OP-10反相微乳体系的相行为研究及纳米复合碳酸盐的制备
发布时间：2019-04-04 20:27
【摘要】：辛烷基酚聚氧乙烯醚(OP-10)作为非离子表面活性剂,具有优良的匀染、乳化、润湿、扩散,抗静电性能。使用OP-10配制微乳液时需要研究形成的稳定微乳区域范围,以便于为微乳法制备纳米材料提供参考。实验绘制了一系列辛烷基酚聚氧乙烯醚(OP-10)+醇(正丁醇、异戊醇或正辛醇)+环己烷+水(或Ca Cl2水溶液)拟三元微乳体系相图,分别研究了正丁醇,异戊醇,正辛醇的添加比例和氯化钙水溶液浓度对微乳区域的影响,发现在纯水的相图中,随着OP-10和正丁醇,异戊醇或正辛醇的质量比逐渐增大,微乳区域所呈现出的拟三元体系的相对面积先增大,后减小;当OP-10:正丁醇=1.5:1,OP-10:异戊醇=2:1,OP-10:正辛醇=2.5:1时,微乳区相对面积最大。在Ca Cl2水溶液相图中,三种醇微乳区相对面积总体上呈现先增大后减小的变化趋势,且添加不同醇对微乳区相对面积的影响也不同,其中微乳区面积最大时的正丁醇、异戊醇和正辛醇体系所对应的Ca Cl2浓度分别为0.1mol/L、0.5mol/L和0.1mol/L。沉积有金属离子的结晶现象在自然界中随处可见,金属离子能够促使碳酸钙晶体形貌或多或少的发生质变,最具代表性的是金属二价离子,通过实验研究能够在机理上深入发掘其对碳酸钙结晶的影响。在碳酸钙晶体结构中插入钡离子会影响其热稳定性,结晶化过程,进而促使生物和非生物之间的形态发生改变。微乳法通过反应物在微乳液所形成的微型反应器中反应,为制备纳米粒子提供了便利。我们采用相变点观察法研究辛烷基酚聚氧乙烯醚(OP-10)+正辛醇+环己烷+(Ca Cl2/Ba Cl2)的拟三元微乳体系相图,分别配制总浓度为1mol/L的七种不同摩尔比的Ca2+/Ba2+微乳液,并与等摩尔的碳酸钠水溶液反应制备共沉淀碳酸盐,通过使用扫描电镜(SEM)对所制备的七组样品进行表征分析,当为纯钙离子盐时,主要形成大的不完整地立方体颗粒;加入钡离子后,当Ca2+/Ba2+=3:1时,沉淀为立方形、球形聚集体的混合;随着钡离子浓度增加,当Ca2+/Ba2+=2:1时,形成团聚体更多、更大;当Ca2+/Ba2+=1:1和1:2时,部分形成团聚体的同时,伴随有大量的球形小颗粒形成,且Ca2+/Ba2+=1:2时形成聚集体更大;当Ca2+/Ba2+=1:3及纯钡离子盐时,沉淀主要为棒状、不规则多面体。从XRD和FTIR分析来看,随着Ba2+浓度的增加,共沉淀产物Ca CO3逐渐从方解石转变为球霰石,最终形成较为稳定的文石结构。
[Abstract]:Octane phenol polyoxyethylene ether (OP-10), as a non-ionic surfactant, has excellent levelling, emulsifying, wetting, diffusion and antistatic properties. In order to provide a reference for the preparation of nanomaterials by microemulsion method, the stable microemulsion region should be studied when OP-10 is used to prepare microemulsion. A series of pseudo-ternary microemulsion phase diagrams of octane phenol polyoxyethylene ether (OP-10) alcohol (n-butanol, isoamyl alcohol or n-octanol) cyclohexane water (or Ca Cl2 aqueous solution) were drawn. The effects of the addition ratio of n-octanol and the concentration of calcium chloride solution on the microemulsion region were studied. It was found that the mass ratio of n-octanol to n-butanol, isoamyl alcohol or n-octanol gradually increased in the phase diagram of pure water. The relative area of the quasi-ternary system presented by the microemulsion region first increased and then decreased. When OP-10: n-butanol = 1.5 渭 1, op _ (10): isoamyl alcohol = 2: 1, op ~ (10): n-octanol = 2.5: 1, the relative area of microemulsion region is the largest. In the phase diagram of Ca Cl2 aqueous solution, the relative area of the microemulsion region of three kinds of alcohols first increased and then decreased, and the effects of different alcohols on the relative area of the microemulsion region were also different, in which the n-butanol with the largest microemulsion area had different effects on the relative area of the microemulsion region. The corresponding Ca Cl2 concentrations of isoamyl alcohol and n-octanol were 0.1 mol / L, 0.5 mol / L and 0.1 mol / L, respectively. Crystallization of deposited metal ions can be seen everywhere in nature, metal ions can make calcium carbonate crystal morphology more or less qualitative change, the most representative is the metal divalent ion, The effect of calcium carbonate on the crystallization of calcium carbonate can be deeply explored through the experimental study. The addition of barium ions into the crystal structure of calcium carbonate will affect the thermal stability and crystallization process of calcium carbonate, and then promote the morphological change between biological and abiotic species. Through the reaction of reactants in the micro-reactor formed by microemulsion, the microemulsion method provides convenience for the preparation of nano-particles. The phase diagram of octane phenol polyoxyethylene ether (OP-10) octanol cyclohexane (Ca Cl2/Ba Cl2) in pseudo-ternary microemulsion system was studied by phase transition point observation. Seven kinds of Ca2 / Ba2 microemulsions with total concentration of 1mol/L were prepared and co-precipitated carbonate was prepared by reacting with the aqueous solution of sodium carbonate of equal molar ratio. The seven groups of samples were characterized by scanning electron microscopy (SEM) (SEM). When it is pure calcium ion salt, it mainly forms large incomplete cubic particles. With the addition of barium ions, when Ca2 / Ba2 = 3: 1, the precipitates are cubic and spherical aggregates are mixed, and when the concentration of barium ions increases, when Ca2 / Ba2 = 2: 1, more aggregates are formed. When Ca2 / Ba2 = 1:1 and 1: 2, some aggregates were formed, accompanied by a large number of small spherical particles, and Ca2 / Ba2 = 1: 2 formed a larger aggregate. When Ca2 / Ba2 = 1:3 and pure barium ion salt, the precipitation is mainly rod-like and irregular polyhedron. According to XRD and FTIR analysis, with the increase of Ba2 concentration, the co-precipitated product Ca CO3 gradually changed from calcite to aragonite, and finally formed a relatively stable aragonite structure.
【学位授予单位】：兰州交通大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ423.2;TB383.1
本文编号：2454142
[Abstract]:Octane phenol polyoxyethylene ether (OP-10), as a non-ionic surfactant, has excellent levelling, emulsifying, wetting, diffusion and antistatic properties. In order to provide a reference for the preparation of nanomaterials by microemulsion method, the stable microemulsion region should be studied when OP-10 is used to prepare microemulsion. A series of pseudo-ternary microemulsion phase diagrams of octane phenol polyoxyethylene ether (OP-10) alcohol (n-butanol, isoamyl alcohol or n-octanol) cyclohexane water (or Ca Cl2 aqueous solution) were drawn. The effects of the addition ratio of n-octanol and the concentration of calcium chloride solution on the microemulsion region were studied. It was found that the mass ratio of n-octanol to n-butanol, isoamyl alcohol or n-octanol gradually increased in the phase diagram of pure water. The relative area of the quasi-ternary system presented by the microemulsion region first increased and then decreased. When OP-10: n-butanol = 1.5 渭 1, op _ (10): isoamyl alcohol = 2: 1, op ~ (10): n-octanol = 2.5: 1, the relative area of microemulsion region is the largest. In the phase diagram of Ca Cl2 aqueous solution, the relative area of the microemulsion region of three kinds of alcohols first increased and then decreased, and the effects of different alcohols on the relative area of the microemulsion region were also different, in which the n-butanol with the largest microemulsion area had different effects on the relative area of the microemulsion region. The corresponding Ca Cl2 concentrations of isoamyl alcohol and n-octanol were 0.1 mol / L, 0.5 mol / L and 0.1 mol / L, respectively. Crystallization of deposited metal ions can be seen everywhere in nature, metal ions can make calcium carbonate crystal morphology more or less qualitative change, the most representative is the metal divalent ion, The effect of calcium carbonate on the crystallization of calcium carbonate can be deeply explored through the experimental study. The addition of barium ions into the crystal structure of calcium carbonate will affect the thermal stability and crystallization process of calcium carbonate, and then promote the morphological change between biological and abiotic species. Through the reaction of reactants in the micro-reactor formed by microemulsion, the microemulsion method provides convenience for the preparation of nano-particles. The phase diagram of octane phenol polyoxyethylene ether (OP-10) octanol cyclohexane (Ca Cl2/Ba Cl2) in pseudo-ternary microemulsion system was studied by phase transition point observation. Seven kinds of Ca2 / Ba2 microemulsions with total concentration of 1mol/L were prepared and co-precipitated carbonate was prepared by reacting with the aqueous solution of sodium carbonate of equal molar ratio. The seven groups of samples were characterized by scanning electron microscopy (SEM) (SEM). When it is pure calcium ion salt, it mainly forms large incomplete cubic particles. With the addition of barium ions, when Ca2 / Ba2 = 3: 1, the precipitates are cubic and spherical aggregates are mixed, and when the concentration of barium ions increases, when Ca2 / Ba2 = 2: 1, more aggregates are formed. When Ca2 / Ba2 = 1:1 and 1: 2, some aggregates were formed, accompanied by a large number of small spherical particles, and Ca2 / Ba2 = 1: 2 formed a larger aggregate. When Ca2 / Ba2 = 1:3 and pure barium ion salt, the precipitation is mainly rod-like and irregular polyhedron. According to XRD and FTIR analysis, with the increase of Ba2 concentration, the co-precipitated product Ca CO3 gradually changed from calcite to aragonite, and finally formed a relatively stable aragonite structure.
【学位授予单位】：兰州交通大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ423.2;TB383.1
【参考文献】
相关期刊论文 前1条
1 朱福送;杨秀全;白亮;;助表面活性剂对乙草胺微乳液相图的影响[J];精细化工;2010年07期
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