低阶煤热解半焦的气化反应特性研究
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摘要
流化床煤气化技术因气化条件温和和气化强度大等诸多优点而受到广泛关注。虽然流化床气化炉的工艺和结构在不断改进,但由于反应器内化学反应十分复杂,反应调控机理仍不太清楚。飞灰含碳量高、气化效率偏低等问题还需要继续开展大量细致的实验研究工作才能得到解决。如果直接在流化床反应器上进行试验摸索,由于操作复杂、实验数据少、重复性差,将花费大量的时间和精力。因此,如果能运用现代精密仪器技术,在接近流化床内的反应条件下获取煤热解气化动力学数据,通过影响因素和动力学分析确定原料的煤气化活性,为操作参数的优化配置提供参考依据,对流化床气化具有非常重要的理论意义和现实指导意义。
本论文在接近流化床条件下,研究了低阶煤的快速热解特性以及煤焦气化活性,综合分析了煤种特性和反应条件对气化活性的影响,并对比研究了实验室制焦与流化床热解炉底渣、气化炉飞灰之间的结构差异和反应性差异。
采用热重-质谱(TG-MS)联用技术研究了不同煤种的程序升温热解特性和气体产物释放规律,并在接近流化床热解炉操作温度范围内,采用快速热解装置制备快速热解煤焦,研究了煤的快速热解特性以及不同热解条件下煤焦的形态结构。
采用热重分析技术研究了气化温度、制焦温度、热解速率等条件分别对煤焦-水蒸气和煤焦-CO2气化活性的影响。结果表明,在本研究采用的实验条件下,热解条件中以热解速率对煤焦气化活性影响较大,制焦温度和制焦停留时间的影响相对较小。温度条件中,煤焦气化反应速率主要受气化温度的影响,制焦温度影响相对较小。随着气化温度增加,煤焦的反应性指数和最大反应速率近似线性增长。煤焦-CO2和煤焦-水蒸气气化的活化能都随着碳转化率的升高而增加。
采用七种不同煤化程度的原煤进行煤焦制备和气化活性测试,总结了普遍适用的规律：碳转化率达到50%对应的比气化速率与相同反应条件下的平均比气化速率在数值上近似相等；灰分的行为对煤焦气化活性有非常重要的影响,它在不同反应阶段和不同气化温度下作用不同,这是由于灰分组成和含量的变化导致的；煤焦孔结构对气化活性的影响在越温和的反应条件下越突出,但煤焦气化活性高低与初始孔结构没有直接关系；煤焦-C02和煤焦-水蒸气气化的相对活性比率随着气化温度的升高而降低,表明高温条件可以缩小煤焦在这两种气氛中活性差距。
对比研究了水平管式炉快速热解煤焦、鼓泡床煤焦、流化床热解炉煤焦表面形貌和结构及其对气化活性的影响。采用不同活性指标进行比较,发现在制焦温度相同或近似时,水平管式炉快速热解煤焦、鼓泡床热解煤焦和循环流化床热解煤焦活性指标之间存在近似线性关系。制焦过程传热传质越剧烈,煤焦孔结构越丰富,晶格有序化程度越低,气化活性越高。
以流化床气化炉旋风分离器出口飞灰样品为研究对象,对比研究气化炉飞灰样品与实验室水平管式炉快速热解煤焦结构及反应性差异。XRD测试结果表明,实验室快速热解煤焦的缩核芳核尺度比飞灰大,且有序化程度比飞灰高。分别采用N2和CO2作为吸附剂煤焦和飞灰的比表面积,结果表明飞灰的孔结构以大孔和过渡孔为主,而快速热解煤焦的孔结构以微孔为主。孔结构的差异导致飞灰的CO2气化活性高于快速热解煤焦,但是水蒸气气化活性比快速热解煤焦低。
根据本论文的研究结果,建立了适用于流化床气化炉的煤种气化活性评价方法,其中涉及样品预处理、快速热解煤焦制备、煤焦气化等一系列标准化实验和分析流程。
The technology of coal gasification in fluidized bed is extensively concerned due to its mild gasification conditions and large gasification intensity. Although the process and structure of fluidized bed gasifier is improved continuously, the regulation mechanism is still unclear because of the complicated chemical reactions in the reactor. A series experiments needs to be carried out in order to solve the problems of high carbon content in fly ash and low gasification efficiency. It will take a lot of time and effort to conduct experiments directly in the fluidized bed reactors because of the complex operations, inadequate data and poor reproducibility. Therefore, it is theoretically and practically significant to study coal pyrolysis and gasification properties in the conditions closing to fluidized bed reactor with modern precision instruments technology. Then the kinetic data can be obtained, and the gasification reactivity of raw coal can be determined by influence factors analysis and dynamics analysis, which provides the important reference for optimizing operation parameters.
In this dissertation, the fast pyrolysis characteristics of low rank coal and gasification reactivity of char at the conditions closing to fluidized bed reactors are investigated. The effects of coal characteristics and reaction conditions on gasification reactivity are analyzed, and the differences in structure and reactivity among the laboratory-prepared fast pyrolysis char, bottom slag and gasifer fly ash of the fluidized bed pyrolysis furnaces are compared.
Characteristics of pyrolysis process and gas products during temperature-programmed pyrolysis of different coals are analyzed with thermogravimetric-mass spectrometry (TG-MS). Fast pyrolysis device is used to prepare fast pyrolysis char at the temperatures close to fluidized bed operating temperatures. The fast pyrolysis characteristics of coal and the char morphology under different pyrolysis conditions are studied.
Contrastive study on the reactivity of the chars gasification with steam and CO2, respectively, is conducted by thermogravimetric technology. The effects of gasification temperature, pyrolysis temperature and pyrolysis rate on gasification reactivity of the chars are investigated. Under the experimental condition, the results show that pyrolysis rate greatly affects gasification reactivity, however the effects of pyrolysis temperature and residence time are relatively small. In the temperature conditions, gasification temperature is the most important factor influencing gasification rate, while the effect of pyrolysis temperature is weaker. The reactivity index and the maximum reaction rate changes linearly with the increase in gasification temperature. The activation energy of both char-CO2and char-steam gasification increases with increase in carbon conversion rate.
Seven types of coals with different coal ranks are used for char preparation and gasification reactivity test, and some conclusions are obtained. It is found that the value of half reaction specific rate is approximate to the average specific rate under the same conditions. Ash behavior plays an important role in the char reactivity, and changes with gasification temperature and reaction degree due to the variation in the compositions and relative amount. The influence of pore structure is more noticeable during a relatively moderate reaction process, but the gasification reactivity of char has no immediate connection with the initial pore structure. The relative gasification reactivity ratio of char-steam to char-CO2generally decreases with the increasing temperature, indicating that high temperature can reduce the reactivity gap between the two reactions.
The surface morphology and structure of the chars from fast pyrolysis in the horizontal tube furnace, a bubbling bed and a fluidized bed are compared, and its effect on gasification reactivity is discussed. Different indicators are used to evaluate the gasification reactivity of the chars, and it is found that there is a linear relationship between the indicators of the chars from different reactors. The more intense of the heat and mass transfer process is, the more orderly of the crystal lattice and the higher of char gasification reactivity will be.
The fly ash from the outlet of the fluidized bed gasifier cyclone is chosen as the research sample. The structure and reactivity differences between fly ash and laboratory-prepared fast pyrolysis chars are compared. The XRD results demonstrate that the aromatic nucleus of laboratory-prepared fast pyrolysis chars is larger and more orderly than that of fly ash. N2and CO2are used as adsorbent for surface area test of char and fly ash, respectively, and it is found that the pores of fly ash are mainly macropores and intermediate pores, while the pores of fast pyrolysis chars are mainly micropores. The CO2gasification reactivity of fly ash is higher than that of fast pyrolysis chars, while its steam gasification reactivity is lower due to the pore structure difference.
A method for coal gasification reactivity evaluation applicable to the fluidized bed gasifiers is established according to the results of this dissertation, including a series of standardized process involving sample preparation, fast pyrolysis char preparation, and char gasification, etc.
本论文在接近流化床条件下,研究了低阶煤的快速热解特性以及煤焦气化活性,综合分析了煤种特性和反应条件对气化活性的影响,并对比研究了实验室制焦与流化床热解炉底渣、气化炉飞灰之间的结构差异和反应性差异。
采用热重-质谱(TG-MS)联用技术研究了不同煤种的程序升温热解特性和气体产物释放规律,并在接近流化床热解炉操作温度范围内,采用快速热解装置制备快速热解煤焦,研究了煤的快速热解特性以及不同热解条件下煤焦的形态结构。
采用热重分析技术研究了气化温度、制焦温度、热解速率等条件分别对煤焦-水蒸气和煤焦-CO2气化活性的影响。结果表明,在本研究采用的实验条件下,热解条件中以热解速率对煤焦气化活性影响较大,制焦温度和制焦停留时间的影响相对较小。温度条件中,煤焦气化反应速率主要受气化温度的影响,制焦温度影响相对较小。随着气化温度增加,煤焦的反应性指数和最大反应速率近似线性增长。煤焦-CO2和煤焦-水蒸气气化的活化能都随着碳转化率的升高而增加。
采用七种不同煤化程度的原煤进行煤焦制备和气化活性测试,总结了普遍适用的规律：碳转化率达到50%对应的比气化速率与相同反应条件下的平均比气化速率在数值上近似相等；灰分的行为对煤焦气化活性有非常重要的影响,它在不同反应阶段和不同气化温度下作用不同,这是由于灰分组成和含量的变化导致的；煤焦孔结构对气化活性的影响在越温和的反应条件下越突出,但煤焦气化活性高低与初始孔结构没有直接关系；煤焦-C02和煤焦-水蒸气气化的相对活性比率随着气化温度的升高而降低,表明高温条件可以缩小煤焦在这两种气氛中活性差距。
对比研究了水平管式炉快速热解煤焦、鼓泡床煤焦、流化床热解炉煤焦表面形貌和结构及其对气化活性的影响。采用不同活性指标进行比较,发现在制焦温度相同或近似时,水平管式炉快速热解煤焦、鼓泡床热解煤焦和循环流化床热解煤焦活性指标之间存在近似线性关系。制焦过程传热传质越剧烈,煤焦孔结构越丰富,晶格有序化程度越低,气化活性越高。
以流化床气化炉旋风分离器出口飞灰样品为研究对象,对比研究气化炉飞灰样品与实验室水平管式炉快速热解煤焦结构及反应性差异。XRD测试结果表明,实验室快速热解煤焦的缩核芳核尺度比飞灰大,且有序化程度比飞灰高。分别采用N2和CO2作为吸附剂煤焦和飞灰的比表面积,结果表明飞灰的孔结构以大孔和过渡孔为主,而快速热解煤焦的孔结构以微孔为主。孔结构的差异导致飞灰的CO2气化活性高于快速热解煤焦,但是水蒸气气化活性比快速热解煤焦低。
根据本论文的研究结果,建立了适用于流化床气化炉的煤种气化活性评价方法,其中涉及样品预处理、快速热解煤焦制备、煤焦气化等一系列标准化实验和分析流程。
The technology of coal gasification in fluidized bed is extensively concerned due to its mild gasification conditions and large gasification intensity. Although the process and structure of fluidized bed gasifier is improved continuously, the regulation mechanism is still unclear because of the complicated chemical reactions in the reactor. A series experiments needs to be carried out in order to solve the problems of high carbon content in fly ash and low gasification efficiency. It will take a lot of time and effort to conduct experiments directly in the fluidized bed reactors because of the complex operations, inadequate data and poor reproducibility. Therefore, it is theoretically and practically significant to study coal pyrolysis and gasification properties in the conditions closing to fluidized bed reactor with modern precision instruments technology. Then the kinetic data can be obtained, and the gasification reactivity of raw coal can be determined by influence factors analysis and dynamics analysis, which provides the important reference for optimizing operation parameters.
In this dissertation, the fast pyrolysis characteristics of low rank coal and gasification reactivity of char at the conditions closing to fluidized bed reactors are investigated. The effects of coal characteristics and reaction conditions on gasification reactivity are analyzed, and the differences in structure and reactivity among the laboratory-prepared fast pyrolysis char, bottom slag and gasifer fly ash of the fluidized bed pyrolysis furnaces are compared.
Characteristics of pyrolysis process and gas products during temperature-programmed pyrolysis of different coals are analyzed with thermogravimetric-mass spectrometry (TG-MS). Fast pyrolysis device is used to prepare fast pyrolysis char at the temperatures close to fluidized bed operating temperatures. The fast pyrolysis characteristics of coal and the char morphology under different pyrolysis conditions are studied.
Contrastive study on the reactivity of the chars gasification with steam and CO2, respectively, is conducted by thermogravimetric technology. The effects of gasification temperature, pyrolysis temperature and pyrolysis rate on gasification reactivity of the chars are investigated. Under the experimental condition, the results show that pyrolysis rate greatly affects gasification reactivity, however the effects of pyrolysis temperature and residence time are relatively small. In the temperature conditions, gasification temperature is the most important factor influencing gasification rate, while the effect of pyrolysis temperature is weaker. The reactivity index and the maximum reaction rate changes linearly with the increase in gasification temperature. The activation energy of both char-CO2and char-steam gasification increases with increase in carbon conversion rate.
Seven types of coals with different coal ranks are used for char preparation and gasification reactivity test, and some conclusions are obtained. It is found that the value of half reaction specific rate is approximate to the average specific rate under the same conditions. Ash behavior plays an important role in the char reactivity, and changes with gasification temperature and reaction degree due to the variation in the compositions and relative amount. The influence of pore structure is more noticeable during a relatively moderate reaction process, but the gasification reactivity of char has no immediate connection with the initial pore structure. The relative gasification reactivity ratio of char-steam to char-CO2generally decreases with the increasing temperature, indicating that high temperature can reduce the reactivity gap between the two reactions.
The surface morphology and structure of the chars from fast pyrolysis in the horizontal tube furnace, a bubbling bed and a fluidized bed are compared, and its effect on gasification reactivity is discussed. Different indicators are used to evaluate the gasification reactivity of the chars, and it is found that there is a linear relationship between the indicators of the chars from different reactors. The more intense of the heat and mass transfer process is, the more orderly of the crystal lattice and the higher of char gasification reactivity will be.
The fly ash from the outlet of the fluidized bed gasifier cyclone is chosen as the research sample. The structure and reactivity differences between fly ash and laboratory-prepared fast pyrolysis chars are compared. The XRD results demonstrate that the aromatic nucleus of laboratory-prepared fast pyrolysis chars is larger and more orderly than that of fly ash. N2and CO2are used as adsorbent for surface area test of char and fly ash, respectively, and it is found that the pores of fly ash are mainly macropores and intermediate pores, while the pores of fast pyrolysis chars are mainly micropores. The CO2gasification reactivity of fly ash is higher than that of fast pyrolysis chars, while its steam gasification reactivity is lower due to the pore structure difference.
A method for coal gasification reactivity evaluation applicable to the fluidized bed gasifiers is established according to the results of this dissertation, including a series of standardized process involving sample preparation, fast pyrolysis char preparation, and char gasification, etc.
引文
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