新型表面活性剂型离子液体的制备及其在纳米材料可控制备中的应用研究

发布时间：2018-06-23 15:21

本文选题：表面活性剂 + 离子液体　；参考：《安徽大学》2015年硕士论文

【摘要】：随着社会经济的快速发展,各种功能材料因其具有很多用途而受到广泛的关注,如羟基磷灰石和金属有机框架材料。离子液体因其具有不挥发、不可燃、导电性强、蒸汽压小、性质稳定,对许多无机盐和有机物有良好的溶解性等优点,在电化学、有机合成、催化、分离等领域被广泛的应用。本论文在三种新型表面活性剂型离子液体合成、表征及其相关性能研究的基础上,以其为模板修饰剂,替代传统的表面活性剂,制备了羟基磷灰石(HA)纳米线、纳米棒以及中空的纳米球和钙金属有机骨架(MOFs)材料,具体内容如下：采用离子交换方法,以四丁基氯化铵和3种经典的阴离子表面活性剂(AOT, SDS和AES)为原料,合成三种具有一定表面活性的表面活性剂型离子液体4[C4N]AOT,4[C4N]DS和4[C4N]AES,并通过核磁共振仪和质谱仪对其进行表征。结果显示三种表面活性剂型离子液体的临界胶束浓度,分别为0.0012 mol/L, 0.0024 mol/L和0.0023 mol/L,较相对应的阴离子表面活性剂的临界胶束浓度明显减小。通过透射电镜(TEM)和动态光散射(DLS)进行表征,结果表明当三种表面活性剂型离子液体浓度在超过其临界胶束浓度(cmc)时可以形成1-3 nm的胶束溶液。进一步,以所合成的表面活性剂型离子液体4[C4N]DS为模板剂,通过调节溶液pH控制HA的002晶面和021晶面方向的生长,成功制备了具有不同尺寸的HA纳米棒和纳米线。以合成的离子液体4[C4N]AES为修饰剂,通过氨水分解产生的氨气缓慢调节体系的pH,成功完成了具有多孔结构的羟基磷灰石纳米花球的制备。考察了HA的形成过程(大块薄片-纳米片状颗粒-薄片自组装而成的中空微球)。XRD结果显示,开始生成的片状产物是CaPO3(OH)·2H2O,然后转变为HA。根据氮气吸附脱附实验说明其具有多孔结构。以此微球为重金属离子吸附剂,考察了其对重金属Cu2+、Pb2+和Zn2+的去除情况。花球状HA对三种重金属的吸附能力为：Pb2+Cu2+Zn2+。其中对Pb2+的吸附率达到99.9%。另外,研究在酸性条件下pH和HA的浓度对Cu2+去除情况,结果表明随着pH和HA的浓度增大,其对Cu2+去除的越多,当HA的浓度达到1.2g/L时,吸附率达到94.96%。金属有机框架因其具有较大的比表面积、很高的孔隙,孔道结构可以调节,使其在药物缓释、多相催化、磁性材料、光电材料、光化学催化、气体吸附和生物传感等方面的应用越来越多。以表面活性剂型离子液体4[C4N]DS为修饰剂,采用水热法制备钙-金属有机骨架材料(MOFs)。测试结果显示,通过改变条件成功获取了Ca-MOFs纳米棒与纳米球。以此Ca-MOFs纳米球作为载体,对尼美舒利进行载药并缓释。Ca-MOFs具有的特殊结构和一定的比表面积有利于载药,并且可以较好的控制尼美舒利的缓释达到较好的药效。
[Abstract]:With the rapid development of social economy, a variety of functional materials, such as hydroxyapatite and organometallic framework materials, have attracted wide attention due to their many applications. Ionic liquids are widely used in the fields of electrochemistry, organic synthesis, catalysis and separation because of their advantages of non-volatile, non-flammable, strong conductivity, low vapor pressure, stable properties and good solubility to many inorganic salts and organic compounds. In this paper, hydroxyapatite (HA) nanowires were prepared by using three new surfactants as template modifiers instead of traditional surfactants on the basis of synthesis, characterization and related properties of three new surfactants. Nanorods as well as hollow nanospheres and calcium metal organic frameworks (MOFs) were prepared by ion exchange method using four Ding Ji ammonium chloride and three classical anionic surfactants (AOT, SDS-AES) as raw materials. Three surfactant ionic liquids 4 [C4N] AOT4 [C4N] DS and 4 [C4N] AESs were synthesized and characterized by NMR and mass spectrometer. The results show that the critical micelle concentrations of the three surfactants are 0.0012 mol / L, 0.0024 mol / L and 0.0023 mol / L, respectively, which are significantly lower than those of the corresponding anionic surfactants. The results of transmission electron microscopy (TEM) and dynamic light scattering (DLS) show that when the concentration of three surfactant ionic liquids exceeds their critical micelle concentration (cmc), a micellar solution of 1-3 nm can be formed. Furthermore, different sizes of HA nanorods and nanowires were successfully prepared by adjusting the pH of the solution to control the growth of the 002 and 021 directions of HA, using the synthesized surfactant ionic liquid 4 [C4N] DS as the template. The synthesis of hydroxyapatite nanospheres with porous structure was successfully completed by slowly adjusting the pH of the system produced by ammonia decomposition with the synthetic ionic liquid 4 [C 4N] AES as modifier. The formation process of HA (hollow microspheres self-assembled by bulk flakes, nanocrystalline particles and thin sheets) was investigated. XRD results showed that the first flake product was CaPO3 (OH) 2H2O, and then the HA was transformed into HA3 (OH) _ 2H _ 2O. According to nitrogen adsorption and desorption experiments, it has porous structure. The removal of Cu _ (2) Pb _ (2) and Zn _ (2) by microspheres as heavy metal ion adsorbents was investigated. The adsorption ability of flower globular HA for three heavy metals was: 1 / Pb 2Cu 2Zn 2. The adsorption rate of PB2 was 99.9%. In addition, the removal of Cu2 by pH and HA concentration in acidic condition was studied. The results showed that the more Cu2 was removed with the increase of pH and HA concentration, the adsorption rate reached 94.96 when HA concentration reached 1.2 g / L. Because of its large specific surface area, high porosity and pore structure, organometallic frames can be adjusted in drug delivery, heterogeneous catalysis, magnetic materials, optoelectronic materials, photochemical catalysis, Gas adsorption and biosensor are more and more widely used. Using surfactant ionic liquid 4 [C 4N] DS as modifier, calcium metal organic skeleton materials (MOFs) were prepared by hydrothermal method. The results showed that Ca-MOFs nanorods and nanospheres were successfully obtained by changing the conditions. Using Ca-MOFs nanospheres as the carrier, the drug was loaded with nimesulide and sustained release. Ca-MOFs had a special structure and specific surface area, which was beneficial to drug delivery, and could control the sustained release of nimesulide to achieve a better drug effect.
【学位授予单位】：安徽大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ423;TB383.1

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