二元表面活性剂微乳液体系微观结构、性质及在农药药物传递中的应用
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摘要
微乳液是由油(O)、水(W)、表面活性剂(S)和助表面活性剂(CS)组成的有序多元体系,具有较大的界面面积、超低界面张力和热力学稳定等性质。微乳液作为药物载体已广泛应用于农药学等领域。农药微乳剂(micro-emulsion)以水作为分散介质,不用或仅用少量有机溶剂,在表面活性剂的作用下,将油溶性原药以超微细状态(粒径0.01-0.1μm)均匀分散于水中,形成热力学稳定的透明均相体系。由于传统农药剂型乳油中含有大量甲苯、二甲苯等芳香烃有机溶剂,造成环境污染和资源浪费。而以水部分或全部替代乳油中有机溶剂的微乳剂便成了国内外农药新剂型研究的热点。
关于农药微乳剂的形成及稳定,目前一些研究主要集中于配方的筛选,尤其是对微乳液形成的关键组分表面活性剂的使用,仍采用随机或经验法,还没有形成有效的理论。
烷基苯磺酸盐和烷基酚聚氧乙烯醚分别为阴离子表面活性剂和非离子表面活性剂中应用最为广泛的两类表面活性剂,具有优良的润湿及乳化性能。本论文从表面活性剂分子间的相互作用入手,研究了烷基酚聚氧乙烯类型的非离子表面活性剂NP-10及TX-100与烷基苯磺酸盐阴离子表面活性剂SDBA及SDBS在水溶液中形成的混合胶团分子间的相互作用,用正规溶液理论计算它们形成混合胶束组成、分子间相互作用参数。深入研究了复配表面活性剂形成胶团和微乳液的微观结构、相行为及热力学性质,制备了以联苯菊酯、氟硅唑为模型药物的高效载药微乳液。
首先研究了阴离子表面活性剂SDBA、SDBS分别与非离子表面活性剂复配体系的协同效应。用表面张力法测定了复配体系的临界胶束浓度(cmc),根据正规溶液理论计算分子间相互作用参数及分子交换能,研究了分子间的相互作用及热力学性质。结果表明:所有混合体系在胶团和溶液表面的相互作用参数β值(分别为-5.23、-4.88、-2.54、-1.30)均为负值,表明所有复配体系都产生了协同效应。混合胶束热力学研究表明,复配体系的吉布斯自由能?G emx均为负值,|βM|随温度升高变得更大,表明在混合胶束中存在有利的相互作用。在4种混合体系中,两种不同阴离子表面活性剂与同一种非离子表面活性剂NP-10复配时,SDBA+NP-10的协同增效作用比SDBS+NP-10强,即|βaMve(SDBA+NP-10)|>|βaMve(SDBS+ NP-10)|;而对于同一种阴离子表面活性剂SDBA与两种非离子表面活性剂复配时,非离子表面活性剂疏水基链碳原子数越多,|β|越大,即|βaMve(SDBA+NP-10)|>|βaMve(SDBA+TX-100)。说明极性头基之间的静电吸引作用及疏水基分子间的相互作用是产生协同效应的主要原因。电解质NaCl可使复配表面活性剂临界胶束浓度降低,且随NaCl浓度增加,溶液的cmc和γcmc都逐步降低。在复配体系中加入正丁醇比加入碳链较短的乙醇更能明显提高混合表面活性剂降低表面张力的能力和效率。通过采用自旋标记电子自旋共振法(ESR)测定了表面活性剂复配体系形成混合胶团的微环境参数。结果表明:SDBA+NP-10复配体系达到cmc时,微黏度变大,形成混合胶团。微极性参数AN随着非离子表面活性剂的增多而变大,表明有更多的非离子表面活性剂插入到阴离子表面活性剂胶团中,有利于形成胶束。同时以芘为荧光探针、二苯甲酮为猝灭剂,用稳态荧光探针法测得4种单一表面活性剂SDBA、SDBS、NP-10、TX-100的胶团聚集数分别为38.0、34.9、55.3、40.4。不同比例复配体系(SDBA/NP-10、SDBA/TX-100、SDBS/NP-10、SDBS/TX-100)的聚集数都比相应单一阴离子表面活性剂的大,但比单一非离子表面活性剂的小。在阴/非表面活性剂相同比例组成下,4个复配体系聚集数的大小关系是:NSDBA/NP-10> NSDBS/NP-10>NSDBA/TX-100> NSDBS/TX-100。用稳态荧光探针法测得复配体系胶束的微观极性(I1/I3)与ESR法一致。表面活性剂复配协同效应总的结果表明,按一定比例复配后表面活性增强,在降低表面张力的效率、能力和形成胶团能力上均显示协同效应。该结果为表面活性剂的高效复配应用提供了基础数据。
为进一步探讨二元表面活性剂复配体系在形成胶团及微乳液过程中协同效应,本文用介观动力学方法(DPD)模拟了SDBA、NP-10、SDBA+NP-10胶团及微乳液动力学的形成过程,包括胶束结构、水在胶束中的密度分数和界面张力等。发现复配表面活性剂SDBA+NP-10形成胶团的过程中,界面层中SDBA不是均匀地排布,而是其头基聚集成小的团簇,由非离子表面活性剂填充空穴,两者紧密镶嵌,产生协同作用。
为获得二元表面活性剂和助表面活性剂在油相和界面上的组成及微乳液液滴尺寸等微观结构方面的信息,采用稀释法测定了助表面活性剂醇(正丁醇及正戊醇)对SDBA+NP-10/ /正构烷(正己烷或正庚烷)/水(盐水)微乳液体系的界面组成、热力学性质及微观结构的影响。结果表明:助表面活性剂(正丁醇及正戊醇)在油水界面的分布( n ai)和在油相(正己烷及正庚烷)中的分布( na o)的值都是随着油链长的增长而增大,即较高碳链长的正庚烷有利于醇分布在界面。所有体系? G<0,正丁醇和正戊醇从油相转移到界面是自发的,但转移过程中的吉布斯自由能在正庚烷中比在癸烷中更易于自发进行。该微乳液微观结构为随着水含量增加(ω=10-50),Re和Rw均增加,而Rw增加幅度更大,液滴的界面层的有效厚度(dI)呈下降趋势,W/O微乳液体系逐渐转向O/W型微乳体系。
为实现微乳液在农药药物高效传递中的应用,本文以上述二元表面活性剂及助表面活性剂体系作为微乳液的关键组分,研究了联苯菊酯、氟硅唑为模型药物的载药微乳液体系的形成(相行为、微观结构和热力学性质)及应用。结果表明:在SDBA+NP-10/正丁醇/联苯菊酯+环己酮/水载药微乳液体系中,NP-10+SDBA复合表面活性剂较单一非离子表面活性剂形成的O/W微乳区域面积大,温度对该微乳液的相行为影响很小。助表面活性剂醇从分散相进入微乳液界面层的标准自由能变化?Gs<0,随着醇碳链的增长,微乳液形成过程?Gs的绝对值增大,有利于微乳液的形成及微乳区面积增大。微乳液形成过程标准焓变-?Hs=0,为无热效应过程,表明标准自由能的变化?Gs是由醇分子的混乱度熵变?SS决定的。通过偏光、电导率、粘度、折射率等分析手段,确定了该体系形成过程中的微观结构变化:在w(H2O)<32%时,为W/O型,在32%63%时,为O/W型微乳液。由于水溶助长剂可增加有机药物在水中的溶解度,为研制有效成分较高的w(氟硅唑)= 8%微乳剂(ME),考察了5种水溶助长剂对SDBA+NP-10/正丁醇/氟硅唑+环己酮/水载药微乳液体系的影响。结果表明:苯甲酸钠浓度为0.5mol?L-1时,水杨酸钠浓度为0.3mol?L-1时,对药物有增溶作用,并随着水溶助长剂浓度的增大,增溶作用更大。尿素对氟硅唑微乳液体系相行为基本没有影响。间苯二酚、葡萄糖、氯化钠均明显减小了氟硅唑微乳剂单相微乳液区的面积。当w(水杨酸钠)=5%时,配制8%氟硅唑微乳剂热贮稳定性好。室内毒力测定及田间药效试验表明, 2.5%联苯菊酯微乳剂及8%氟硅唑微乳剂均为与环境友好及防效优良的农药药物新制剂。
Microemulsion (ME) is a kind of ordered multi-system, consisting of oil (O), water (W), surfactant (S) and co-surfactant (CS). Because of large interfacial area, ultra-low interfacial tension, and thermodynamic stability, microemulsion has been widely used as drug carrier in agrochemical and other fields. With water as the dispersion medium, microemulsion of agrochemicals can form a thermodynamically stable system. In the microemulsion of agrochemicals, with help of the surfactants, the oil-soluble original drug can be completely disp ersed into water to form ultra-fine particles with size of 0.01-0.1μm. There is few organic solvent in microemulsion of agrochemicals. Usually, agrochemical emulsion includes a lot of aromatic sovent, such as toluene and xylene, causing serious environmental pollution. Nowadays, microemulsion of agrochemicals becomes a worldwide hot topic for the agrochemical new-formulation .Surfactant plays a key role in the formation of microemulsion. However, there is little report about the fundmental investigation of surfactant in the applications of agrochemicals drug delivery.
In this paper, a binary surfactants microemulsion system was prepared by mixing an anionic surfactant and a non-ionic surfactant, and its microstructure、physicochemical properties, and application in agrochemicals drug delivery has been intensively studied. The main achievements are described as follows.
Firstly, two types of alkylbenzene sulfonate, SDBA and SDBS, were selected as anionic surfactants, and two types of alkylphenol ethoxylate, NP-10 and TX-100, were selected as non-ionic surfactants. And then an anionic surfactant was mixed with a non-ionic surfactan to form a binary surfactants system. The mixed critical micelle concentration (CMC) of the binary surfactants system was determined by surface tension measurement. CMC was used to calculate the molecular interaction parameters and molecule-exchanging energy according to regular solution theory of the binary surfactant mixtures. The interaction parameterβvalues in the mixed micelles and air/water interface were measured to be all negative values, indicating that a synergistic effect was produced in all of the mixtures. Thermodynamics investigation of mixed micelles showed that the Gibbs free energy values of all the mixed systems were negative, and |βM | increased with the increasing temperature. It suggested that there existed favorable interactions that improve the micelle formation. When NP-10 was used to mix with SDBA or SDBS, two binary mixtures, SDBA/NP-10 and SDBS/ NP-10, were formed. The |βaMve| of SDBA/NP-10 is larger than that of SDBS/NP-10, which suggested that the synergism interaction of SDBA and NP-10 was stronger than that of SDBS and NP-10. When SDBA was used to mix with NP-10 or TX-100, two binary mixtures, SDBA/NP-10 and SDBS/ TX-100, were formed. The |βaMve| of SDBA/NP-10 is larger than that of SDBS/TX-100. It suggested that the value of |β| was greater when the carbon atom number of the hydrophobic chain of nonionic surfactant was bigger. This synergy phenomenon was caused mailnly by the electrostatic attraction between the polar head groups of the ionic component and the interaction between the hydrophobic molecules.
The critical micelle concentration (cmc) of mixed surfactants was decreased by adding electrolyte, such as NaCl. With increasing concentration of NaCl, the cmc andγcmc were decreased gradually. It was more significant to improve the capacity and efficiency of mixed surfactants in reducing surface tension by adding n-butanol into the mixed system than ethanol.
The micro-environmental parameters of mixed surfactant micelle were determined by electron spin resonance (ESR). When the concentration of the SDBA/NP-10 mixture reached cmc, its microviscosity increased suddently, and then formed mixed micelles. The micropolar parameters AN became bigger with the increasing concentration of non-ionic surfactant. It indicated that more non-ionic surfactant entered into the anionic surfactant micelle, which was helpful for the formation of micelles. At the same time, the aggregation numbers of micelles for four pure surfactants SDBA, SDBS, NP-10 and TX-100 were determined to be 38, 34.9, 40.4, and 55.3 by steady-state fluorescence probe method with pyrene as fluorescence probe and benzophenone as quencher. The aggregation numbers of micelles for the mixed systems (SDBA/NP-10, SDBA/TX-100, SDBS/NP-10, SDBS/TX-100) were all bigger than that of the pure anionic surfactants, but smaller than that of pure non-ionic surfactants. The order of aggregation numbers of the four mixed system was NSDBA/NP-10> NSDBS/NP-10>NSDBA/TX-100> NSDBS/TX-100. The micropolarity of mixed micelles (I1/I3) determined by steady-state fluorescence probe method was agreement with the ESR results. The analysis result showed that there existed a synergistic effect both in the efficiency and ability of reducing the surface tension and forming micelles when two surfactants were mixed with a certain proportion. These results would provide some basic reference for the application of mixed surfactants with high efficiency.
In this paper dissipative particle dynamics (DPD) was applied to simulate the micelle formation process of SDBA, NP-10, and SDBA/NP-10, and the dynamics process of microemulsion, including the structure of micelles, density distribution and fraction of water in the micelles and interfacial tension.
During the micelle formation of mixture of SDBA/NP-10, the SDBA molecules were not evenly arranged, but formed some small clusters through their head groups. The cavities of clusters were filled by TX-100 molecules.
For the microemulsion system of SDBA/NP-10/n-butanol (or amyl alcohol)/n-hexane (or n-heptane)/water (or salt water), the effect of cosurfactant alcohol on the interfacial composition, microstructure and its thermodynamic properties was studied by the dilution method. The distribution of cosurfactant (1-butanol and 1-pentanol) between the oil-water interfacial region (nai) and the continuous oil phase (n-hexane and heptane) (nao) were both increased with the increase of oil’s molecular chain length. The longer carbon chain of oil would improve the dispersion of alcohol in the interface. For all these systems, ?G<0, so it was spontaneous for 1-butanol and1-pentanol to transfer to the interface from the oil phase. However, the transfer process was easier for n-heptane than for n-decane because of the lower Gibbs free energy. The ionic surfactant would give important effect on the W/O microemulsion with the presence of non-ionic surfactant. Both Re and Rw values increased with increasing water content (ω=10-50) in all these surfactant systems. Rw increased more quickly than Re, so the effective thickness of interface layer of liquid drops (dI) tended to decrease. It suggested that the transition from W/O to O/W microemulsion would occur at high water content (ω).
The phase behavior, microstructure and thermodynamic properties of drug-carried microemulsion system (SDBA/ NP-10) /1-butanol / (bifenthrin / cyclohexanone) / water were studied through ternary phase diagram. The results showed that the O/W microemulsion region area of mixed surfactants (NP-10 / SDBA) was larger than that of a single nonionic surfactant, and the temperature had little effect on the phase behavior of microemulsion. The standard free energy change of cosurfactant alcohol transfered into the microemulsion interface layer from the dispersed phase was negative, e.g. ?Gs <0. The absolute value of ?Gs for the process of microemulsion formation increased with the growth of alcohol’s carbon chain, which would improve the formation of microemulsion and increase its area of microemulsion. The standard enthalpy change of microemulsion formation was zero, e.g. -?Hs = 0, which revealed that the process is non-thermal. It indicated that the standard free energy change ?Gs were contributed by the entropy change of the alcohol molecules ?SS. The structure change of the formation process of the system was detected by conductivity, viscosity, refractive index and polarizing microscope. It was a W/O microemulsion system when the mass fraction of water is less than 32 %, e.g. w (H2O) <32%. The liquid crystal structure was formed at 32%63%. The allied toxicity measurement and field efficacy trials results showed that 2.5 wt% bifenthrin microemulsions was an environment-friendly agrochemical formula with long duration of the efficacy.
The influence of several soluble promotors on the (SDBA/NP-10) / butanol / (flusilazole / cyclohexanone) / water system was tested. The results showed that 0.5 mol?L-1 sodium benzoate and 0.3mol?L-1 sodium salicylate could improve the solubility of flusilazole in water, and the solubility increased with the increase of the two hydrotrope concentration. The effect of urea on the phase behavior of flusilazole microemulsion was insignificant. Resorcinol, glucose and sodium chloride reduced noticably the flusilazole microemulsion zones of the ternary phase diagram. 8wt% flusilazole microemulsion prepared by 5 wt% sodium salicylate showed good heat storage stability. The allied toxicity measurement and field efficacy trials results showed that 8 wt% flusilazole microemulsions had great control effect against pear scab, indicating that it was an environmentally friendly fungicide.
关于农药微乳剂的形成及稳定,目前一些研究主要集中于配方的筛选,尤其是对微乳液形成的关键组分表面活性剂的使用,仍采用随机或经验法,还没有形成有效的理论。
烷基苯磺酸盐和烷基酚聚氧乙烯醚分别为阴离子表面活性剂和非离子表面活性剂中应用最为广泛的两类表面活性剂,具有优良的润湿及乳化性能。本论文从表面活性剂分子间的相互作用入手,研究了烷基酚聚氧乙烯类型的非离子表面活性剂NP-10及TX-100与烷基苯磺酸盐阴离子表面活性剂SDBA及SDBS在水溶液中形成的混合胶团分子间的相互作用,用正规溶液理论计算它们形成混合胶束组成、分子间相互作用参数。深入研究了复配表面活性剂形成胶团和微乳液的微观结构、相行为及热力学性质,制备了以联苯菊酯、氟硅唑为模型药物的高效载药微乳液。
首先研究了阴离子表面活性剂SDBA、SDBS分别与非离子表面活性剂复配体系的协同效应。用表面张力法测定了复配体系的临界胶束浓度(cmc),根据正规溶液理论计算分子间相互作用参数及分子交换能,研究了分子间的相互作用及热力学性质。结果表明:所有混合体系在胶团和溶液表面的相互作用参数β值(分别为-5.23、-4.88、-2.54、-1.30)均为负值,表明所有复配体系都产生了协同效应。混合胶束热力学研究表明,复配体系的吉布斯自由能?G emx均为负值,|βM|随温度升高变得更大,表明在混合胶束中存在有利的相互作用。在4种混合体系中,两种不同阴离子表面活性剂与同一种非离子表面活性剂NP-10复配时,SDBA+NP-10的协同增效作用比SDBS+NP-10强,即|βaMve(SDBA+NP-10)|>|βaMve(SDBS+ NP-10)|;而对于同一种阴离子表面活性剂SDBA与两种非离子表面活性剂复配时,非离子表面活性剂疏水基链碳原子数越多,|β|越大,即|βaMve(SDBA+NP-10)|>|βaMve(SDBA+TX-100)。说明极性头基之间的静电吸引作用及疏水基分子间的相互作用是产生协同效应的主要原因。电解质NaCl可使复配表面活性剂临界胶束浓度降低,且随NaCl浓度增加,溶液的cmc和γcmc都逐步降低。在复配体系中加入正丁醇比加入碳链较短的乙醇更能明显提高混合表面活性剂降低表面张力的能力和效率。通过采用自旋标记电子自旋共振法(ESR)测定了表面活性剂复配体系形成混合胶团的微环境参数。结果表明:SDBA+NP-10复配体系达到cmc时,微黏度变大,形成混合胶团。微极性参数AN随着非离子表面活性剂的增多而变大,表明有更多的非离子表面活性剂插入到阴离子表面活性剂胶团中,有利于形成胶束。同时以芘为荧光探针、二苯甲酮为猝灭剂,用稳态荧光探针法测得4种单一表面活性剂SDBA、SDBS、NP-10、TX-100的胶团聚集数分别为38.0、34.9、55.3、40.4。不同比例复配体系(SDBA/NP-10、SDBA/TX-100、SDBS/NP-10、SDBS/TX-100)的聚集数都比相应单一阴离子表面活性剂的大,但比单一非离子表面活性剂的小。在阴/非表面活性剂相同比例组成下,4个复配体系聚集数的大小关系是:NSDBA/NP-10> NSDBS/NP-10>NSDBA/TX-100> NSDBS/TX-100。用稳态荧光探针法测得复配体系胶束的微观极性(I1/I3)与ESR法一致。表面活性剂复配协同效应总的结果表明,按一定比例复配后表面活性增强,在降低表面张力的效率、能力和形成胶团能力上均显示协同效应。该结果为表面活性剂的高效复配应用提供了基础数据。
为进一步探讨二元表面活性剂复配体系在形成胶团及微乳液过程中协同效应,本文用介观动力学方法(DPD)模拟了SDBA、NP-10、SDBA+NP-10胶团及微乳液动力学的形成过程,包括胶束结构、水在胶束中的密度分数和界面张力等。发现复配表面活性剂SDBA+NP-10形成胶团的过程中,界面层中SDBA不是均匀地排布,而是其头基聚集成小的团簇,由非离子表面活性剂填充空穴,两者紧密镶嵌,产生协同作用。
为获得二元表面活性剂和助表面活性剂在油相和界面上的组成及微乳液液滴尺寸等微观结构方面的信息,采用稀释法测定了助表面活性剂醇(正丁醇及正戊醇)对SDBA+NP-10/ /正构烷(正己烷或正庚烷)/水(盐水)微乳液体系的界面组成、热力学性质及微观结构的影响。结果表明:助表面活性剂(正丁醇及正戊醇)在油水界面的分布( n ai)和在油相(正己烷及正庚烷)中的分布( na o)的值都是随着油链长的增长而增大,即较高碳链长的正庚烷有利于醇分布在界面。所有体系? G<0,正丁醇和正戊醇从油相转移到界面是自发的,但转移过程中的吉布斯自由能在正庚烷中比在癸烷中更易于自发进行。该微乳液微观结构为随着水含量增加(ω=10-50),Re和Rw均增加,而Rw增加幅度更大,液滴的界面层的有效厚度(dI)呈下降趋势,W/O微乳液体系逐渐转向O/W型微乳体系。
为实现微乳液在农药药物高效传递中的应用,本文以上述二元表面活性剂及助表面活性剂体系作为微乳液的关键组分,研究了联苯菊酯、氟硅唑为模型药物的载药微乳液体系的形成(相行为、微观结构和热力学性质)及应用。结果表明:在SDBA+NP-10/正丁醇/联苯菊酯+环己酮/水载药微乳液体系中,NP-10+SDBA复合表面活性剂较单一非离子表面活性剂形成的O/W微乳区域面积大,温度对该微乳液的相行为影响很小。助表面活性剂醇从分散相进入微乳液界面层的标准自由能变化?Gs<0,随着醇碳链的增长,微乳液形成过程?Gs的绝对值增大,有利于微乳液的形成及微乳区面积增大。微乳液形成过程标准焓变-?Hs=0,为无热效应过程,表明标准自由能的变化?Gs是由醇分子的混乱度熵变?SS决定的。通过偏光、电导率、粘度、折射率等分析手段,确定了该体系形成过程中的微观结构变化:在w(H2O)<32%时,为W/O型,在32%
Microemulsion (ME) is a kind of ordered multi-system, consisting of oil (O), water (W), surfactant (S) and co-surfactant (CS). Because of large interfacial area, ultra-low interfacial tension, and thermodynamic stability, microemulsion has been widely used as drug carrier in agrochemical and other fields. With water as the dispersion medium, microemulsion of agrochemicals can form a thermodynamically stable system. In the microemulsion of agrochemicals, with help of the surfactants, the oil-soluble original drug can be completely disp ersed into water to form ultra-fine particles with size of 0.01-0.1μm. There is few organic solvent in microemulsion of agrochemicals. Usually, agrochemical emulsion includes a lot of aromatic sovent, such as toluene and xylene, causing serious environmental pollution. Nowadays, microemulsion of agrochemicals becomes a worldwide hot topic for the agrochemical new-formulation .Surfactant plays a key role in the formation of microemulsion. However, there is little report about the fundmental investigation of surfactant in the applications of agrochemicals drug delivery.
In this paper, a binary surfactants microemulsion system was prepared by mixing an anionic surfactant and a non-ionic surfactant, and its microstructure、physicochemical properties, and application in agrochemicals drug delivery has been intensively studied. The main achievements are described as follows.
Firstly, two types of alkylbenzene sulfonate, SDBA and SDBS, were selected as anionic surfactants, and two types of alkylphenol ethoxylate, NP-10 and TX-100, were selected as non-ionic surfactants. And then an anionic surfactant was mixed with a non-ionic surfactan to form a binary surfactants system. The mixed critical micelle concentration (CMC) of the binary surfactants system was determined by surface tension measurement. CMC was used to calculate the molecular interaction parameters and molecule-exchanging energy according to regular solution theory of the binary surfactant mixtures. The interaction parameterβvalues in the mixed micelles and air/water interface were measured to be all negative values, indicating that a synergistic effect was produced in all of the mixtures. Thermodynamics investigation of mixed micelles showed that the Gibbs free energy values of all the mixed systems were negative, and |βM | increased with the increasing temperature. It suggested that there existed favorable interactions that improve the micelle formation. When NP-10 was used to mix with SDBA or SDBS, two binary mixtures, SDBA/NP-10 and SDBS/ NP-10, were formed. The |βaMve| of SDBA/NP-10 is larger than that of SDBS/NP-10, which suggested that the synergism interaction of SDBA and NP-10 was stronger than that of SDBS and NP-10. When SDBA was used to mix with NP-10 or TX-100, two binary mixtures, SDBA/NP-10 and SDBS/ TX-100, were formed. The |βaMve| of SDBA/NP-10 is larger than that of SDBS/TX-100. It suggested that the value of |β| was greater when the carbon atom number of the hydrophobic chain of nonionic surfactant was bigger. This synergy phenomenon was caused mailnly by the electrostatic attraction between the polar head groups of the ionic component and the interaction between the hydrophobic molecules.
The critical micelle concentration (cmc) of mixed surfactants was decreased by adding electrolyte, such as NaCl. With increasing concentration of NaCl, the cmc andγcmc were decreased gradually. It was more significant to improve the capacity and efficiency of mixed surfactants in reducing surface tension by adding n-butanol into the mixed system than ethanol.
The micro-environmental parameters of mixed surfactant micelle were determined by electron spin resonance (ESR). When the concentration of the SDBA/NP-10 mixture reached cmc, its microviscosity increased suddently, and then formed mixed micelles. The micropolar parameters AN became bigger with the increasing concentration of non-ionic surfactant. It indicated that more non-ionic surfactant entered into the anionic surfactant micelle, which was helpful for the formation of micelles. At the same time, the aggregation numbers of micelles for four pure surfactants SDBA, SDBS, NP-10 and TX-100 were determined to be 38, 34.9, 40.4, and 55.3 by steady-state fluorescence probe method with pyrene as fluorescence probe and benzophenone as quencher. The aggregation numbers of micelles for the mixed systems (SDBA/NP-10, SDBA/TX-100, SDBS/NP-10, SDBS/TX-100) were all bigger than that of the pure anionic surfactants, but smaller than that of pure non-ionic surfactants. The order of aggregation numbers of the four mixed system was NSDBA/NP-10> NSDBS/NP-10>NSDBA/TX-100> NSDBS/TX-100. The micropolarity of mixed micelles (I1/I3) determined by steady-state fluorescence probe method was agreement with the ESR results. The analysis result showed that there existed a synergistic effect both in the efficiency and ability of reducing the surface tension and forming micelles when two surfactants were mixed with a certain proportion. These results would provide some basic reference for the application of mixed surfactants with high efficiency.
In this paper dissipative particle dynamics (DPD) was applied to simulate the micelle formation process of SDBA, NP-10, and SDBA/NP-10, and the dynamics process of microemulsion, including the structure of micelles, density distribution and fraction of water in the micelles and interfacial tension.
During the micelle formation of mixture of SDBA/NP-10, the SDBA molecules were not evenly arranged, but formed some small clusters through their head groups. The cavities of clusters were filled by TX-100 molecules.
For the microemulsion system of SDBA/NP-10/n-butanol (or amyl alcohol)/n-hexane (or n-heptane)/water (or salt water), the effect of cosurfactant alcohol on the interfacial composition, microstructure and its thermodynamic properties was studied by the dilution method. The distribution of cosurfactant (1-butanol and 1-pentanol) between the oil-water interfacial region (nai) and the continuous oil phase (n-hexane and heptane) (nao) were both increased with the increase of oil’s molecular chain length. The longer carbon chain of oil would improve the dispersion of alcohol in the interface. For all these systems, ?G<0, so it was spontaneous for 1-butanol and1-pentanol to transfer to the interface from the oil phase. However, the transfer process was easier for n-heptane than for n-decane because of the lower Gibbs free energy. The ionic surfactant would give important effect on the W/O microemulsion with the presence of non-ionic surfactant. Both Re and Rw values increased with increasing water content (ω=10-50) in all these surfactant systems. Rw increased more quickly than Re, so the effective thickness of interface layer of liquid drops (dI) tended to decrease. It suggested that the transition from W/O to O/W microemulsion would occur at high water content (ω).
The phase behavior, microstructure and thermodynamic properties of drug-carried microemulsion system (SDBA/ NP-10) /1-butanol / (bifenthrin / cyclohexanone) / water were studied through ternary phase diagram. The results showed that the O/W microemulsion region area of mixed surfactants (NP-10 / SDBA) was larger than that of a single nonionic surfactant, and the temperature had little effect on the phase behavior of microemulsion. The standard free energy change of cosurfactant alcohol transfered into the microemulsion interface layer from the dispersed phase was negative, e.g. ?Gs <0. The absolute value of ?Gs for the process of microemulsion formation increased with the growth of alcohol’s carbon chain, which would improve the formation of microemulsion and increase its area of microemulsion. The standard enthalpy change of microemulsion formation was zero, e.g. -?Hs = 0, which revealed that the process is non-thermal. It indicated that the standard free energy change ?Gs were contributed by the entropy change of the alcohol molecules ?SS. The structure change of the formation process of the system was detected by conductivity, viscosity, refractive index and polarizing microscope. It was a W/O microemulsion system when the mass fraction of water is less than 32 %, e.g. w (H2O) <32%. The liquid crystal structure was formed at 32%
The influence of several soluble promotors on the (SDBA/NP-10) / butanol / (flusilazole / cyclohexanone) / water system was tested. The results showed that 0.5 mol?L-1 sodium benzoate and 0.3mol?L-1 sodium salicylate could improve the solubility of flusilazole in water, and the solubility increased with the increase of the two hydrotrope concentration. The effect of urea on the phase behavior of flusilazole microemulsion was insignificant. Resorcinol, glucose and sodium chloride reduced noticably the flusilazole microemulsion zones of the ternary phase diagram. 8wt% flusilazole microemulsion prepared by 5 wt% sodium salicylate showed good heat storage stability. The allied toxicity measurement and field efficacy trials results showed that 8 wt% flusilazole microemulsions had great control effect against pear scab, indicating that it was an environmentally friendly fungicide.
引文
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