬离子的机理,认为复合凝胶粒子中由于含有大量酰胺基团及羧酸等基团,其吸附三价铬(Cr(Ⅲ))和六价铬(Cr(Ⅵ))均取得了较好的效果,在pH达到4.5以后,吸附Cr(Ⅲ)离子的去除率最高可达67.6%。而Cr(Ⅵ)的吸附量随着pH值的增加表现为先增大后减少的现象,最大的吸附去除率为82.9%。
2、采用胶束聚合法将丙烯酰胺(AM)、2-丙烯酰胺基-2-甲基丙磺酸钠和孪尾疏水单体N,N-二正丁基甲基丙烯酰胺(DBMAM)三元共聚合成一系列不同组成的疏水缔合型水溶性共聚物PAAD。通过1H-NMR、元素分析、静态光散射(SLS)等手段对这一系列共聚物进行表征测试,并通过动态光散射法、表面张力等对这类聚合物的溶液性能进行了详细研究,对其在水溶液中聚集和解聚集行为机理从分子水平上进行了深入研究。同时,还进行了重金属铬离子的沉降实验,检验共聚物PAAD的应用性能。研究结果表明,当浓度较低时,共聚物分子链构象较为伸展,Cr(Ⅲ)离子被吸附于共聚物周围与-SO3-配位,使铬盐富集在PADD的分子链上。随着浓度的增加,孪尾疏水链发生缔合作用,聚合物分子链发生蜷曲,当PAAD浓度大于1.0g/L,包裹铬离子的大聚集体沉淀出现。
3、合成和表征了一系列挛尾单体功能性单体N,N-二己基丙烯酰胺(DHMAM)、N,N-二辛基丙烯酰胺(DOMAM)、N, N-二癸基-N-甲基-N-(4-乙烯基苄基)氯化铵(DDMVBA)、将上述孪尾单体与丙烯酰胺(AM)、甲基丙烯酰氧乙基-N,N-二甲基丙磺酸盐(DMAPS)、乙烯基磺酸钠(SVS)分别进行共聚制备了一系列疏水缔合水溶性共聚物,并通过动态光散射法、表面张力等对这类聚合物的溶液性能进行了表征,结果表明,由于两性离子及疏水单体的引入,聚合物溶液具有良好的表面活性、增黏性能及耐温抗盐性能。与油田用驱油剂AP-P4、SNF等复配后,使得驱油剂体系的增粘性及热稳定性都有所提高,具有较好的潜在应用性能。
4、利用原子转移自由基聚合(ATRP)法合成和表征了单甲醚聚乙二醇改性的大分子引发剂(MAI)与孪尾长链疏水单体(DHMAM)参与的一系列孪尾疏水改性的双亲嵌段共聚物,通过1H-NMR、FT-IR等手段对这一系列共聚物进行表征测试,并通过动态光散射法、透射电镜等对这类聚合物在溶液中的聚集行为和乳化性能进行了研究。
Amphiphilic water-soluble polymer exhibited viscosity performance heat resistance, salt resistance and shear resistance stability due to the hydrophobic effect of hydrophobic groups in aqueous solution because of intermolecular and intramolecular association. Making the comparison for the same total hydrophobe chain length, double-chain hydrophobes considerably enhance the thickening efficiency, heat resistance, and salt resistance with respect to single chain hydrophobes. In this article, a series of novel amphiphilic water-soluble polymer and its derivatives involving sulfonate monomer, amphoteric monomer, and twin-tailed hydrophobic monomer are described and their properties of hydrophobic association, heat resistance, salt resistance, and enrichment of chromium ions in aqueous solution were studied by DLS, and TEM measurements. Main research work are divided into the following several aspects:
1. Hydrolyzed polyacrylamide(HPAM)-chitosan gel beads were utilized as an adsorbent in removing Cr(Ⅵ) and Cr(Ⅲ) from aqueous media. The high percentage of removal for Cr(Ⅵ)-82.9%and Cr(Ⅲ)-67.6%suggests the great potential for HPAM-chitosan gel beads as an adsorbent for the removal of chromium(Cr) ion from aqueous solution. The kinetic data have been tested in the process of adsorption for Cr(Ⅲ) and Cr(Ⅵ), and proved that it follows the pseudo-second-order rate equation. Both Langmuir equations and Freundlich equations were used for explaining the experimental data of adsorption isotherm, which demonstrated a better fit to the Lagmuir model. Thus it suggests a monolayer adsorption process onto the gel beads. Moreover, Chromium adsorption profile onto HPAM-chitosan gel beads is suggested through the schematic representation.
2. Hydrophobically modified polyacrylamides (PAAD) were synthesized by the micellar copolymerization of (AM), sodium2-acrylamide-2-methyl propane sulfonic (AMPSNa) and di-n-butylmethacrylamide (DBMAM). The structure, composition, molecular weight of copolymers were studied by'H-NMR, Elemental analyse(EA), and the static light Scatting(SLS). Then their properties in aqueous solution were studied by DLS and surface tension. The behavior and mechanism of aggregation and degradation for PAAD in aqueous solution were studied, while the experiments for PAAD as an adsorbent for the removal of chromium(Cr) ion from aqueous solution were carried. The results revealed that the adsorption capacity of PAAD on chromium(Cr) ion depended on PADO concentration. At the lower concentration, Cr (Ⅲ) ions coordinated with SO3-ion were adsorbed around the rigid chain of PADD, while PAAD concentration is greater than1.0g/L, the polymer molecular chain curled up because of the association from twin-tailed hydrophobic groups, and the large aggregate precipitate containing Cr (Ⅲ) ions appeared.
3. The twin-tailed functional monomers namely di-n-hexylmethacrylamide, di-n-octylmethacrylamide, and N, N-didecyl-N-methyl-N-(4-vinylbenzyl) ammonium chloride were prepared and characterized. A series of novel hydrophobically modified water-soluble copolymers (DDSPAM) containing the above hydrophobic twin-tailed monomers,3-N-(2-methacroyloylethyl)-N,N-dimethylammonio-propane sulfonate (DMAPS), or sodium Vinylsulfonate (SVS) were prepared by an aqueous micellar polymerization. Then their properties in aqueous solution were characterized by DLS, and surface tension. The molecular weights of the copolymers were obtained via static light scattering. The hydrodynamic radius of aggregates was investigated by dynamic light scattering. The cmc and γ cmc values of DDSPAM were measured by fluorescence measurements and identify with that obtained by surface tension measurements. In addition, the results from the viscosity stability of DDSPAM and hydrolyzed polyacrylamide (HPAM) showed that DDSPAM with twin-tailed hydrophobical groups have better performance of salt tolerance and temperature resistance than that of HPAM. The results show that the copolymers exhibited good surface activity, which can increase the viscosity and provided heat resistance and salt resistance because of the introduction of zwitterions and hydrophobic monomer. In addition, the compound systems of copolymers with oil-displacing agent (AP-P4or SNF) can greatly improve the viscosity and thermal stability and it has the high practical application performance in oil recovery.
4. A series of novel amphiphilic block copolymers involving macromolecular initiator (MAI) and di-n-hexylmethacrylamide (DHMAM) were prepared by ATRP. The structure and composition of DDSPAM were characterized by1H-NMR and FT-IR. The aggregation behavior and emulsion properties of these copolymers in solution were studied though DLS and TEM.
1、用Al3+作为交联剂制备HPAM-AI的凝胶粒子,并将凝胶粒子与壳聚糖相互作用形成HPAM-chitosan复合凝胶粒子。研究了吸附时间、吸附剂用量、溶液pH、时间、温度和溶液离子浓度等对于凝胶粒子吸附性能的影响,结果表明,准二级动力学方程为复合凝胶粒子吸附动力学的最佳模型,Langmuir模型为其吸附等温线的最佳模型。同时提出了该类复合凝胶粒子吸附铬离子的机理,认为复合凝胶粒子中由于含有大量酰胺基团及羧酸等基团,其吸附三价铬(Cr(Ⅲ))和六价铬(Cr(Ⅵ))均取得了较好的效果,在pH达到4.5以后,吸附Cr(Ⅲ)离子的去除率最高可达67.6%。而Cr(Ⅵ)的吸附量随着pH值的增加表现为先增大后减少的现象,最大的吸附去除率为82.9%。
2、采用胶束聚合法将丙烯酰胺(AM)、2-丙烯酰胺基-2-甲基丙磺酸钠和孪尾疏水单体N,N-二正丁基甲基丙烯酰胺(DBMAM)三元共聚合成一系列不同组成的疏水缔合型水溶性共聚物PAAD。通过1H-NMR、元素分析、静态光散射(SLS)等手段对这一系列共聚物进行表征测试,并通过动态光散射法、表面张力等对这类聚合物的溶液性能进行了详细研究,对其在水溶液中聚集和解聚集行为机理从分子水平上进行了深入研究。同时,还进行了重金属铬离子的沉降实验,检验共聚物PAAD的应用性能。研究结果表明,当浓度较低时,共聚物分子链构象较为伸展,Cr(Ⅲ)离子被吸附于共聚物周围与-SO3-配位,使铬盐富集在PADD的分子链上。随着浓度的增加,孪尾疏水链发生缔合作用,聚合物分子链发生蜷曲,当PAAD浓度大于1.0g/L,包裹铬离子的大聚集体沉淀出现。
3、合成和表征了一系列挛尾单体功能性单体N,N-二己基丙烯酰胺(DHMAM)、N,N-二辛基丙烯酰胺(DOMAM)、N, N-二癸基-N-甲基-N-(4-乙烯基苄基)氯化铵(DDMVBA)、将上述孪尾单体与丙烯酰胺(AM)、甲基丙烯酰氧乙基-N,N-二甲基丙磺酸盐(DMAPS)、乙烯基磺酸钠(SVS)分别进行共聚制备了一系列疏水缔合水溶性共聚物,并通过动态光散射法、表面张力等对这类聚合物的溶液性能进行了表征,结果表明,由于两性离子及疏水单体的引入,聚合物溶液具有良好的表面活性、增黏性能及耐温抗盐性能。与油田用驱油剂AP-P4、SNF等复配后,使得驱油剂体系的增粘性及热稳定性都有所提高,具有较好的潜在应用性能。
4、利用原子转移自由基聚合(ATRP)法合成和表征了单甲醚聚乙二醇改性的大分子引发剂(MAI)与孪尾长链疏水单体(DHMAM)参与的一系列孪尾疏水改性的双亲嵌段共聚物,通过1H-NMR、FT-IR等手段对这一系列共聚物进行表征测试,并通过动态光散射法、透射电镜等对这类聚合物在溶液中的聚集行为和乳化性能进行了研究。
Amphiphilic water-soluble polymer exhibited viscosity performance heat resistance, salt resistance and shear resistance stability due to the hydrophobic effect of hydrophobic groups in aqueous solution because of intermolecular and intramolecular association. Making the comparison for the same total hydrophobe chain length, double-chain hydrophobes considerably enhance the thickening efficiency, heat resistance, and salt resistance with respect to single chain hydrophobes. In this article, a series of novel amphiphilic water-soluble polymer and its derivatives involving sulfonate monomer, amphoteric monomer, and twin-tailed hydrophobic monomer are described and their properties of hydrophobic association, heat resistance, salt resistance, and enrichment of chromium ions in aqueous solution were studied by DLS, and TEM measurements. Main research work are divided into the following several aspects:
1. Hydrolyzed polyacrylamide(HPAM)-chitosan gel beads were utilized as an adsorbent in removing Cr(Ⅵ) and Cr(Ⅲ) from aqueous media. The high percentage of removal for Cr(Ⅵ)-82.9%and Cr(Ⅲ)-67.6%suggests the great potential for HPAM-chitosan gel beads as an adsorbent for the removal of chromium(Cr) ion from aqueous solution. The kinetic data have been tested in the process of adsorption for Cr(Ⅲ) and Cr(Ⅵ), and proved that it follows the pseudo-second-order rate equation. Both Langmuir equations and Freundlich equations were used for explaining the experimental data of adsorption isotherm, which demonstrated a better fit to the Lagmuir model. Thus it suggests a monolayer adsorption process onto the gel beads. Moreover, Chromium adsorption profile onto HPAM-chitosan gel beads is suggested through the schematic representation.
2. Hydrophobically modified polyacrylamides (PAAD) were synthesized by the micellar copolymerization of (AM), sodium2-acrylamide-2-methyl propane sulfonic (AMPSNa) and di-n-butylmethacrylamide (DBMAM). The structure, composition, molecular weight of copolymers were studied by'H-NMR, Elemental analyse(EA), and the static light Scatting(SLS). Then their properties in aqueous solution were studied by DLS and surface tension. The behavior and mechanism of aggregation and degradation for PAAD in aqueous solution were studied, while the experiments for PAAD as an adsorbent for the removal of chromium(Cr) ion from aqueous solution were carried. The results revealed that the adsorption capacity of PAAD on chromium(Cr) ion depended on PADO concentration. At the lower concentration, Cr (Ⅲ) ions coordinated with SO3-ion were adsorbed around the rigid chain of PADD, while PAAD concentration is greater than1.0g/L, the polymer molecular chain curled up because of the association from twin-tailed hydrophobic groups, and the large aggregate precipitate containing Cr (Ⅲ) ions appeared.
3. The twin-tailed functional monomers namely di-n-hexylmethacrylamide, di-n-octylmethacrylamide, and N, N-didecyl-N-methyl-N-(4-vinylbenzyl) ammonium chloride were prepared and characterized. A series of novel hydrophobically modified water-soluble copolymers (DDSPAM) containing the above hydrophobic twin-tailed monomers,3-N-(2-methacroyloylethyl)-N,N-dimethylammonio-propane sulfonate (DMAPS), or sodium Vinylsulfonate (SVS) were prepared by an aqueous micellar polymerization. Then their properties in aqueous solution were characterized by DLS, and surface tension. The molecular weights of the copolymers were obtained via static light scattering. The hydrodynamic radius of aggregates was investigated by dynamic light scattering. The cmc and γ cmc values of DDSPAM were measured by fluorescence measurements and identify with that obtained by surface tension measurements. In addition, the results from the viscosity stability of DDSPAM and hydrolyzed polyacrylamide (HPAM) showed that DDSPAM with twin-tailed hydrophobical groups have better performance of salt tolerance and temperature resistance than that of HPAM. The results show that the copolymers exhibited good surface activity, which can increase the viscosity and provided heat resistance and salt resistance because of the introduction of zwitterions and hydrophobic monomer. In addition, the compound systems of copolymers with oil-displacing agent (AP-P4or SNF) can greatly improve the viscosity and thermal stability and it has the high practical application performance in oil recovery.
4. A series of novel amphiphilic block copolymers involving macromolecular initiator (MAI) and di-n-hexylmethacrylamide (DHMAM) were prepared by ATRP. The structure and composition of DDSPAM were characterized by1H-NMR and FT-IR. The aggregation behavior and emulsion properties of these copolymers in solution were studied though DLS and TEM.
引文
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