C_2～C_4醇类燃料的热解及低温等离子体研究
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摘要
本论文利用同步辐射真空紫外单光子电离、分子束取样和反射式时间质谱相结合的技术，详细地研究生物质醇类燃料(C_2～C_4醇)的热解反应及低温等离子体放电反应。
在第一章中，首先阐述了开展生物质燃料热解研究的重要性和必要性。简要介绍了一些与热解相关的概念。综述和评价了热解研究中的实验方法，与其它的热解诊断方法相比较，分子束质谱结合可调的真空紫外光电离技术有更多的优点，这包括：高的信噪比、软电离以及在很宽的范围内连续可调的光子能量。这些优点将有利于热解反应中各物种的鉴定和浓度测量。
在第二章中，主要介绍了热解研究所用的实验装置。首先介绍了同步辐射的优点和特点，国家同步辐射实验室储存环和U10和U14C的结构性能和相关参数，并介绍了U14C光束线新增加的气体滤波器。然后，描述了实验站的工作原理和实验程序。最后，简单介绍热解研究中用到的一些理论计算方法。
在第三章中，我们研究了低压条件下的乙醇热解反应：(1)通过测量和分析热解产物的光电离效率谱，鉴定了稳定的生成物和不稳定的自由基，并区分了它们的同分异构体。产物包括H_2、CH_3、CH_4、H2_O、C_2H_2、C_2H_4、CO、H_2CO、C_3H_4、C_2H_2O、C_2H_4O、C_2H_4O、C_4H_6和C_4H_8；(2)通过选择合适的光子能量以保证近阈值电离，测量了每一种产物随温度变化的曲线，从而推导出了它们的摩尔分数曲线；(3)用G383的方法对乙醇解离通道和消耗反应路径进行了理论计算，结合实验数据，详细分析了热解产物的生成机理。
在第四章中，我们讨论了低压条件下的C_3系列醇——正／异丙醇的热解反应，并结合理论计算结果，详细分析了产物的形成机理。并概括了正／异丙醇热解反应的异同点。总体来看，两者的“同”在于：在低温时，以母体脱H_2O生成丙烯的反应为主；在高温时，自由基参与的分解反应及其引发的链式反应占主导地位；至于H_2消去和CH_4消去反应，与母体解离反应及自由基参与反应相竞争。至于两者热解产物的种类不同，浓度不同，出现温度和最高浓度对应温度的不同，理论计算给出了合理的解释。归根到底，这些不同的原因是由热解母体正／异丙醇的结构的不同所致，特别是与羟基的位置有直接关系。
在第五章中，我们探测了低压条件下的C_4系列醇——正／仲／异／叔丁醇的热解反应：确定了热解产物的具体结构，推导出了它们的摩尔分数曲线。并结合G3B3的理论计算结果，讨论了热解产物的反应通道。同时比较了四种丁醇中产生的热解产物及其形成机理的异同点。结果表明：比较容易产生的物质来自于热解的初级反应，包括四元环消去反应和直接的母体解离反应；由热解初级反应产生的热解产物的种类不同，浓度不同，出现温度和最高摩尔分数对应的温度的不同，是由热解母体丁醇的结构所致；而由二次及多次反应生成的物质往往比较相似，与母体丁醇的结构关系不大。
在第六章中，我们利用低温等离子体条件模拟星际等离子体环境，特别是恒星形成区域的热核环境，并将同步辐射单光子电离技术作为一种等离子体化学诊断的新方法，在醇类物质的等离子体介质阻挡放电过程中探测到了C_2至C_4系列的烯醇。研究发现，放电过程中产生的烯醇及其醛类和酮类的同分异结构体与醇类母体在分子结构上，特别是碳链中羟基的位置上具有很强的关联性。这表明烯醇等不饱和含氧有机分子可以由醇类物质直接在等离子体环境中产生，结合近年来在星际环境中对乙烯醇及醇类物质的检测，可以推断出更大的烯醇——丙烯醇和丁烯醇在星际环境中存在的可能性。这些实验结果对判断星际物质中新的化学分子及其生成途径有重要的指导意义。
In this dissertation, the pyrolysis and cold plasma discharges of biomass fuels, including C_2, C_3 and C_4 alcohols, have been investigated by the tunable synchrotron vacuum ultraviolet (VUV) photoionization combined with molecular-beam mass spectrometry (MBMS).
In the first chapter, the importance and necessity of pyrolysis studies of biomass fuels are described. Some basic concepts related to pyrolysis are briefly introduced. The development of the experimental methods on pyrolysis diagnostic technology is reviewed and evaluated. The advantages of tunable synchrotron VUV photoionization combined with molecular beam mass spectrometry offer significant improvements over previous methods, which are superior signal-to-noise, soft ionization, and tunability of photon energy for isomeric identification of complex pyrolysis products.
In Chapter 2, the experiment setup of pyrolysis is introduced in detail. Firstly, the advantages of synchrotron radiation light source, the parameters of storage ring of National Synchrotron Radiation Laboratory (NSRL) and the structures of U10 and U14C beamlines are presented. Secondly, the operation principle of the endstation and the experimental procedures are described. Finally, the theoretical methods used in this thesis are briefly introduced.
In Chapter 3, the pyrolysis study of ethanol at low pressure is presented in detail. Products Observed from ethanol pyrolysis, including H_2、CH_3、CH_4、H_2O、C_2H_2、C_2H_4、CO、H_2CO、C_3H_4、C_2H_2O、C_2H_4O、C_2H_4O、C_4H_6 and C_4H_8, are identified unambiguously by measurements of photoionization efficiency spectra. Mole fraction profiles of these pyrolysis species are measured at the selective photon energies near ionization thresholds. The dissociation channels and consumption reactions of ethanol are calculated by ab initio Gaussian-3 (G3) procedure. The experimental results are in good agreement with theoretical predictions
Pyrolysis of C_3 alcohols (1-propanol and 2-propanol) has been studied in Chapter 4. The formation pathways of pyrolysis species are investigated with the help of G3B3 method. In general, the decomposition of the two precursors occurs primarily by the dehydration reaction at low temperature, and the production of radicals becomes dominant and the decomposition reaction is controlled by chain processes at high temperature. Different types of H_2- and CH_4-molecular elimination processes are involved in radical reactions. The pyrolysis species in the two systems are strongly affected by the structures of their precursors, especially the position of OH in 1-/2-propanol.
Pyrolysis studies of C_4 alcohols including 1-butanol, 2-butanol, i-butanol and t-butanol at low pressure have been reported in Chapter 5. The identification of reaction species, the measurements of mole fraction and the theoretical calculations of decomposition pathways are discussed in detail. The species produced by primary reactions have a strong relationship with the structures of pyrolysis precursors, while the species generated by the secondary reactions are independent of the butanol structures. The dissociation mechanisms of the butanols include complex fission, simple fission and H-atom abstraction, which are in roughly good agreement with previous results.
In the last chapter, low-pressure cold plasma discharges, which are used to simulate some hot core environments in the star-forming region, have been investigated by employing single-photon vacuum ultraviolet photoionization mass spectrometry. Enols with two to four carbon atoms are detected in plasma discharges of alcohols, indicating that enols can result from alcohol destructions induced by ultraviolet and cosmic radiation and accelerated electrons that are abundant in the interstellar medium. This observation, together with the detection of ethenol toward Sgr B2, suggests that larger enols, such as propenols and butenols, could be in the search list of potential molecular species to be identified in interstellar space. The laboratorial effort presented here shows that VUV photoionization sampling of plasma discharges is a potential method for understanding new interstellar molecules and their formation mechanisms.
在第一章中，首先阐述了开展生物质燃料热解研究的重要性和必要性。简要介绍了一些与热解相关的概念。综述和评价了热解研究中的实验方法，与其它的热解诊断方法相比较，分子束质谱结合可调的真空紫外光电离技术有更多的优点，这包括：高的信噪比、软电离以及在很宽的范围内连续可调的光子能量。这些优点将有利于热解反应中各物种的鉴定和浓度测量。
在第二章中，主要介绍了热解研究所用的实验装置。首先介绍了同步辐射的优点和特点，国家同步辐射实验室储存环和U10和U14C的结构性能和相关参数，并介绍了U14C光束线新增加的气体滤波器。然后，描述了实验站的工作原理和实验程序。最后，简单介绍热解研究中用到的一些理论计算方法。
在第三章中，我们研究了低压条件下的乙醇热解反应：(1)通过测量和分析热解产物的光电离效率谱，鉴定了稳定的生成物和不稳定的自由基，并区分了它们的同分异构体。产物包括H_2、CH_3、CH_4、H2_O、C_2H_2、C_2H_4、CO、H_2CO、C_3H_4、C_2H_2O、C_2H_4O、C_2H_4O、C_4H_6和C_4H_8；(2)通过选择合适的光子能量以保证近阈值电离，测量了每一种产物随温度变化的曲线，从而推导出了它们的摩尔分数曲线；(3)用G383的方法对乙醇解离通道和消耗反应路径进行了理论计算，结合实验数据，详细分析了热解产物的生成机理。
在第四章中，我们讨论了低压条件下的C_3系列醇——正／异丙醇的热解反应，并结合理论计算结果，详细分析了产物的形成机理。并概括了正／异丙醇热解反应的异同点。总体来看，两者的“同”在于：在低温时，以母体脱H_2O生成丙烯的反应为主；在高温时，自由基参与的分解反应及其引发的链式反应占主导地位；至于H_2消去和CH_4消去反应，与母体解离反应及自由基参与反应相竞争。至于两者热解产物的种类不同，浓度不同，出现温度和最高浓度对应温度的不同，理论计算给出了合理的解释。归根到底，这些不同的原因是由热解母体正／异丙醇的结构的不同所致，特别是与羟基的位置有直接关系。
在第五章中，我们探测了低压条件下的C_4系列醇——正／仲／异／叔丁醇的热解反应：确定了热解产物的具体结构，推导出了它们的摩尔分数曲线。并结合G3B3的理论计算结果，讨论了热解产物的反应通道。同时比较了四种丁醇中产生的热解产物及其形成机理的异同点。结果表明：比较容易产生的物质来自于热解的初级反应，包括四元环消去反应和直接的母体解离反应；由热解初级反应产生的热解产物的种类不同，浓度不同，出现温度和最高摩尔分数对应的温度的不同，是由热解母体丁醇的结构所致；而由二次及多次反应生成的物质往往比较相似，与母体丁醇的结构关系不大。
在第六章中，我们利用低温等离子体条件模拟星际等离子体环境，特别是恒星形成区域的热核环境，并将同步辐射单光子电离技术作为一种等离子体化学诊断的新方法，在醇类物质的等离子体介质阻挡放电过程中探测到了C_2至C_4系列的烯醇。研究发现，放电过程中产生的烯醇及其醛类和酮类的同分异结构体与醇类母体在分子结构上，特别是碳链中羟基的位置上具有很强的关联性。这表明烯醇等不饱和含氧有机分子可以由醇类物质直接在等离子体环境中产生，结合近年来在星际环境中对乙烯醇及醇类物质的检测，可以推断出更大的烯醇——丙烯醇和丁烯醇在星际环境中存在的可能性。这些实验结果对判断星际物质中新的化学分子及其生成途径有重要的指导意义。
In this dissertation, the pyrolysis and cold plasma discharges of biomass fuels, including C_2, C_3 and C_4 alcohols, have been investigated by the tunable synchrotron vacuum ultraviolet (VUV) photoionization combined with molecular-beam mass spectrometry (MBMS).
In the first chapter, the importance and necessity of pyrolysis studies of biomass fuels are described. Some basic concepts related to pyrolysis are briefly introduced. The development of the experimental methods on pyrolysis diagnostic technology is reviewed and evaluated. The advantages of tunable synchrotron VUV photoionization combined with molecular beam mass spectrometry offer significant improvements over previous methods, which are superior signal-to-noise, soft ionization, and tunability of photon energy for isomeric identification of complex pyrolysis products.
In Chapter 2, the experiment setup of pyrolysis is introduced in detail. Firstly, the advantages of synchrotron radiation light source, the parameters of storage ring of National Synchrotron Radiation Laboratory (NSRL) and the structures of U10 and U14C beamlines are presented. Secondly, the operation principle of the endstation and the experimental procedures are described. Finally, the theoretical methods used in this thesis are briefly introduced.
In Chapter 3, the pyrolysis study of ethanol at low pressure is presented in detail. Products Observed from ethanol pyrolysis, including H_2、CH_3、CH_4、H_2O、C_2H_2、C_2H_4、CO、H_2CO、C_3H_4、C_2H_2O、C_2H_4O、C_2H_4O、C_4H_6 and C_4H_8, are identified unambiguously by measurements of photoionization efficiency spectra. Mole fraction profiles of these pyrolysis species are measured at the selective photon energies near ionization thresholds. The dissociation channels and consumption reactions of ethanol are calculated by ab initio Gaussian-3 (G3) procedure. The experimental results are in good agreement with theoretical predictions
Pyrolysis of C_3 alcohols (1-propanol and 2-propanol) has been studied in Chapter 4. The formation pathways of pyrolysis species are investigated with the help of G3B3 method. In general, the decomposition of the two precursors occurs primarily by the dehydration reaction at low temperature, and the production of radicals becomes dominant and the decomposition reaction is controlled by chain processes at high temperature. Different types of H_2- and CH_4-molecular elimination processes are involved in radical reactions. The pyrolysis species in the two systems are strongly affected by the structures of their precursors, especially the position of OH in 1-/2-propanol.
Pyrolysis studies of C_4 alcohols including 1-butanol, 2-butanol, i-butanol and t-butanol at low pressure have been reported in Chapter 5. The identification of reaction species, the measurements of mole fraction and the theoretical calculations of decomposition pathways are discussed in detail. The species produced by primary reactions have a strong relationship with the structures of pyrolysis precursors, while the species generated by the secondary reactions are independent of the butanol structures. The dissociation mechanisms of the butanols include complex fission, simple fission and H-atom abstraction, which are in roughly good agreement with previous results.
In the last chapter, low-pressure cold plasma discharges, which are used to simulate some hot core environments in the star-forming region, have been investigated by employing single-photon vacuum ultraviolet photoionization mass spectrometry. Enols with two to four carbon atoms are detected in plasma discharges of alcohols, indicating that enols can result from alcohol destructions induced by ultraviolet and cosmic radiation and accelerated electrons that are abundant in the interstellar medium. This observation, together with the detection of ethenol toward Sgr B2, suggests that larger enols, such as propenols and butenols, could be in the search list of potential molecular species to be identified in interstellar space. The laboratorial effort presented here shows that VUV photoionization sampling of plasma discharges is a potential method for understanding new interstellar molecules and their formation mechanisms.
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