聚乙烯亚胺系侧链液晶高分子的合成表征及吸附性能研究
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摘要
本论文概述聚乙烯亚胺类侧链型液晶高分子的研究进展及其在螯合吸附方面的应用。在分析高分子液晶结构与性能关系的基础上,设计并合成了三个系列以聚乙烯亚胺为主链,亚甲基为柔性间隔基,联苯类衍生物为液晶基元的新型侧链液晶高分子及其离子型聚合物。核磁共振、红外光谱等手段对合成聚合物的结构进行了表征,~1H NMR分析计算得到聚合物的取代度和季铵化程度。
探讨了合成反应条件对聚合物取代度的影响。结果表明,聚合物的取代度随着反应时间的增加而逐渐增大;均相聚合反应比异相聚合反应得到的聚合物取代度更高;聚合物取代度随侧链液晶基元柔性间隔基的增加而降低。这表明聚合物链的不良溶解性和庞大侧基的位阻效应是导致取代度降低的原因。示差扫描量热,偏光显微镜,X射线衍射研究了聚合物的液晶相行为和液晶相结构。结果表明,液晶相的生成与否以及液晶相的类型与液晶基元、柔性间隔基(n)和取代度有关。对于聚合物POMen,只有当间隔基亚甲基数目(n)大于2时才呈现近晶S_B相,分子内部液晶基元成单分子层排列。聚合物PHn液晶相为近晶S_E相,分子内部液晶基元具有以单分子层排列为主的复杂结构,层内还存在高度的分子间位置序。聚合物PCNn液晶相为向列相,分子的质心没有远程位置序,仅存在近程有序。聚合物POMen、PHn和PCNn的清亮点温度随n值的增加而降低,并呈现明显的奇偶效应。只有当液晶基元在主链上的取代度达到一定程度时,聚合物才呈现液晶态,聚合物的相变温度和相变焓随着取代度的增加而升高。
DSC、POM、XRD表征了聚合物季铵盐POMe4CH_3、POMe4OMe4和PCNnCH_3的液晶性能。结果表明聚合物季铵盐POMe4CH_3、POMe4OMe4液晶相结构为近晶S_A相,聚合物分子内部具有离子层和非离子层双层结构;聚合物季铵盐PCNnCH_3液晶相结构为向列相。与聚合物POMe4相比,聚合物季铵盐POMe4CH_3、POMe4OMe4的结晶性减弱(ΔHm减小),液晶性增强(ΔHi减小),且液晶态稳定性增加(ΔT增大)。表明季胺化可以增强其液晶性。聚合物季铵盐POMe4CH_3、POMe4OMe4的结晶性和液晶性先随着季铵化程度的增加而减弱;后又随着季铵化程度的增加而增加。TG分析表明聚合物季铵盐热稳定性较差。
静态吸附法研究了聚合物树脂对Hg(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)、Cd(Ⅱ)、Co(Ⅱ)、zn(Ⅱ)的吸附性能。结果表明,树脂POMen和PHn对Hg(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)和Cd(Ⅱ)有较好的吸附能力,对Co(Ⅱ)和Zn(Ⅱ)的吸附能力小。聚合物树脂POMen和PHn在混合金属离子溶液中对Hg(Ⅱ)表现出很好的选择吸附性。对比聚合物树脂在不同聚集态结构下对单个金属离子最大吸附容量,结果显示,液晶高分子树脂在其液晶态淬火处理后对金属离子的吸附能力,特别是吸附选择性有所提高。这表明聚合物侧链液晶基元的有序排列有助于提高树脂的吸附性能和选择吸附性。聚合物树脂对金属离子的吸附容量随温度的增加而增大,树脂PH4在其液晶态下(温度T＞Tg)对Hg(Ⅱ)的吸附容量发生突跃式的增长。对Hg(Ⅱ)和Pb(Ⅱ)的吸附动力学研究表明,树脂达到吸附平衡所需的时间都比较短。同时,聚合物树脂还具有较好的解吸和重复使用性能。
Polyethyleneimine-based side-chain liquid-crystalline polymers(SCLCP) and their adsorption properties for heavy metal ions were studied.New series of PEI-based SCLCP containing biphenyl mesogenic groups and their ionic familiy with the spacer length from 2 to 6 methylene units were synthesized upon the study of the relationship between chemical structure and properties for SCLCP.The structures of the synthesized polymers were confirmed by IR and ~1H NMR spectroscopy.The substitution degrees of the mesogenic side groups on N-H units of PEI and the quaternization ratios the amino group in the backbone were calculated from ~1H NMR.
It is shown that the substitution degree of mesogenic groups depends on the solvent used for the polymerization and the reaction time.The substitution degree of mesogenic groups increased as the reaction proceeded.Polymerizations carded out in the homogeneous medium result in higher substitution degree than those in the heterogenous medium.In addition,the substitution degree of mesogenic groups decreases with the increasing spacer length under the same reaction conditions.The poor swelling of the polymer backbone and the large size of the mesogenic groups are probably the causes.
The thermal properties of these polymers were investigated by differential scanning calorimetry(DSC),polarized optical macroscopic(POM) and X-ray diffraction(XRD).It is shown that poly(ethyleneimine) is flexible and acts as a suitable main chain component for side-chain liquid crystalline polymers.The thermal properties and LC formation of the polymers are shown to be strongly affected by the type of mesogens,the length of spacer units and the degree of substitution in the side chain.POMen(n＞2) exhibits S_B-type thermotropic liquid-crystalline behaviour with fan textures.There is a lamellar order in these polymers.PHn performs a mesomorphic behaviour of S_E phase with mosaic textures.PCNn shows liquid-crystalline phases of nematic type with schlieren textures,and there is no order in the direction of the molecular long axes.The clearing temperatures decreased as the spacer length increased.A pronounced odd-even effect was observed.There is a minimum substitution degree for liquid crystal formation.The phase transition temperatures increase and the mesomorphic properties become stabilized as the substituting degree increases.
DSC,POM and XRD indicate that POMe4CH_3 and POMe4OMe4 exhibit thermotropic smectic A phases and PCNnCH_3 show thermotropic nematic phases. The ionic liquid crystalline polymers formed a partial bilayer structure in the smectic A phase.The ionic liquid crystalline polymers(POMe4CH_3,POMe4OMe4) show wider mesomorphic temperature ranges(ΔT) compared to the non-ionic liquid crystalline polymers.It seems that the quaternization enhances and stabilizes the mesomorphic properties.The effect of the quaternization ratios of the amino group in the backbone on the thermal properties was investigated.Thermogravimetry anylasis shows that the quaternization leads to thermal degradation of the PEl-base SCLCPs at lower temperatures.
The adsorption properties of the chelating resins for Hg(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)、Cd(Ⅱ)、Co(Ⅱ)、Zn(Ⅱ) were studied.It is shown that the resins can well absorb Hg(Ⅱ)、Pb(Ⅱ)、Cd(Ⅱ) and Cu(Ⅱ) rather than Co(Ⅱ) and Zn(Ⅱ).Besides,the resins have excellent absorptive selectivity for Hg(Ⅱ).By quenching at liquid crystalline phase and isotropic phase,aggregation structures with different orders were obtained.The adsorption results indicate that liquid-crystalline ordered aggregation structure of the chelating resins dramatically improves the adsorption properties and the absorptive selectivity.For PH4,the adsorption capacity for Hg(Ⅱ) dramatically increased at the temperature above Tg.The dynamics investigation of the resins indicated that the adsorption equilibrium time for Hg(Ⅱ) and Pb(Ⅱ) is very short.In addition,the PEI-based polymer resins have excellent regeneration properties.
探讨了合成反应条件对聚合物取代度的影响。结果表明,聚合物的取代度随着反应时间的增加而逐渐增大;均相聚合反应比异相聚合反应得到的聚合物取代度更高;聚合物取代度随侧链液晶基元柔性间隔基的增加而降低。这表明聚合物链的不良溶解性和庞大侧基的位阻效应是导致取代度降低的原因。示差扫描量热,偏光显微镜,X射线衍射研究了聚合物的液晶相行为和液晶相结构。结果表明,液晶相的生成与否以及液晶相的类型与液晶基元、柔性间隔基(n)和取代度有关。对于聚合物POMen,只有当间隔基亚甲基数目(n)大于2时才呈现近晶S_B相,分子内部液晶基元成单分子层排列。聚合物PHn液晶相为近晶S_E相,分子内部液晶基元具有以单分子层排列为主的复杂结构,层内还存在高度的分子间位置序。聚合物PCNn液晶相为向列相,分子的质心没有远程位置序,仅存在近程有序。聚合物POMen、PHn和PCNn的清亮点温度随n值的增加而降低,并呈现明显的奇偶效应。只有当液晶基元在主链上的取代度达到一定程度时,聚合物才呈现液晶态,聚合物的相变温度和相变焓随着取代度的增加而升高。
DSC、POM、XRD表征了聚合物季铵盐POMe4CH_3、POMe4OMe4和PCNnCH_3的液晶性能。结果表明聚合物季铵盐POMe4CH_3、POMe4OMe4液晶相结构为近晶S_A相,聚合物分子内部具有离子层和非离子层双层结构;聚合物季铵盐PCNnCH_3液晶相结构为向列相。与聚合物POMe4相比,聚合物季铵盐POMe4CH_3、POMe4OMe4的结晶性减弱(ΔHm减小),液晶性增强(ΔHi减小),且液晶态稳定性增加(ΔT增大)。表明季胺化可以增强其液晶性。聚合物季铵盐POMe4CH_3、POMe4OMe4的结晶性和液晶性先随着季铵化程度的增加而减弱;后又随着季铵化程度的增加而增加。TG分析表明聚合物季铵盐热稳定性较差。
静态吸附法研究了聚合物树脂对Hg(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)、Cd(Ⅱ)、Co(Ⅱ)、zn(Ⅱ)的吸附性能。结果表明,树脂POMen和PHn对Hg(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)和Cd(Ⅱ)有较好的吸附能力,对Co(Ⅱ)和Zn(Ⅱ)的吸附能力小。聚合物树脂POMen和PHn在混合金属离子溶液中对Hg(Ⅱ)表现出很好的选择吸附性。对比聚合物树脂在不同聚集态结构下对单个金属离子最大吸附容量,结果显示,液晶高分子树脂在其液晶态淬火处理后对金属离子的吸附能力,特别是吸附选择性有所提高。这表明聚合物侧链液晶基元的有序排列有助于提高树脂的吸附性能和选择吸附性。聚合物树脂对金属离子的吸附容量随温度的增加而增大,树脂PH4在其液晶态下(温度T＞Tg)对Hg(Ⅱ)的吸附容量发生突跃式的增长。对Hg(Ⅱ)和Pb(Ⅱ)的吸附动力学研究表明,树脂达到吸附平衡所需的时间都比较短。同时,聚合物树脂还具有较好的解吸和重复使用性能。
Polyethyleneimine-based side-chain liquid-crystalline polymers(SCLCP) and their adsorption properties for heavy metal ions were studied.New series of PEI-based SCLCP containing biphenyl mesogenic groups and their ionic familiy with the spacer length from 2 to 6 methylene units were synthesized upon the study of the relationship between chemical structure and properties for SCLCP.The structures of the synthesized polymers were confirmed by IR and ~1H NMR spectroscopy.The substitution degrees of the mesogenic side groups on N-H units of PEI and the quaternization ratios the amino group in the backbone were calculated from ~1H NMR.
It is shown that the substitution degree of mesogenic groups depends on the solvent used for the polymerization and the reaction time.The substitution degree of mesogenic groups increased as the reaction proceeded.Polymerizations carded out in the homogeneous medium result in higher substitution degree than those in the heterogenous medium.In addition,the substitution degree of mesogenic groups decreases with the increasing spacer length under the same reaction conditions.The poor swelling of the polymer backbone and the large size of the mesogenic groups are probably the causes.
The thermal properties of these polymers were investigated by differential scanning calorimetry(DSC),polarized optical macroscopic(POM) and X-ray diffraction(XRD).It is shown that poly(ethyleneimine) is flexible and acts as a suitable main chain component for side-chain liquid crystalline polymers.The thermal properties and LC formation of the polymers are shown to be strongly affected by the type of mesogens,the length of spacer units and the degree of substitution in the side chain.POMen(n＞2) exhibits S_B-type thermotropic liquid-crystalline behaviour with fan textures.There is a lamellar order in these polymers.PHn performs a mesomorphic behaviour of S_E phase with mosaic textures.PCNn shows liquid-crystalline phases of nematic type with schlieren textures,and there is no order in the direction of the molecular long axes.The clearing temperatures decreased as the spacer length increased.A pronounced odd-even effect was observed.There is a minimum substitution degree for liquid crystal formation.The phase transition temperatures increase and the mesomorphic properties become stabilized as the substituting degree increases.
DSC,POM and XRD indicate that POMe4CH_3 and POMe4OMe4 exhibit thermotropic smectic A phases and PCNnCH_3 show thermotropic nematic phases. The ionic liquid crystalline polymers formed a partial bilayer structure in the smectic A phase.The ionic liquid crystalline polymers(POMe4CH_3,POMe4OMe4) show wider mesomorphic temperature ranges(ΔT) compared to the non-ionic liquid crystalline polymers.It seems that the quaternization enhances and stabilizes the mesomorphic properties.The effect of the quaternization ratios of the amino group in the backbone on the thermal properties was investigated.Thermogravimetry anylasis shows that the quaternization leads to thermal degradation of the PEl-base SCLCPs at lower temperatures.
The adsorption properties of the chelating resins for Hg(Ⅱ)、Pb(Ⅱ)、Cu(Ⅱ)、Cd(Ⅱ)、Co(Ⅱ)、Zn(Ⅱ) were studied.It is shown that the resins can well absorb Hg(Ⅱ)、Pb(Ⅱ)、Cd(Ⅱ) and Cu(Ⅱ) rather than Co(Ⅱ) and Zn(Ⅱ).Besides,the resins have excellent absorptive selectivity for Hg(Ⅱ).By quenching at liquid crystalline phase and isotropic phase,aggregation structures with different orders were obtained.The adsorption results indicate that liquid-crystalline ordered aggregation structure of the chelating resins dramatically improves the adsorption properties and the absorptive selectivity.For PH4,the adsorption capacity for Hg(Ⅱ) dramatically increased at the temperature above Tg.The dynamics investigation of the resins indicated that the adsorption equilibrium time for Hg(Ⅱ) and Pb(Ⅱ) is very short.In addition,the PEI-based polymer resins have excellent regeneration properties.
引文
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