氧化铈复合纳米粒子的非水微乳液制备及其应用性能研究
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摘要
甲醇燃油作为一种清洁燃料已经在我国的山西、陕西、贵州、江苏等省得到了广泛的推广应用。但在甲醇燃油的实际应用中发现：甲醇较高的汽化潜热导致甲醇汽油燃烧温度低,并伴随含甲醛尾气产生；甲醇汽油较低的尾气温度可导致三效催化器对NOx等物质的转化效率下降；对甲醇柴油来说,在降低烟度的同时却增加了甲醇柴油CO、HC、PM等的排放。尽管甲醇燃油具有替代比高、易于推广、经济效益明显等优点,但目前产业界尚无有效方法解决甲醇燃油尾气排放问题。
论文从提高汽车燃油效率、降低有害物排放量角度出发,通过筛选适合的表面活性剂,获得了形成以甲醇/甲酰胺为极性相,正辛烷为非极性相,AE03为表面活性剂的非水微乳液体系；在此基础上研究了前驱物种类、浓度对微乳液相行为的影响规律；最终通过微乳液法制备参杂铜、锆的纳米级的氧化铈,并将之添加到甲醇燃油中,进行了氧化铈复合纳米粒子对90#汽油及M15甲醇汽油的动力性能、燃油经济性能、尾气排放性能的测试,得出了氧化铈复合纳米粒子对燃油尾气排放及动力性的影响规律。本论文主要研究工作及结论如下：
1.与常规微乳液不同,非水微乳液不含水,而是以极性溶剂代替水相形成的具有常规微乳液结构的体系。但目前国内外对非水微乳液研究很少,甚至对非水微乳液是否具有类似常规微乳液的结构都存在争议。论文以甲醇、甲酰胺为极性相,研究了不同类型表面活性剂与正辛烷形成微乳液的规律。在微乳液相图考察基础上,以甲基橙、亚甲基蓝为显色探针,通过紫外-可见吸收光谱研究了AE03/甲醇(甲酰胺)/正辛烷体系的微观结构,确定了该非水体系是一种粒径较小、正辛烷为连续相、甲醇或甲酰胺为分散相的反相微乳液,首次证明了该体系具有与常规含水反相微乳液相同的微结构。
2.以微乳液中纳米级水滴为微反应器合成纳米粒子已经成为当前制备纳米粒子的常规方法,但非水微乳液制备纳米粒子仅有数篇文献报道。尽管非水微乳液具有后处理相对简单、可制备水溶性纳米粒子等优势,但利用非水微乳液制备纳米粒子的一般过程、机理、合成规律均非常缺乏。论文通过电导率、动态光散射等手段首次确定了含有0.075M NaOH和0.025M Ce(NO3)3前驱物的AE03/甲酰胺／正辛烷体系具有典型的油包水微乳液结构,AE03/甲醇／正辛烷体系呈现双连续结构。在此基础上,首次用非水微乳液法制备了氧化铈及参杂铜、锆的氧化铈纳米粒子,并用TEM、XRD等进行了表征。研究结果发现:非水微乳液可以通过与常规微乳液相同的机理形成纳米粒子,微乳液结构将确定纳米粒子的形貌及粒径分布,甲醇、甲酰胺的极性将明显影响纳米粒子形貌。此外,通过研究非水微乳液制备的纳米粒子形貌,进一步证实了甲酰胺微乳液具有类似含水常规微乳液的油包水结构,而甲醇微乳液具有双连续的微结构。
3.与含水的常规微乳液不同,非水微乳液加入甲醇汽油中不会引起相分离。受此启发,论文在甲酰胺非水微乳液中进行了以Ce3+、Cu2+、Zr4+为前驱物的复合纳米粒子合成,仅通过高速离心分离后,以100ppm浓度将该纳米粒子分散于甲醇汽油中,静置30天未发现相分离和沉淀。这一方法避免了含水微乳液制备纳米粒子需要多次洗涤、离心、干燥等步骤,工艺更为简单,具有更好的经济性。为了进一步验证氧化铈复合纳米粒子对甲醇汽油尾气的清洁效果,论文进行了发动机尾气排放测试实验,实验结果显示：在100ppm添加量下,氧化铈、参杂铜的氧化铈、参杂铜、锆的氧化铈纳米粒子可以明显降低90#汽油及M15甲醇汽油的CO、HC、PM、NOx排放；此外,90#汽油及M15甲醇汽油中加入上述纳米粒子后,在发动机高转速下有提高油品动力性能的特点。以上研究结果作为核心技术已成功用于山西艾得成公司的甲醇汽(柴)油产品调制中,并通过山西省科技厅成果鉴定(登记号091206；登记号091207)。上述研究成果及应用已经申请国家发明专利(CN 101591576A),正在实质审核中。
As a clean alternative fuel, methanol gasoline has been widely applied in Shanxi, Shannxi, Guizhou, and Jiangsu provinces. However, some researches found that the higher latent heat of vaporization of methanol induced combustion under low temperature, and the reduction in exhaust gas temperature promoted the emission of formaldehyde. For methanol/diesel fuel, some papers have reported that the emission of CO, HC, and PM was increased while the smoke intensity was decreased. Up to the date, there is no effective solution for the exhaust emission of methanol gasoline.
From the perspective of promoting power efficiency and reducing the exhaust emission, the components of nonaqueous microemulsion was identified. The nonaqueous microemulsion was composed of methanol/ formamide as polar phase, n-octane as oil phase, and AEO3 as surfactant. The effect of concentrations of Ce3+, OH-, Cu2+ and Zr4+ on the microemulsion phase behavior was also investigated. The nanoparticles of cerium oxide with Cu, Zr doping were prepared and applied in 90# gasoline and M15 methanol gasoline. The power performance, fuel economy performance, and the exhause emission of oil with nanoparticles added were investigated by platform experiments. The main results are as follows:
1. Nonaqueous microemulsions with polar nonaqueous solvents replaced the water in the common microemulsion, which have a silimar micro-structrue as that of common microemuslion. Nonaqueous microemulsion were rarely studied, even some researches strongly indicated these polar organic solvent-hydrocarbon dispersions to be molecular solutions without well-defined microemulsion droplets. In the paper, the microemulsion phase diagram and the mechanism of surfactants, methanol/formamide, and n-octane forming microemulsion werer investigated. Moreover, the methyl orange (MO) and methylene blue (MB) were used as absorption probes. The microstructure of nonaqueous microemulsions was probed with uv-vis spectroscopy measurements. The results indicated that an n-octane continuous structure with formamide nano-droplets formed in formamide/AEO3/n-octane system.
2. Microemulsions are thermodynamically stable, transparent and isotropic liquid mediums with nanosized "water pools" dispersed in a continuous phase, which have been widely used to prepare stable colloidal dispersions of different types of nanoparticles. However, there are only few publications on formation of nanoparticles from nonaqueous microemulsions. Although nonaqueous microemulsion showed some advantages on simple post-processing deal, the use in water-sensitive environments, the general process, mechanism, synthesis rules were rarely reported. In the paper, the microstructure of nonaqueous microemulsion containing 0.075M NaOH and 0.025M Ce (NO3)3 were investigated by DLS measurements and conductivity measurements. The results showed that formamide systems have similar microstructure to aqueous microemulsions and bi-continuous structure was shown in methanol system. Moreover, cerium oxide and Zr, Cu doping nanoparticles were synthesized by mixing formamide/AEO3/ n-octaneoil continuous microemulsion containing cerium nitrate and sodium hydroxide. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the phase and morphology of synthesized nanoparticles. It was found that the synthesis mechanism within nonaqueous microemulsions were similar with that of aqueous microemulison. The micro-structure of microemulsion affected the size distribution and the morphology of nanoparticles. The polarity of methanol/formamide influenced the morphology of nanoparticles obviously. Furthermore, the morphology of nanoparticles induced the bi-continuous structure or nano polar solvent pool formed in these nonaqueous systems.
3. As a waterless system, nonaqueous microemulsion could not induce phase separation in methanol gasoline. Inspired by the phenomena, nonaqueous microemulsion was applied to prepare Zr, Cu doping cerium oxide nanoparticle. With the high-speed centrifuge, doping cerium oxide nanoparticles were added in M15 methanol gasoline with 100 ppm for 30 days, and no obvious aggregations were found. This method overcomes the disadvantages of the relatively complicated process in common microemulsions, such as washing, centrifuge, dry and so on, which is a more economic and easy method. Moreover, platform experiments for the 90# gasoline and M15 methanol gasoline with 100 ppm cerium oxide and Zr, Cu doping nanoparticle added were preceded. As the results shown, the content of CO, HC, PM, and NOx in the exhausted emission of 90# gasoline/M15 were markedly decreased with the nanoparticles added. All the gasoline with different additives showed well external characteristics and power performance, and the output torque were promoted at higher engine speed. This technics has been successfully applied in the methanol gasoline production of Shanxi Aidec Science and Technologies Co. as a key technology. The technology progeny has been certificated by the Shanxi science and technology department, and the certificate of identification is domestic advanced level (No.091206; No.091207). Furthermore, the technics has inquiry China Invention Patent (CN 101591576A).
论文从提高汽车燃油效率、降低有害物排放量角度出发,通过筛选适合的表面活性剂,获得了形成以甲醇/甲酰胺为极性相,正辛烷为非极性相,AE03为表面活性剂的非水微乳液体系；在此基础上研究了前驱物种类、浓度对微乳液相行为的影响规律；最终通过微乳液法制备参杂铜、锆的纳米级的氧化铈,并将之添加到甲醇燃油中,进行了氧化铈复合纳米粒子对90#汽油及M15甲醇汽油的动力性能、燃油经济性能、尾气排放性能的测试,得出了氧化铈复合纳米粒子对燃油尾气排放及动力性的影响规律。本论文主要研究工作及结论如下：
1.与常规微乳液不同,非水微乳液不含水,而是以极性溶剂代替水相形成的具有常规微乳液结构的体系。但目前国内外对非水微乳液研究很少,甚至对非水微乳液是否具有类似常规微乳液的结构都存在争议。论文以甲醇、甲酰胺为极性相,研究了不同类型表面活性剂与正辛烷形成微乳液的规律。在微乳液相图考察基础上,以甲基橙、亚甲基蓝为显色探针,通过紫外-可见吸收光谱研究了AE03/甲醇(甲酰胺)/正辛烷体系的微观结构,确定了该非水体系是一种粒径较小、正辛烷为连续相、甲醇或甲酰胺为分散相的反相微乳液,首次证明了该体系具有与常规含水反相微乳液相同的微结构。
2.以微乳液中纳米级水滴为微反应器合成纳米粒子已经成为当前制备纳米粒子的常规方法,但非水微乳液制备纳米粒子仅有数篇文献报道。尽管非水微乳液具有后处理相对简单、可制备水溶性纳米粒子等优势,但利用非水微乳液制备纳米粒子的一般过程、机理、合成规律均非常缺乏。论文通过电导率、动态光散射等手段首次确定了含有0.075M NaOH和0.025M Ce(NO3)3前驱物的AE03/甲酰胺／正辛烷体系具有典型的油包水微乳液结构,AE03/甲醇／正辛烷体系呈现双连续结构。在此基础上,首次用非水微乳液法制备了氧化铈及参杂铜、锆的氧化铈纳米粒子,并用TEM、XRD等进行了表征。研究结果发现:非水微乳液可以通过与常规微乳液相同的机理形成纳米粒子,微乳液结构将确定纳米粒子的形貌及粒径分布,甲醇、甲酰胺的极性将明显影响纳米粒子形貌。此外,通过研究非水微乳液制备的纳米粒子形貌,进一步证实了甲酰胺微乳液具有类似含水常规微乳液的油包水结构,而甲醇微乳液具有双连续的微结构。
3.与含水的常规微乳液不同,非水微乳液加入甲醇汽油中不会引起相分离。受此启发,论文在甲酰胺非水微乳液中进行了以Ce3+、Cu2+、Zr4+为前驱物的复合纳米粒子合成,仅通过高速离心分离后,以100ppm浓度将该纳米粒子分散于甲醇汽油中,静置30天未发现相分离和沉淀。这一方法避免了含水微乳液制备纳米粒子需要多次洗涤、离心、干燥等步骤,工艺更为简单,具有更好的经济性。为了进一步验证氧化铈复合纳米粒子对甲醇汽油尾气的清洁效果,论文进行了发动机尾气排放测试实验,实验结果显示：在100ppm添加量下,氧化铈、参杂铜的氧化铈、参杂铜、锆的氧化铈纳米粒子可以明显降低90#汽油及M15甲醇汽油的CO、HC、PM、NOx排放；此外,90#汽油及M15甲醇汽油中加入上述纳米粒子后,在发动机高转速下有提高油品动力性能的特点。以上研究结果作为核心技术已成功用于山西艾得成公司的甲醇汽(柴)油产品调制中,并通过山西省科技厅成果鉴定(登记号091206；登记号091207)。上述研究成果及应用已经申请国家发明专利(CN 101591576A),正在实质审核中。
As a clean alternative fuel, methanol gasoline has been widely applied in Shanxi, Shannxi, Guizhou, and Jiangsu provinces. However, some researches found that the higher latent heat of vaporization of methanol induced combustion under low temperature, and the reduction in exhaust gas temperature promoted the emission of formaldehyde. For methanol/diesel fuel, some papers have reported that the emission of CO, HC, and PM was increased while the smoke intensity was decreased. Up to the date, there is no effective solution for the exhaust emission of methanol gasoline.
From the perspective of promoting power efficiency and reducing the exhaust emission, the components of nonaqueous microemulsion was identified. The nonaqueous microemulsion was composed of methanol/ formamide as polar phase, n-octane as oil phase, and AEO3 as surfactant. The effect of concentrations of Ce3+, OH-, Cu2+ and Zr4+ on the microemulsion phase behavior was also investigated. The nanoparticles of cerium oxide with Cu, Zr doping were prepared and applied in 90# gasoline and M15 methanol gasoline. The power performance, fuel economy performance, and the exhause emission of oil with nanoparticles added were investigated by platform experiments. The main results are as follows:
1. Nonaqueous microemulsions with polar nonaqueous solvents replaced the water in the common microemulsion, which have a silimar micro-structrue as that of common microemuslion. Nonaqueous microemulsion were rarely studied, even some researches strongly indicated these polar organic solvent-hydrocarbon dispersions to be molecular solutions without well-defined microemulsion droplets. In the paper, the microemulsion phase diagram and the mechanism of surfactants, methanol/formamide, and n-octane forming microemulsion werer investigated. Moreover, the methyl orange (MO) and methylene blue (MB) were used as absorption probes. The microstructure of nonaqueous microemulsions was probed with uv-vis spectroscopy measurements. The results indicated that an n-octane continuous structure with formamide nano-droplets formed in formamide/AEO3/n-octane system.
2. Microemulsions are thermodynamically stable, transparent and isotropic liquid mediums with nanosized "water pools" dispersed in a continuous phase, which have been widely used to prepare stable colloidal dispersions of different types of nanoparticles. However, there are only few publications on formation of nanoparticles from nonaqueous microemulsions. Although nonaqueous microemulsion showed some advantages on simple post-processing deal, the use in water-sensitive environments, the general process, mechanism, synthesis rules were rarely reported. In the paper, the microstructure of nonaqueous microemulsion containing 0.075M NaOH and 0.025M Ce (NO3)3 were investigated by DLS measurements and conductivity measurements. The results showed that formamide systems have similar microstructure to aqueous microemulsions and bi-continuous structure was shown in methanol system. Moreover, cerium oxide and Zr, Cu doping nanoparticles were synthesized by mixing formamide/AEO3/ n-octaneoil continuous microemulsion containing cerium nitrate and sodium hydroxide. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the phase and morphology of synthesized nanoparticles. It was found that the synthesis mechanism within nonaqueous microemulsions were similar with that of aqueous microemulison. The micro-structure of microemulsion affected the size distribution and the morphology of nanoparticles. The polarity of methanol/formamide influenced the morphology of nanoparticles obviously. Furthermore, the morphology of nanoparticles induced the bi-continuous structure or nano polar solvent pool formed in these nonaqueous systems.
3. As a waterless system, nonaqueous microemulsion could not induce phase separation in methanol gasoline. Inspired by the phenomena, nonaqueous microemulsion was applied to prepare Zr, Cu doping cerium oxide nanoparticle. With the high-speed centrifuge, doping cerium oxide nanoparticles were added in M15 methanol gasoline with 100 ppm for 30 days, and no obvious aggregations were found. This method overcomes the disadvantages of the relatively complicated process in common microemulsions, such as washing, centrifuge, dry and so on, which is a more economic and easy method. Moreover, platform experiments for the 90# gasoline and M15 methanol gasoline with 100 ppm cerium oxide and Zr, Cu doping nanoparticle added were preceded. As the results shown, the content of CO, HC, PM, and NOx in the exhausted emission of 90# gasoline/M15 were markedly decreased with the nanoparticles added. All the gasoline with different additives showed well external characteristics and power performance, and the output torque were promoted at higher engine speed. This technics has been successfully applied in the methanol gasoline production of Shanxi Aidec Science and Technologies Co. as a key technology. The technology progeny has been certificated by the Shanxi science and technology department, and the certificate of identification is domestic advanced level (No.091206; No.091207). Furthermore, the technics has inquiry China Invention Patent (CN 101591576A).
引文
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