超细煤粉O_2/CO_2燃烧及NOx异相还原机理
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摘要
随着社会的发展,生态环境越来越受到人们的重视,如今人类正面临着三大环境问题的困扰:温室效应、酸雨和臭氧层破坏。后二者均已爆发过严重的环境危机,如1952年的英国伦敦烟雾酸雨事件、美国洛杉矶烟雾事件和南极臭氧层空洞,因此早在20世纪60、70年代就引起了国际社会的重视,至今已发展了一系列卓有成效的控制和减排技术与措施。但化石燃料尤其是煤燃烧过程排放的大量二氧化碳造成的温室效应近年来才引起了各国的普遍重视。许多控制CO_2排放的技术应运而生。其中O_2/CO_2燃烧技术是一种行之有效且性价比较高的综合控制污染物排放的新型洁净燃烧技术。本文提出的超细煤粉O_2/CO_2燃烧技术将超细煤粉应用于传统的O_2/CO_2燃烧技术,试图将两者的优点结合起来以达到扬长补短的效果,进一步发展成为既拥有良好的燃烧性质,又具有较好的污染物排放性能的煤粉燃烧新技术,研究成果可为新一轮的高效低污染燃烧设备的开发提供技术支撑,甚至有可能成为一种值得大力推广的污染物协同脱除的新兴技术。本论文主要采用热显微镜、热天平、固定床试验台和携带流综合燃烧试验台,结合X射线光电子能谱仪(XPS)和量子化学计算软件,对超细煤粉/焦表面性质和超细煤粉在O_2/CO_2气氛中热解和燃烧过程、污染物排放特性以及NO异相还原机理等关键问题,进行了一系列探索性的研究。
机械力化学效应在无机物制备领域不仅是一个研究热点,而且已得到应用;但在煤研究领域却鲜有研究或报道。本文第一章对超细煤粉粉磨过程中机械力化学效应进行了研究,利用XPS对超细煤粉表面的元素种类和碳、氮、氧和硫元素存在形态进行了测试和分析,得到了它们随粒径变化的规律,可为粉碎理论和超细煤粉表面化学特性提供参考。结果表明机械力化学作用对不同元素作用的程度不同。
热解过程是煤转化过程的初级阶段,对其进行深入研究有助于增进对煤的利用过程如燃烧、气化、液化等的理解。为此在固定床试验台上进行了超细煤粉CO_2气氛中的热解试验,研究了煤种、煤粉粒度和温度对超细煤粉在高浓度CO_2下的热解气体成分的影响,并分析了它们的生成机理。结果显示煤中氮主要以NH3、HCN和N2O形式析出,N2O的生成与NO的存在以及CO_2气氛有较大关系;热解气氛、温度和粒径对于CO析出的影响都较大。
了解燃烧特性是燃料利用的前提和基础。本文分别在热显微镜和高温热天平中研究了超细煤粉在O_2/CO_2气氛中的着火和燃烧特性。在改装的热显微镜系统中观察和分析了超细煤粉在O_2/CO_2气氛中着火形态和火焰特征,揭示了气氛、煤粉粒径、氧气流量和氧气浓度等参数对着火的影响规律。试验发现在所设定的条件下,煤柱在N2/O_2中比在CO_2/O_2中更容易着火,火焰更明显。煤粉粒径会影响着火方式;实验条件下,平均粒径为33.68μm的煤粉是均相着火方式,而平均粒径低于20μm的煤粉都是非均相着火。在热重试验中,采用非等温热重分析方法,详细分析了煤粉粒径、升温速率、气氛和氧气含量等因素对细化和超细化煤粉在O_2/CO_2气氛中燃烧的影响。结果表明:氧气浓度对超细煤粉在O_2/CO_2气氛中的燃烧性能影响最大;煤粉平均粒径越小,煤粉的燃烧性能也越好;升温速率的增大在氧气浓度较高时对于煤粉燃烧性能的提升作用较明显。
为进一步了解超细煤粉在O_2/CO_2气氛中燃烧的特点和污染物的析出特性,设计、建成了一个能够较好地模拟燃烧过程的携带流综合燃烧试验台。通过试验得出了煤粉粒度、炉膛温度和过量空气系数、循环NOx以及气氛等因素对CO_2、CO气体和NOx排放的影响规律,对它们的影响机理进行了分析。采用灰色关联方法对过氧系数、煤粉粒径、温度和循环NO浓度等4个因素对5种烟气成分(CO_2,CO,N2O,NO和NO)和氮转化率的关联度进行了排序,结果发现循环NO浓度只对NO_2影响较明显,铁法烟煤的其他三种对各种母因素的影响都比较明显,而内蒙古煤稍有不同,过氧系数和温度对CO_2、NO和氮转化率的影响比较明显而粒径对CO_2、CO和氮转化率影响比较明显。
超细煤粉在高浓度CO_2气氛中热解过程中煤粉/焦表面氮官能团的变化对于理解煤粉在O_2/CO_2气氛中热解、燃烧时氮元素的转化过程有重要参考作用,也可为后续的量子化学模拟提供参考。本文在固定床试验台上在高浓度CO_2气体中制取了不同温度下的煤焦,并对它们进行了XPS测试,得到了NO在高浓度CO_2气氛下与煤焦异相反应的重要信息。基于试验结果,以密度泛函理论和有机反应理论为基础,本文从微观角度对超细煤粉在O_2/CO_2气氛中NO异相还原机理进行了研究。提出了气化/燃烧过程的简化煤焦模型,计算了小分子在超细煤焦表面吸附和NO在气化煤焦表面吸附的热力学、结构参数和吸附选择性,发现气体分子在煤焦表面倾向于以分子整体或部分在两个活性点之间侧向平行方式吸附;未气化煤焦表面有利于NO的吸附而气化煤焦表面相对不利。以反应热和布居数分析为基础,进一步详细分析了异相还原反应通道的各个反应步骤,最后确定出可能的NO异相还原的反应机理,可为煤粉在O_2/CO_2气氛中燃烧过程中NOx转化机理提供参考。
With the development of the society, more and more attention has been paid to ecological environment. Nowadays, mankind is facing three serious environmental problems: greenhouse effect, acid rain and ozone depletion. The latter two have ever caused serious environmental crisis, such as the London smog rain event in 1952,Los Angeles smog event and Antarctic ozone hole which have aroused the attention of the international community during the 60s and 70s of 20th century. From then on, a series of effective technologies and measures for control and reduction of pollutant have been developed. However, the greenhouse effect, caused by emission of carbon dioxide from fossil fuel combustion especially coal combustion, has gained attention and credibility in recent years. Many technologies for controlling CO_2 emission are developing, among which O_2/CO_2 combustion technology is an effective, high cost-effective, highly competitive comprehensive clean combustion technology. Superfine pulverized coal O_2/CO_2 combustion technology is proposed in the paper which applies superfine pulverized coal to the traditional O_2/CO_2 combustion technology. We attempt to combine the advantages of both in order to achieve good combustion properties and lower pollutant emission. The research results could provide technical support for a new round of research and design of high efficiency and low combustion equipments and might become a new widely promoting technology for simultaneous removal of contaminants.
A series of exploratory studies have been conducted on many key issues concerning superfine pulverized coal O_2/CO_2 combustion technology. Surface properties of superfine coal/char, the pyrolysis and combustion process of superfine coal in O_2/CO_2, pollutants emission characteristics and NO heterogeneous reduction mechanism have been studied using hot stage microscope, thermogravimetric analysis(TGA), fixed-bed reactor bench and entrained flow comprehensive combustion bench combined with X-ray photoelectron spectroscopy(XPS) and quantum chemistry calculation software.
Mechanochemical effect is not only a research focus, but also has been applied in inorganic preparation. However, there are few reports in coal research field. The mechanochemical effect during the grinding process was studied in the first chapter. The element types,the functionalities of carbon, nitrogen, oxygen and sulfur on coal surface and their variations with coal particle size have been tested and analyzed using X-ray photoelectron spectroscopy (XPS). The results showed that mechanical force have different effects on different elements. The research could enrich the comminution theory and surface chemical characteristics of superfine pulverized coal.
Pyrolysis is the initial stage of coal conversion process. Therefore a thorough study on pyrolysis helps to understand coal utilization processes such as combustion, gasification, liquefaction. Pyrolysis experiment of superfine pulverized coal in CO_2 using the fixed bed reactor bench were carried out. Moreover, the effects of coal type, particle size and temperature on the evolved gas composition and the gas release mechanism were analyzed. The results showed that nitrogen in coal evolves mainly in the forms of NH3, HCN and N2O while the occurrence of N2O and NO are closely related to the existence of CO_2 atmosphere. The atmosphere, temperature and coal particle size have great influence on the release of CO.
A deep insight into the combustion characteristics of fossil fuel provides the prerequisite and basis for their usage. The ignition and combustion characteristics of superfine pulverized coal were investigated using a thermogravimetry and a hot stage microscopy. Ignition flame characteristics of superfine pulverized coal in the O_2/CO_2 atmosphere have been observed using a hot stage microscope attaching a camera. The effects of atmosphere, particle size, oxygen flow rate and oxygen concentration on the ignition characteristics of micro-pulverized coal were analyzed. It is found that it is easier for coal to ignite in N2/O_2 mixture than in CO_2/O_2 mixture and for the coals particle size above 20μm, the ignition process become more violent for the volatile matter evolves intensively. Particle size of coal affects the ignition mode. Homogeneous ignition occurred in the case of 33.68μm while heterogeneous ignition took place in the cases of lower than 20μm. On the thermogravimetry the effects of oxygen concentration, particle size and heating rate on the coal combustion characteristics under O_2/CO_2 atmosphere were analyzed. The results indicated that oxygen concentration played the most important role. As the particle size decreases, the ignition and burnout temperatures decrease while the comprehensive combustion index S increases. Higher oxygen concentration helps to promote the effect of heating rate.
An entrained flow comprehensive combustion test bench has been designed and built to further study the combustion and emission characteristics of superfine pulverized coal in the O_2/CO_2 atmosphere. The effects of particle size, furnace temperature, stoichiometric ratio, recycled NOx on the CO_2, CO and NOx emissions have been analyzed. Grey correlation method has been applied to calculate and sort the relation degrees of the factors over the gases CO_2, CO, N2O, NO_2 and NO and nitrogen conversion rate. The results indicated that the concentration of recycled NO only have apparent impact on the formation of NO_2 .Other three factors have great influence on the gases and nitrogen conversion rate for Tiefa bituminous coal while it is slightly different for Neimenggu coal. Furnace temperature and stoichiometric ratio have obvious influence on CO_2 and NO concentrations and nitrogen conversion rate while particle size has apparent influence on CO_2 and CO concentrations and nitrogen conversion rate.
The variations of functional groups on the surface of superfine pulverized coal/char during pyrolysis in CO_2 atmosphere promote the understanding of the conversion process of the functional groups during pyrolysis and combustion in the O_2/CO_2 atmosphere and it is also an important reference to the simulation of quantum chemistry. We have acquired coal char in the high concentration of CO_2 at different temperatures on the fixed bed reactor. Afterwards, XPS tests have been conducted to reveal the variations of the functional groups of coal/char at different stages of pyrolysis.The heterogeneous mechanism of NO reduction during superfine pulverized coal O_2/CO_2 combustion has been investigated from a microscopic view based on the experimental results and combined with the density functional theory and organic reaction theory. Simplified models of coal char during gasification and combustion have been proposed and the thermodynamic, structural parameters and adsorption selectivity of adsorption process of small molecules the surfaces of coal char and coal char during gasification. It is found that small gas molecules tend to wholly or partly adsorb onto the char surfaces between two active sites in a side parallel way. The ungasified coal char surface is more favorable of NO adsorption than the coal char during gasification. On the basis of reaction heat and population analysis, heterogeneous reduction reaction steps and pathways are further analyzed in detail and finally the NO heterogeneous reduction mechanism is concluded which could provide a reference for the conversion of NOx in the oxy-fuel combustion process.
机械力化学效应在无机物制备领域不仅是一个研究热点,而且已得到应用;但在煤研究领域却鲜有研究或报道。本文第一章对超细煤粉粉磨过程中机械力化学效应进行了研究,利用XPS对超细煤粉表面的元素种类和碳、氮、氧和硫元素存在形态进行了测试和分析,得到了它们随粒径变化的规律,可为粉碎理论和超细煤粉表面化学特性提供参考。结果表明机械力化学作用对不同元素作用的程度不同。
热解过程是煤转化过程的初级阶段,对其进行深入研究有助于增进对煤的利用过程如燃烧、气化、液化等的理解。为此在固定床试验台上进行了超细煤粉CO_2气氛中的热解试验,研究了煤种、煤粉粒度和温度对超细煤粉在高浓度CO_2下的热解气体成分的影响,并分析了它们的生成机理。结果显示煤中氮主要以NH3、HCN和N2O形式析出,N2O的生成与NO的存在以及CO_2气氛有较大关系;热解气氛、温度和粒径对于CO析出的影响都较大。
了解燃烧特性是燃料利用的前提和基础。本文分别在热显微镜和高温热天平中研究了超细煤粉在O_2/CO_2气氛中的着火和燃烧特性。在改装的热显微镜系统中观察和分析了超细煤粉在O_2/CO_2气氛中着火形态和火焰特征,揭示了气氛、煤粉粒径、氧气流量和氧气浓度等参数对着火的影响规律。试验发现在所设定的条件下,煤柱在N2/O_2中比在CO_2/O_2中更容易着火,火焰更明显。煤粉粒径会影响着火方式;实验条件下,平均粒径为33.68μm的煤粉是均相着火方式,而平均粒径低于20μm的煤粉都是非均相着火。在热重试验中,采用非等温热重分析方法,详细分析了煤粉粒径、升温速率、气氛和氧气含量等因素对细化和超细化煤粉在O_2/CO_2气氛中燃烧的影响。结果表明:氧气浓度对超细煤粉在O_2/CO_2气氛中的燃烧性能影响最大;煤粉平均粒径越小,煤粉的燃烧性能也越好;升温速率的增大在氧气浓度较高时对于煤粉燃烧性能的提升作用较明显。
为进一步了解超细煤粉在O_2/CO_2气氛中燃烧的特点和污染物的析出特性,设计、建成了一个能够较好地模拟燃烧过程的携带流综合燃烧试验台。通过试验得出了煤粉粒度、炉膛温度和过量空气系数、循环NOx以及气氛等因素对CO_2、CO气体和NOx排放的影响规律,对它们的影响机理进行了分析。采用灰色关联方法对过氧系数、煤粉粒径、温度和循环NO浓度等4个因素对5种烟气成分(CO_2,CO,N2O,NO和NO)和氮转化率的关联度进行了排序,结果发现循环NO浓度只对NO_2影响较明显,铁法烟煤的其他三种对各种母因素的影响都比较明显,而内蒙古煤稍有不同,过氧系数和温度对CO_2、NO和氮转化率的影响比较明显而粒径对CO_2、CO和氮转化率影响比较明显。
超细煤粉在高浓度CO_2气氛中热解过程中煤粉/焦表面氮官能团的变化对于理解煤粉在O_2/CO_2气氛中热解、燃烧时氮元素的转化过程有重要参考作用,也可为后续的量子化学模拟提供参考。本文在固定床试验台上在高浓度CO_2气体中制取了不同温度下的煤焦,并对它们进行了XPS测试,得到了NO在高浓度CO_2气氛下与煤焦异相反应的重要信息。基于试验结果,以密度泛函理论和有机反应理论为基础,本文从微观角度对超细煤粉在O_2/CO_2气氛中NO异相还原机理进行了研究。提出了气化/燃烧过程的简化煤焦模型,计算了小分子在超细煤焦表面吸附和NO在气化煤焦表面吸附的热力学、结构参数和吸附选择性,发现气体分子在煤焦表面倾向于以分子整体或部分在两个活性点之间侧向平行方式吸附;未气化煤焦表面有利于NO的吸附而气化煤焦表面相对不利。以反应热和布居数分析为基础,进一步详细分析了异相还原反应通道的各个反应步骤,最后确定出可能的NO异相还原的反应机理,可为煤粉在O_2/CO_2气氛中燃烧过程中NOx转化机理提供参考。
With the development of the society, more and more attention has been paid to ecological environment. Nowadays, mankind is facing three serious environmental problems: greenhouse effect, acid rain and ozone depletion. The latter two have ever caused serious environmental crisis, such as the London smog rain event in 1952,Los Angeles smog event and Antarctic ozone hole which have aroused the attention of the international community during the 60s and 70s of 20th century. From then on, a series of effective technologies and measures for control and reduction of pollutant have been developed. However, the greenhouse effect, caused by emission of carbon dioxide from fossil fuel combustion especially coal combustion, has gained attention and credibility in recent years. Many technologies for controlling CO_2 emission are developing, among which O_2/CO_2 combustion technology is an effective, high cost-effective, highly competitive comprehensive clean combustion technology. Superfine pulverized coal O_2/CO_2 combustion technology is proposed in the paper which applies superfine pulverized coal to the traditional O_2/CO_2 combustion technology. We attempt to combine the advantages of both in order to achieve good combustion properties and lower pollutant emission. The research results could provide technical support for a new round of research and design of high efficiency and low combustion equipments and might become a new widely promoting technology for simultaneous removal of contaminants.
A series of exploratory studies have been conducted on many key issues concerning superfine pulverized coal O_2/CO_2 combustion technology. Surface properties of superfine coal/char, the pyrolysis and combustion process of superfine coal in O_2/CO_2, pollutants emission characteristics and NO heterogeneous reduction mechanism have been studied using hot stage microscope, thermogravimetric analysis(TGA), fixed-bed reactor bench and entrained flow comprehensive combustion bench combined with X-ray photoelectron spectroscopy(XPS) and quantum chemistry calculation software.
Mechanochemical effect is not only a research focus, but also has been applied in inorganic preparation. However, there are few reports in coal research field. The mechanochemical effect during the grinding process was studied in the first chapter. The element types,the functionalities of carbon, nitrogen, oxygen and sulfur on coal surface and their variations with coal particle size have been tested and analyzed using X-ray photoelectron spectroscopy (XPS). The results showed that mechanical force have different effects on different elements. The research could enrich the comminution theory and surface chemical characteristics of superfine pulverized coal.
Pyrolysis is the initial stage of coal conversion process. Therefore a thorough study on pyrolysis helps to understand coal utilization processes such as combustion, gasification, liquefaction. Pyrolysis experiment of superfine pulverized coal in CO_2 using the fixed bed reactor bench were carried out. Moreover, the effects of coal type, particle size and temperature on the evolved gas composition and the gas release mechanism were analyzed. The results showed that nitrogen in coal evolves mainly in the forms of NH3, HCN and N2O while the occurrence of N2O and NO are closely related to the existence of CO_2 atmosphere. The atmosphere, temperature and coal particle size have great influence on the release of CO.
A deep insight into the combustion characteristics of fossil fuel provides the prerequisite and basis for their usage. The ignition and combustion characteristics of superfine pulverized coal were investigated using a thermogravimetry and a hot stage microscopy. Ignition flame characteristics of superfine pulverized coal in the O_2/CO_2 atmosphere have been observed using a hot stage microscope attaching a camera. The effects of atmosphere, particle size, oxygen flow rate and oxygen concentration on the ignition characteristics of micro-pulverized coal were analyzed. It is found that it is easier for coal to ignite in N2/O_2 mixture than in CO_2/O_2 mixture and for the coals particle size above 20μm, the ignition process become more violent for the volatile matter evolves intensively. Particle size of coal affects the ignition mode. Homogeneous ignition occurred in the case of 33.68μm while heterogeneous ignition took place in the cases of lower than 20μm. On the thermogravimetry the effects of oxygen concentration, particle size and heating rate on the coal combustion characteristics under O_2/CO_2 atmosphere were analyzed. The results indicated that oxygen concentration played the most important role. As the particle size decreases, the ignition and burnout temperatures decrease while the comprehensive combustion index S increases. Higher oxygen concentration helps to promote the effect of heating rate.
An entrained flow comprehensive combustion test bench has been designed and built to further study the combustion and emission characteristics of superfine pulverized coal in the O_2/CO_2 atmosphere. The effects of particle size, furnace temperature, stoichiometric ratio, recycled NOx on the CO_2, CO and NOx emissions have been analyzed. Grey correlation method has been applied to calculate and sort the relation degrees of the factors over the gases CO_2, CO, N2O, NO_2 and NO and nitrogen conversion rate. The results indicated that the concentration of recycled NO only have apparent impact on the formation of NO_2 .Other three factors have great influence on the gases and nitrogen conversion rate for Tiefa bituminous coal while it is slightly different for Neimenggu coal. Furnace temperature and stoichiometric ratio have obvious influence on CO_2 and NO concentrations and nitrogen conversion rate while particle size has apparent influence on CO_2 and CO concentrations and nitrogen conversion rate.
The variations of functional groups on the surface of superfine pulverized coal/char during pyrolysis in CO_2 atmosphere promote the understanding of the conversion process of the functional groups during pyrolysis and combustion in the O_2/CO_2 atmosphere and it is also an important reference to the simulation of quantum chemistry. We have acquired coal char in the high concentration of CO_2 at different temperatures on the fixed bed reactor. Afterwards, XPS tests have been conducted to reveal the variations of the functional groups of coal/char at different stages of pyrolysis.The heterogeneous mechanism of NO reduction during superfine pulverized coal O_2/CO_2 combustion has been investigated from a microscopic view based on the experimental results and combined with the density functional theory and organic reaction theory. Simplified models of coal char during gasification and combustion have been proposed and the thermodynamic, structural parameters and adsorption selectivity of adsorption process of small molecules the surfaces of coal char and coal char during gasification. It is found that small gas molecules tend to wholly or partly adsorb onto the char surfaces between two active sites in a side parallel way. The ungasified coal char surface is more favorable of NO adsorption than the coal char during gasification. On the basis of reaction heat and population analysis, heterogeneous reduction reaction steps and pathways are further analyzed in detail and finally the NO heterogeneous reduction mechanism is concluded which could provide a reference for the conversion of NOx in the oxy-fuel combustion process.
引文
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