咪唑类离子液体表面活性剂形成的微乳液的相行为及其应用
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摘要
本论文包括四部分，第一章为绪论；第二章为酸碱盐对CnmimBr形成的W/O微乳液的界面组成、热力学性质及结构参数的影响；第三章为非水微乳液体系C12mimBr/[bmim][BF_4]/正戊醇/正辛烷的相行为和物化性质；第四章为无机盐及合成纳米粒子对W/O微乳液的物化性质和结构参数的影响。
一．绪论
介绍了离子液体和研究微乳液相行为的W/O稀释法，综述了离子液体和非离子表面活性剂Brij-35缔合结构体系的研究进展。对微乳液作为反应介质在纳米合成方面的应用也进行了评述。
二．酸碱盐对CnmimBr形成的W/O微乳液的界面组成、热力学性质及结构参数的影响
用W/O稀释法，研究了CnmimBr/醇/油/盐水W/O型微乳液体系的界面组成、热力学性质及微乳液滴的结构等，探讨了水相中酸碱盐对上述微乳液体系界面组成及结构参数等的影响。
1.离子液体型表面活性剂溴代1-十二烷基-3-甲基咪唑(C12mimBr)、溴代1-十四烷基-3-甲基咪唑(C14mimBr)和溴代1-十六烷基-3-甲基咪唑(C16mimBr)在不同的水相介质中(NaCl, HCl或NaOH)均易于形成W/O型微乳液。
2.不同水相介质(NaCl、HCl或NaOH)对W/O型离子液体微乳液体系的影响规律相同，即随水相介质中酸碱盐浓度的增大，醇在油中的摩尔溶解度X o醇在界面层中的摩尔分数X ia减小，而K和ΔGo
o→i值增大，液滴半径(Rw和Re)增大。
3.不同的水相介质对W/O型微乳液物化参数的影响顺序为：HCl >> NaCl>NaOH (X o
a、X i
a)，NaOH > NaCl >> HCl (ΔGo
o→i、Rw )。以NaOH为水相的体系中的水池半径与以NaCl或HCl为水相的体系比较显著增大。
三.非水微乳液体系C12mimBr/[bmim][BF_4]/正戊醇/正辛烷的相行为和物化性质
对非水微乳液体系C12mimBr/ [bmim][BF_4]/正戊醇/正辛烷的相行为和热力学性质进行了研究，并将其与含水微乳液体系C12mimBr/ H2O/正戊醇/正辛烷进行了比较。
1.当使用不同的亲水相时，单相区区域的大小顺序为H2O< 5% [bmim][BF_4]水溶液<5% NaCl水溶液< [bmim][BF_4]。
2. [bmim][BF_4]微乳液体系的X oa和X ia值总是分别大于水相体系的，IL/O型微乳液形成的自发性小于传统的W/O型微乳液。IL/O微乳液液滴小于传统的W/O型微乳液液滴。
3.随醇碳链长度的增加，IL/O微乳液形成的自发性增强。烷烃对微乳液物化参数的影响与醇的影响相反。即随烷烃碳链长度的增长，体系物化性质的变化规律与随醇碳链长度的增长导致的变化规律不同。
4.盐效应对IL/O微乳液体系的界面组成和结构参数没有明显影响。
5.在较高温度下，IL/O微乳液形成的自发性变小，而W/O型微乳液形成的自发性变大。
四．无机盐及合成纳米粒子对W/O微乳液的物化性质和结构参数的影响
利用W/O稀释法，研究了分别以Na_2CO_3、CaCl2和两种无机盐的混合物为水相，C16mimBr（或Brij35）/正戊醇/正辛烷/水溶液的W/O微乳液体系的界面组成、热力学性质及结构参数等。
考察了在上述微乳液体系中，在不同ωo(水与表面活性剂的摩尔比)及不同Na_2CO_3、CaCl2浓度下，合成纳米粒子CaCO3过程前后，微乳液体系的组成及微乳液滴结构参数的变化。
1.在不同ωo值下，合成CaCO3纳米粒子前后，醇在油相中的摩尔分数Xo均增加，醇在界面膜中的摩尔分数X i
a均减小，ΔG oo→i值均减小，微乳液滴均增大。合成CaCO3纳米粒子后，微乳液液滴的水池半径与Na_2CO_3、CaCl2微乳液体系相比均有所增大。
2.随Na_2CO_3、CaCl2浓度增加，C16mimBr(或Brij35)/正戊醇/正辛烷/水溶液W/O微乳液体系的X oa均减小，X ia、ΔGoo→i均增大，Rw均有所减小。但合成CaCO3纳米粒子后，微乳液液滴的水池半径增大。
3.含水量ωo和Na_2CO_3、CaCl_2浓度对两种微乳液体系的界面组成、热力学性质及结构参数等都有影响，但ωo的影响较之盐浓度的影响要大。
This thesis contains four parts. Chapter I. Introduction；Chapter II. The effects ofNaCl(HCl/NaOH) on the interfacial composition, thermodynamic properties andstructural parameters of the W/O microemulsions formed by CnmimBr. Chapter III.Phase behavior and thermodynamic properties of nonaqueous microemulsion systemscontaining C12mimBr/ [bmim][BF_4]/ pentanol/ n-octane. Chapter IV. Effects ofinorganic salts and synthesized nanoparticles on the physicochemical properties andstructural parameters of W/O microemulsions.
Chapter I. Introduction
The basic knowledge about ionic liquids and the W/O dilution method used toinvestigate the phase behavior of microemulsions were introduced. The researchprogresses of the association structure systems formed by ionic liquids and non-ionicsurfactant Brij35 were revewed. The application of microemulsion systems asreaction media in the synthesis of nanoparticles is also disscussed.
Chapter II. The effects of NaCl(HCl/NaOH) on the interfacialcomposition, thermodynamic properties and structural parameters ofthe W/O microemulsions formed by CnmimBr.
The interfacial composition, thermodynamic properties and structure parameters ofthe W/O microemulsions CnmimBr/ 1-pentanol/ n-octane/ brine with the W/O dilutionmethod. The effects of NaCl (HCl/NaOH) on the above items were discussed.
1. The W/O microemulsions containing surfactant-like ionic liquid 1-dodecyl-3-methylimidazolium bromide (C12mimBr) [or 1-tetradecyl-3-methylimidazoliumbromide (C14mimBr), 1-hexadecyl-3-methylimidazolium bromide (C16mimBr)] areeasier to form (largerΔGoo→ivalues) in different aqueous phases (NaCl, HCl orNaOH).
2. The different aqueous phases (NaCl, HCl or NaOH) have the same influencingtrends on the ionic liquids based W/O microemulsions. That is, both the molesolubility of the alcohol in the oil phaseX oa, and the mole fraction of alcohol at theinterfacial layerX iadecreases, while K andΔGo droplets (Reand Rw) increase with increasing aqueous media concentrations.
3. The physicochemical parameters of the microemulsion systems with differentaqueous phases are in the order HCl>> NaCl> NaOH (X oaandX ia), NaOH > NaCl>> HCl (ΔGoo→iandRw ). The W/O microemulsions have the larger radii of thewater pool with NaOH aqueous phase compared with the systems formed with NaClor HCl aqueous phase.
Chapter III. Phase behavior and thermodynamic properties ofnonaqueous microemulsion systems containing C12mimBr/[bmim][BF_4]/ 1-pentanol/ n-octane
The phase behavior and thermodynamic properties of nonaqueous microemulsionsystems containing C12mimBr/ [bmim][BF_4]/ 1-pentanol/n-octane was studied andcompared with that of aqueous systems containing C12mimBr/ water/ 1-pentanol/n-octane.
1. When different hydrophilic phases are used, the magnitude of the areas of thesingle-phase domain is as follows: pure water< 5% [bmim][BF_4] aqueoussolution<5% NaCl aqueous solution< pure [bmim][BF_4] .
2. BothX oaandX iain [bmim][BF_4] microemulsion systems are always largerthanX oaandX iain H2O systems, respectively. The formation of IL/O microemulsionwas less stable and the droplets of IL/O microemulsions were smaller than theconventional W/O microemulsions.
3. As the carbon chain lengths of the alcohol increases, the formation of IL/Omicroemulsion was increasingly stable. While the pattern of change of all theparameters resulting from different carbon chain lengths of alkanes is in the contraryto the pattern of change resulting from different carbon chain lengths of alcohols.
4. Salinity has no effect on the interfacial composition and structural parametersfor IL/O microemulsion systems.5. At higher temperatures, the IL/O microemulsion was less stable, while theW/O microemulsion was more stable. The radii of the IL/O and W/O microemulsiondroplets decrease as well. Chapter IV. Effects of inorganic salts and synthesized nanoparticleson the physicochemical properties and structural parameters of W/Omicroemulsions.
The effects of Na_2CO_3, CaCl2and the mixture of the two salts as the aqueousphase on the interfacial compositions, thermodynamic properties and structureparameters of the W/O microemulsions C16mimBr (Brij35)/ 1-pentanol/ n-octane/aqueous phase have been investigated.
The changes of the compositions and the structure parameters of the W/Omicroemulsions withωovalue (the molar ratio of water to surfactant) , Na_2CO_3andCaCl2concentrations were investigated. The effect of the reaction between Na_2CO_3and CaCl2to form CaCO3was also discussed.
1. At differentωovalues, the reaction between Na_2CO_3and CaCl2to form CaCO3resuls in the decreases inX oavalues, increases inX ia,ΔG oo→iand the radius of thewater pool. TheRw values of the microemulsion systems containg CaCO3are largerthan that of the systems containg Na_2CO_3or CaCl2.
2. As Na_2CO_3or CaCl2concentration increases,X oadecreases,X iaandΔGoo→iincrease, andRw also decreases, the droplets of the water pool increase with theformation of CaCO3particles for the W/O microemulsion systems of C16mimBr(Brij35)/ 1-pentanol/ n-octane/ aqueous phase.
3.ωovalues, Na_2CO_3and CaCl2concentrations all have effects on the interfacialcomposition, thermodynamic properties and structure parameters of the W/Omicroemulsions. However, the effect ofωois stronger than that of Na_2CO_3andCaCl2concentrations.
一．绪论
介绍了离子液体和研究微乳液相行为的W/O稀释法，综述了离子液体和非离子表面活性剂Brij-35缔合结构体系的研究进展。对微乳液作为反应介质在纳米合成方面的应用也进行了评述。
二．酸碱盐对CnmimBr形成的W/O微乳液的界面组成、热力学性质及结构参数的影响
用W/O稀释法，研究了CnmimBr/醇/油/盐水W/O型微乳液体系的界面组成、热力学性质及微乳液滴的结构等，探讨了水相中酸碱盐对上述微乳液体系界面组成及结构参数等的影响。
1.离子液体型表面活性剂溴代1-十二烷基-3-甲基咪唑(C12mimBr)、溴代1-十四烷基-3-甲基咪唑(C14mimBr)和溴代1-十六烷基-3-甲基咪唑(C16mimBr)在不同的水相介质中(NaCl, HCl或NaOH)均易于形成W/O型微乳液。
2.不同水相介质(NaCl、HCl或NaOH)对W/O型离子液体微乳液体系的影响规律相同，即随水相介质中酸碱盐浓度的增大，醇在油中的摩尔溶解度X o醇在界面层中的摩尔分数X ia减小，而K和ΔGo
o→i值增大，液滴半径(Rw和Re)增大。
3.不同的水相介质对W/O型微乳液物化参数的影响顺序为：HCl >> NaCl>NaOH (X o
a、X i
a)，NaOH > NaCl >> HCl (ΔGo
o→i、Rw )。以NaOH为水相的体系中的水池半径与以NaCl或HCl为水相的体系比较显著增大。
三.非水微乳液体系C12mimBr/[bmim][BF_4]/正戊醇/正辛烷的相行为和物化性质
对非水微乳液体系C12mimBr/ [bmim][BF_4]/正戊醇/正辛烷的相行为和热力学性质进行了研究，并将其与含水微乳液体系C12mimBr/ H2O/正戊醇/正辛烷进行了比较。
1.当使用不同的亲水相时，单相区区域的大小顺序为H2O< 5% [bmim][BF_4]水溶液<5% NaCl水溶液< [bmim][BF_4]。
2. [bmim][BF_4]微乳液体系的X oa和X ia值总是分别大于水相体系的，IL/O型微乳液形成的自发性小于传统的W/O型微乳液。IL/O微乳液液滴小于传统的W/O型微乳液液滴。
3.随醇碳链长度的增加，IL/O微乳液形成的自发性增强。烷烃对微乳液物化参数的影响与醇的影响相反。即随烷烃碳链长度的增长，体系物化性质的变化规律与随醇碳链长度的增长导致的变化规律不同。
4.盐效应对IL/O微乳液体系的界面组成和结构参数没有明显影响。
5.在较高温度下，IL/O微乳液形成的自发性变小，而W/O型微乳液形成的自发性变大。
四．无机盐及合成纳米粒子对W/O微乳液的物化性质和结构参数的影响
利用W/O稀释法，研究了分别以Na_2CO_3、CaCl2和两种无机盐的混合物为水相，C16mimBr（或Brij35）/正戊醇/正辛烷/水溶液的W/O微乳液体系的界面组成、热力学性质及结构参数等。
考察了在上述微乳液体系中，在不同ωo(水与表面活性剂的摩尔比)及不同Na_2CO_3、CaCl2浓度下，合成纳米粒子CaCO3过程前后，微乳液体系的组成及微乳液滴结构参数的变化。
1.在不同ωo值下，合成CaCO3纳米粒子前后，醇在油相中的摩尔分数Xo均增加，醇在界面膜中的摩尔分数X i
a均减小，ΔG oo→i值均减小，微乳液滴均增大。合成CaCO3纳米粒子后，微乳液液滴的水池半径与Na_2CO_3、CaCl2微乳液体系相比均有所增大。
2.随Na_2CO_3、CaCl2浓度增加，C16mimBr(或Brij35)/正戊醇/正辛烷/水溶液W/O微乳液体系的X oa均减小，X ia、ΔGoo→i均增大，Rw均有所减小。但合成CaCO3纳米粒子后，微乳液液滴的水池半径增大。
3.含水量ωo和Na_2CO_3、CaCl_2浓度对两种微乳液体系的界面组成、热力学性质及结构参数等都有影响，但ωo的影响较之盐浓度的影响要大。
This thesis contains four parts. Chapter I. Introduction；Chapter II. The effects ofNaCl(HCl/NaOH) on the interfacial composition, thermodynamic properties andstructural parameters of the W/O microemulsions formed by CnmimBr. Chapter III.Phase behavior and thermodynamic properties of nonaqueous microemulsion systemscontaining C12mimBr/ [bmim][BF_4]/ pentanol/ n-octane. Chapter IV. Effects ofinorganic salts and synthesized nanoparticles on the physicochemical properties andstructural parameters of W/O microemulsions.
Chapter I. Introduction
The basic knowledge about ionic liquids and the W/O dilution method used toinvestigate the phase behavior of microemulsions were introduced. The researchprogresses of the association structure systems formed by ionic liquids and non-ionicsurfactant Brij35 were revewed. The application of microemulsion systems asreaction media in the synthesis of nanoparticles is also disscussed.
Chapter II. The effects of NaCl(HCl/NaOH) on the interfacialcomposition, thermodynamic properties and structural parameters ofthe W/O microemulsions formed by CnmimBr.
The interfacial composition, thermodynamic properties and structure parameters ofthe W/O microemulsions CnmimBr/ 1-pentanol/ n-octane/ brine with the W/O dilutionmethod. The effects of NaCl (HCl/NaOH) on the above items were discussed.
1. The W/O microemulsions containing surfactant-like ionic liquid 1-dodecyl-3-methylimidazolium bromide (C12mimBr) [or 1-tetradecyl-3-methylimidazoliumbromide (C14mimBr), 1-hexadecyl-3-methylimidazolium bromide (C16mimBr)] areeasier to form (largerΔGoo→ivalues) in different aqueous phases (NaCl, HCl orNaOH).
2. The different aqueous phases (NaCl, HCl or NaOH) have the same influencingtrends on the ionic liquids based W/O microemulsions. That is, both the molesolubility of the alcohol in the oil phaseX oa, and the mole fraction of alcohol at theinterfacial layerX iadecreases, while K andΔGo droplets (Reand Rw) increase with increasing aqueous media concentrations.
3. The physicochemical parameters of the microemulsion systems with differentaqueous phases are in the order HCl>> NaCl> NaOH (X oaandX ia), NaOH > NaCl>> HCl (ΔGoo→iandRw ). The W/O microemulsions have the larger radii of thewater pool with NaOH aqueous phase compared with the systems formed with NaClor HCl aqueous phase.
Chapter III. Phase behavior and thermodynamic properties ofnonaqueous microemulsion systems containing C12mimBr/[bmim][BF_4]/ 1-pentanol/ n-octane
The phase behavior and thermodynamic properties of nonaqueous microemulsionsystems containing C12mimBr/ [bmim][BF_4]/ 1-pentanol/n-octane was studied andcompared with that of aqueous systems containing C12mimBr/ water/ 1-pentanol/n-octane.
1. When different hydrophilic phases are used, the magnitude of the areas of thesingle-phase domain is as follows: pure water< 5% [bmim][BF_4] aqueoussolution<5% NaCl aqueous solution< pure [bmim][BF_4] .
2. BothX oaandX iain [bmim][BF_4] microemulsion systems are always largerthanX oaandX iain H2O systems, respectively. The formation of IL/O microemulsionwas less stable and the droplets of IL/O microemulsions were smaller than theconventional W/O microemulsions.
3. As the carbon chain lengths of the alcohol increases, the formation of IL/Omicroemulsion was increasingly stable. While the pattern of change of all theparameters resulting from different carbon chain lengths of alkanes is in the contraryto the pattern of change resulting from different carbon chain lengths of alcohols.
4. Salinity has no effect on the interfacial composition and structural parametersfor IL/O microemulsion systems.5. At higher temperatures, the IL/O microemulsion was less stable, while theW/O microemulsion was more stable. The radii of the IL/O and W/O microemulsiondroplets decrease as well. Chapter IV. Effects of inorganic salts and synthesized nanoparticleson the physicochemical properties and structural parameters of W/Omicroemulsions.
The effects of Na_2CO_3, CaCl2and the mixture of the two salts as the aqueousphase on the interfacial compositions, thermodynamic properties and structureparameters of the W/O microemulsions C16mimBr (Brij35)/ 1-pentanol/ n-octane/aqueous phase have been investigated.
The changes of the compositions and the structure parameters of the W/Omicroemulsions withωovalue (the molar ratio of water to surfactant) , Na_2CO_3andCaCl2concentrations were investigated. The effect of the reaction between Na_2CO_3and CaCl2to form CaCO3was also discussed.
1. At differentωovalues, the reaction between Na_2CO_3and CaCl2to form CaCO3resuls in the decreases inX oavalues, increases inX ia,ΔG oo→iand the radius of thewater pool. TheRw values of the microemulsion systems containg CaCO3are largerthan that of the systems containg Na_2CO_3or CaCl2.
2. As Na_2CO_3or CaCl2concentration increases,X oadecreases,X iaandΔGoo→iincrease, andRw also decreases, the droplets of the water pool increase with theformation of CaCO3particles for the W/O microemulsion systems of C16mimBr(Brij35)/ 1-pentanol/ n-octane/ aqueous phase.
3.ωovalues, Na_2CO_3and CaCl2concentrations all have effects on the interfacialcomposition, thermodynamic properties and structure parameters of the W/Omicroemulsions. However, the effect ofωois stronger than that of Na_2CO_3andCaCl2concentrations.
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