海藻酸钠及其衍生物有序组合体的构筑和功能特性的研究
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摘要
海藻酸盐是一类生物高分子,因其具有天然、无毒、安全性好、生物相容性好、在体内可降解吸收等特点,在生物医药、食品、化妆品等诸多领域有广泛应用。本文基于海藻酸钠(NaAlg)在水溶液中的自组装行为和规律,考察了环境因素的改变及NaAlg疏水修饰对其聚集体结构和聚集行为的影响,探讨了NaAlg与表面活性剂的相互作用机制,并以NaAlg及其与表面活性剂复配体系为软模板,制备了尺寸形貌较为特殊的金、银纳/微米粒子。主要研究结果如下:
1.在含盐的NaAlg稀溶液中,随着介质的pH改变,NaAlg分子结构中-COO-基团可以转变为-COOH基团,从而导致NaAlg分子从舒展链状向胶束转变,直至无规团状沉淀生成。当介质pH为3.0~4.0时,NaAlg胶束的几何形状为球状胶束,这一方面可以从TEM和AFM结果得到明证,还可以从荧光光谱、电学性质和激光光散射等实验结果得到佐证。当溶液的pH进一步降低到2.5附近时,各胶束间的静电排斥明显削弱,使得胶束互相靠近并聚集,随环境的pH进一步下降,海藻酸大量团聚,最终出现沉淀。
2.利用等温滴定微量热、表面张力、电导、Zeta电位、粘度、荧光光谱等测试手段分别从热力学、表面物理化学、电学、流变学和光谱学等角度考察了阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)与NaAlg之间的相互作用。在NaAlg / CTAB体系中,随NaAlg浓度的增加,使得CTAB的c1减小,而c2则增大。表面活性剂浓度小于c1时,CTAB单体主要在表面定向性吸附,溶液的表面张力明显降低;当浓度增加超过c1时,CTAB分子的阳离子极性头基与NaAlg主链上的-COO-发生静电作用,并产生疏水微区;当CTAB浓度进一步增加超过溶液Zeta电位为零时的浓度(cζ=0)后,CTAB分子的疏水链与NaAlg / CTAB复合物的疏水微区发生疏水作用,形成新的NaAlg / CTAB复合胶束;当浓度进一步增加超过c2时,CTAB分子在NaAlg高分子链上的结合达到饱和,CTAB单体开始形成自由胶束,并与NaAlg / CTAB复合胶束共存。此外,随介质pH值降低,能形成更大的网状交联聚集体,使溶液粘度急剧增加。
3.阴离子表面活性剂十二烷基硫酸钠(SDS)、非离子表面活性剂辛基酚聚氧乙烯醚(Tritonx-100)与NaAlg之间也可以形成复合胶束,但复合胶束形成与否依赖于溶液的pH和盐浓度。对NaAlg / SDS体系而言,当pH从7.0降到5.0时,SDS与NaAlg很难结合;当pH由5.0降低到3.0时,疏水作用促使SDS与NaAlg形成NaAlg / SDS复合胶束。对TritonX-100-NaAlg体系而言,在酸性条件下TritonX-100与NaAlg主要发生疏水作用,从而形成NaAlg / TritonX-100复合胶束。
4.采用1-乙基-(3-二甲氨基丙基)碳二亚胺(EDC)为偶联剂,NaAlg与脂肪胺发生酰胺化反应,合成了疏水修饰的NaAlg衍生物。衍生物结构分别以FT-IR、1H-NMR、DSC和TG等技术手段得到表征。通过元素分析确定酰胺的取代度,利用等温滴定微量热、荧光光谱、表面张力、电导等手段研究了疏水修饰NaAlg衍生物在水溶液的聚集行为及与表面活性剂的相互作用。研究结果表明,在稀溶液中,衍生物溶液的表面张力随浓度及疏水取代度的增加而下降;对相同浓度和取代度的衍生物,表面张力随疏水链碳数的增加而下降;相同浓度的衍生物溶液的电导率随取代度的增加而下降。荧光光谱测定显示溶液在较低浓度时即形成疏水微区,微区极性随取代度的增加而降低。表面张力测定结果显示,SDS与疏水修饰NaAlg衍生物复合体系比相同浓度单一体系的表面张力数值更低,并且随NaAlg衍生物取代度的增加,将导致SDS的c1降低和c2增大。
5.基于以上研究,将NaAlg-表面活性剂体系应用于金、银纳/微米粒子的制备。在NaAlg溶液中,采用晶种生长法制备金、银纳/微米粒子,通过紫外光谱、FT-IR、X射线衍射和透射电镜等测试手段探究了NaAlg及NaAlg与不同表面活性剂混合溶液中金、银纳/微米粒子的形成机理,揭示了金、银纳/微米材料的微观结构、尺寸大小和生长形貌的变化规律。研究结果表明,在NaAlg与氯金酸反应体系中,NaAlg能将氯金酸Au(Ⅲ)还原成Au(0);微波辐照能强化成核过程,晶核一旦形成,金离子则易在晶核上还原成金单质而生长;X射线衍射分析表明金纳米更易沿着非最低能量(111)表面生长,而表面活性剂的加入对NaAlg制备的金纳米粒子的形貌有独特的影响。此外,在室温条件下,NaAlg可缓慢地将Ag+还原成Ag原子,最终形成枝状结构,该结构的形貌受NaAlg浓度调控。
Alginate has been extensively used in the fields of pharmacy, food and cosmetics due to its natural, non-toxic, safty, biocompatibility, degradability and absorbability. Based on the self-assembly behaviors of sodium alginate (NaAlg) in aqueous solution, the effects of pH and hydrophobic modification on the properties and structures of NaAlg aggregates have been investigated. The possible mechanisms of the interactions between NaAlg and traditional surfactants have been proposed. Subsquently, gold and silver nanoparticles with particular size and morphology have been fabricated using NaAlg (and NaAlg/surfactants aggregates) as soft templates.
Main results and conclusions are as follows,
1. In the dilute NaAlg solution containing inorganic salt, the pH effect on the aggregate structures was investigated. Because plenty of hydrophilic–COO- groups in the NaAlg polymer chain switched to–COOH groups, which can induce the NaAlg molecular chains aggregating into micelles untile the random group-like precipitate is generated. At pH 3.0-4.0, spherical micelles can be clearly observed by TEM and AFM, which was in the coindence with the proofs of fluorescence spectroscopy, electrical properties, laser light scattering and other experimental results. When pH value of the system decreases to about 2.0, electrostatic repulsion among the micelles obviously weakens, resulting in approach and aggregation among micelles. As the pH value further decreases, alginate acid heavily aggregates, and the precipitation finally appears.
2. Interactions between cationic surfactant cetyltrimethylammonium bromide (CTAB) and NaAlg are studied with isothermal titration calorimetry, surface tension, conductivity, Zeta potential, viscosity and fluorescence spectrum, etc. In the NaAlg / CTAB system, the c1 of CTAB decreases and c2 increases as the concentration of NaAlg increases. As the surfactant concentration is less than c1, CTAB monomers mainly manifest oriented adsorption on the solution surface, and surface tension of the solution apparently decreases. When the surfactant concentration is over c1, electrostatic interactions between the cationic polar heads on CTAB monomers and -COO- groups along alginate chains take place, and hydrophobic microdomain forms. When the CTAB concentration further increases and excesses cζ=0, hydrophobic interactions happen between hydrophobic chains of CTAB monomers and hydrophobic microdomain of CTAB/alginate complexes. When the CTAB concentration further increases till more than c2, the degree of combination of CTAB molecules with alginate macromolecule chain is saturated, then CTAB monomers begin to form free micelles that coexist with mixed CTAB/alginate micelles. Moreover, with the decrease of the pH of the solution, this makes larger networking aggregate and the viscosity of solution sharply increase.
3. The complex micelle can be formed between NaAlg and the anionic surfactant sodium dodecyl sulfate (SDS) as well as the non-ionic surfactant octylphenol polyethoxylates (Tritonx-100), which depends upon the pH value and salt concentration of the solution. In the experimental conditions, when the pH value of the solution decreases from 7.0 to 5.0, SDS can not combine with alginate because of electrostatic repulsion. As the pH value of solution decreases from 5.0 to 3.0, NaAlg combines with SDS to form complex micelle by hydrophobic interaction. At the same time, TritonX-100 and NaAlg form complex micelle by hydrophobic interaction in the acidic solution.
4. NaAlg reacts with fatty amine in the presence of the coupling agent, 1-ethyl- (3-dimethylamino-propyl) carbodiimide (EDC) to obtain hydrophobically modified alginate derivative. The products are characterized by FT-IR, 1H-NMR, DSC and TG, etc, and the substituting degree of amide is confirmed by elementary analysis. The self-assembled behaviors of the hydrophobically modified alginate derivatives (HMA-R) and the interactions between alginate derivatives and surfactants in aqueous solution are investigated by isothermal titration calorimetry, fluorescence spectrum, surface tension and conductivity, etc. In the dilute solution, surface tension of the derivatives solutions decreases as the concentration increases. At the same concentration, the surface tension and conductivity decreases as the substituting degree increases. At the same substituting degree and concentration, surface tension decreases as the number of carbon in the hydrophobic pendants increases. Fluorescence spectroscopy shows hydrophobic microdomain can be formed in the lower concentration and the polarity of microdomain decreases as substituting degree increases. Interactions between SDS and hydrophobically modified alginate derivatives mainly manifest the hydrophobic combination, and the surface tension of mixed system is much lower compared to that of indivadule system. In the mixed system the c1 of SDS will decrease and the c2 of SDS increase with substitution degree increasing.
5. The gold and silver nano-micnon particles are fabricated by a seeding growth approach in NaAlg solution. The formation mechanisms of noble metal nano-micnon particles are explored in NaAlg solution with or without different surfactants by means of UV-vis spectrum, FT-IR, X-ray diffraction and transmission electron microscope (TEM), etc, and then the variation laws of microstructures, sizes and morphologies of the noble metal materials are revealed. The results show that NaAlg reduces HAuCl to Au in NaAlg/HAuCl4 reaction system, and the nucleation process can be strengthened by the microwave radiation. Once crystal nucleus forms, Au ion on crystal nucleus can be easily reduced to elementary substance and then grow. From X-ray diffraction analysis, the crystal face (111) of prepared gold nanoparticles show a great diffraction intensity, which demonstrates that gold nanoparticles can easily grow along the face. We also find that surfactants have unique influence on preparing gold nanoparticles. At ambient condition, sodium alginate slowly reduces Ag(I) to Ag(0) on the surfaces of Ag seeds, and then form branch structure. Ag particles aggregate into the branch structures with different morphologies under various concentration of NaAlg aqueous solution.
1.在含盐的NaAlg稀溶液中,随着介质的pH改变,NaAlg分子结构中-COO-基团可以转变为-COOH基团,从而导致NaAlg分子从舒展链状向胶束转变,直至无规团状沉淀生成。当介质pH为3.0~4.0时,NaAlg胶束的几何形状为球状胶束,这一方面可以从TEM和AFM结果得到明证,还可以从荧光光谱、电学性质和激光光散射等实验结果得到佐证。当溶液的pH进一步降低到2.5附近时,各胶束间的静电排斥明显削弱,使得胶束互相靠近并聚集,随环境的pH进一步下降,海藻酸大量团聚,最终出现沉淀。
2.利用等温滴定微量热、表面张力、电导、Zeta电位、粘度、荧光光谱等测试手段分别从热力学、表面物理化学、电学、流变学和光谱学等角度考察了阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)与NaAlg之间的相互作用。在NaAlg / CTAB体系中,随NaAlg浓度的增加,使得CTAB的c1减小,而c2则增大。表面活性剂浓度小于c1时,CTAB单体主要在表面定向性吸附,溶液的表面张力明显降低;当浓度增加超过c1时,CTAB分子的阳离子极性头基与NaAlg主链上的-COO-发生静电作用,并产生疏水微区;当CTAB浓度进一步增加超过溶液Zeta电位为零时的浓度(cζ=0)后,CTAB分子的疏水链与NaAlg / CTAB复合物的疏水微区发生疏水作用,形成新的NaAlg / CTAB复合胶束;当浓度进一步增加超过c2时,CTAB分子在NaAlg高分子链上的结合达到饱和,CTAB单体开始形成自由胶束,并与NaAlg / CTAB复合胶束共存。此外,随介质pH值降低,能形成更大的网状交联聚集体,使溶液粘度急剧增加。
3.阴离子表面活性剂十二烷基硫酸钠(SDS)、非离子表面活性剂辛基酚聚氧乙烯醚(Tritonx-100)与NaAlg之间也可以形成复合胶束,但复合胶束形成与否依赖于溶液的pH和盐浓度。对NaAlg / SDS体系而言,当pH从7.0降到5.0时,SDS与NaAlg很难结合;当pH由5.0降低到3.0时,疏水作用促使SDS与NaAlg形成NaAlg / SDS复合胶束。对TritonX-100-NaAlg体系而言,在酸性条件下TritonX-100与NaAlg主要发生疏水作用,从而形成NaAlg / TritonX-100复合胶束。
4.采用1-乙基-(3-二甲氨基丙基)碳二亚胺(EDC)为偶联剂,NaAlg与脂肪胺发生酰胺化反应,合成了疏水修饰的NaAlg衍生物。衍生物结构分别以FT-IR、1H-NMR、DSC和TG等技术手段得到表征。通过元素分析确定酰胺的取代度,利用等温滴定微量热、荧光光谱、表面张力、电导等手段研究了疏水修饰NaAlg衍生物在水溶液的聚集行为及与表面活性剂的相互作用。研究结果表明,在稀溶液中,衍生物溶液的表面张力随浓度及疏水取代度的增加而下降;对相同浓度和取代度的衍生物,表面张力随疏水链碳数的增加而下降;相同浓度的衍生物溶液的电导率随取代度的增加而下降。荧光光谱测定显示溶液在较低浓度时即形成疏水微区,微区极性随取代度的增加而降低。表面张力测定结果显示,SDS与疏水修饰NaAlg衍生物复合体系比相同浓度单一体系的表面张力数值更低,并且随NaAlg衍生物取代度的增加,将导致SDS的c1降低和c2增大。
5.基于以上研究,将NaAlg-表面活性剂体系应用于金、银纳/微米粒子的制备。在NaAlg溶液中,采用晶种生长法制备金、银纳/微米粒子,通过紫外光谱、FT-IR、X射线衍射和透射电镜等测试手段探究了NaAlg及NaAlg与不同表面活性剂混合溶液中金、银纳/微米粒子的形成机理,揭示了金、银纳/微米材料的微观结构、尺寸大小和生长形貌的变化规律。研究结果表明,在NaAlg与氯金酸反应体系中,NaAlg能将氯金酸Au(Ⅲ)还原成Au(0);微波辐照能强化成核过程,晶核一旦形成,金离子则易在晶核上还原成金单质而生长;X射线衍射分析表明金纳米更易沿着非最低能量(111)表面生长,而表面活性剂的加入对NaAlg制备的金纳米粒子的形貌有独特的影响。此外,在室温条件下,NaAlg可缓慢地将Ag+还原成Ag原子,最终形成枝状结构,该结构的形貌受NaAlg浓度调控。
Alginate has been extensively used in the fields of pharmacy, food and cosmetics due to its natural, non-toxic, safty, biocompatibility, degradability and absorbability. Based on the self-assembly behaviors of sodium alginate (NaAlg) in aqueous solution, the effects of pH and hydrophobic modification on the properties and structures of NaAlg aggregates have been investigated. The possible mechanisms of the interactions between NaAlg and traditional surfactants have been proposed. Subsquently, gold and silver nanoparticles with particular size and morphology have been fabricated using NaAlg (and NaAlg/surfactants aggregates) as soft templates.
Main results and conclusions are as follows,
1. In the dilute NaAlg solution containing inorganic salt, the pH effect on the aggregate structures was investigated. Because plenty of hydrophilic–COO- groups in the NaAlg polymer chain switched to–COOH groups, which can induce the NaAlg molecular chains aggregating into micelles untile the random group-like precipitate is generated. At pH 3.0-4.0, spherical micelles can be clearly observed by TEM and AFM, which was in the coindence with the proofs of fluorescence spectroscopy, electrical properties, laser light scattering and other experimental results. When pH value of the system decreases to about 2.0, electrostatic repulsion among the micelles obviously weakens, resulting in approach and aggregation among micelles. As the pH value further decreases, alginate acid heavily aggregates, and the precipitation finally appears.
2. Interactions between cationic surfactant cetyltrimethylammonium bromide (CTAB) and NaAlg are studied with isothermal titration calorimetry, surface tension, conductivity, Zeta potential, viscosity and fluorescence spectrum, etc. In the NaAlg / CTAB system, the c1 of CTAB decreases and c2 increases as the concentration of NaAlg increases. As the surfactant concentration is less than c1, CTAB monomers mainly manifest oriented adsorption on the solution surface, and surface tension of the solution apparently decreases. When the surfactant concentration is over c1, electrostatic interactions between the cationic polar heads on CTAB monomers and -COO- groups along alginate chains take place, and hydrophobic microdomain forms. When the CTAB concentration further increases and excesses cζ=0, hydrophobic interactions happen between hydrophobic chains of CTAB monomers and hydrophobic microdomain of CTAB/alginate complexes. When the CTAB concentration further increases till more than c2, the degree of combination of CTAB molecules with alginate macromolecule chain is saturated, then CTAB monomers begin to form free micelles that coexist with mixed CTAB/alginate micelles. Moreover, with the decrease of the pH of the solution, this makes larger networking aggregate and the viscosity of solution sharply increase.
3. The complex micelle can be formed between NaAlg and the anionic surfactant sodium dodecyl sulfate (SDS) as well as the non-ionic surfactant octylphenol polyethoxylates (Tritonx-100), which depends upon the pH value and salt concentration of the solution. In the experimental conditions, when the pH value of the solution decreases from 7.0 to 5.0, SDS can not combine with alginate because of electrostatic repulsion. As the pH value of solution decreases from 5.0 to 3.0, NaAlg combines with SDS to form complex micelle by hydrophobic interaction. At the same time, TritonX-100 and NaAlg form complex micelle by hydrophobic interaction in the acidic solution.
4. NaAlg reacts with fatty amine in the presence of the coupling agent, 1-ethyl- (3-dimethylamino-propyl) carbodiimide (EDC) to obtain hydrophobically modified alginate derivative. The products are characterized by FT-IR, 1H-NMR, DSC and TG, etc, and the substituting degree of amide is confirmed by elementary analysis. The self-assembled behaviors of the hydrophobically modified alginate derivatives (HMA-R) and the interactions between alginate derivatives and surfactants in aqueous solution are investigated by isothermal titration calorimetry, fluorescence spectrum, surface tension and conductivity, etc. In the dilute solution, surface tension of the derivatives solutions decreases as the concentration increases. At the same concentration, the surface tension and conductivity decreases as the substituting degree increases. At the same substituting degree and concentration, surface tension decreases as the number of carbon in the hydrophobic pendants increases. Fluorescence spectroscopy shows hydrophobic microdomain can be formed in the lower concentration and the polarity of microdomain decreases as substituting degree increases. Interactions between SDS and hydrophobically modified alginate derivatives mainly manifest the hydrophobic combination, and the surface tension of mixed system is much lower compared to that of indivadule system. In the mixed system the c1 of SDS will decrease and the c2 of SDS increase with substitution degree increasing.
5. The gold and silver nano-micnon particles are fabricated by a seeding growth approach in NaAlg solution. The formation mechanisms of noble metal nano-micnon particles are explored in NaAlg solution with or without different surfactants by means of UV-vis spectrum, FT-IR, X-ray diffraction and transmission electron microscope (TEM), etc, and then the variation laws of microstructures, sizes and morphologies of the noble metal materials are revealed. The results show that NaAlg reduces HAuCl to Au in NaAlg/HAuCl4 reaction system, and the nucleation process can be strengthened by the microwave radiation. Once crystal nucleus forms, Au ion on crystal nucleus can be easily reduced to elementary substance and then grow. From X-ray diffraction analysis, the crystal face (111) of prepared gold nanoparticles show a great diffraction intensity, which demonstrates that gold nanoparticles can easily grow along the face. We also find that surfactants have unique influence on preparing gold nanoparticles. At ambient condition, sodium alginate slowly reduces Ag(I) to Ag(0) on the surfaces of Ag seeds, and then form branch structure. Ag particles aggregate into the branch structures with different morphologies under various concentration of NaAlg aqueous solution.
引文
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