钙基脱硫剂硫化反应产物层扩散机制研究
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摘要
SO_2排放控制是洁净燃烧研究领域的重中之重。干法脱硫中钙基脱硫剂(石灰石)的脱硫效率不高、钙利用率较低。本文从影响钙基脱硫剂微观结构的主要成因,颗粒微观结构分形特性,晶粒团聚模式的粘附融合规律,颗粒孔隙中的气体扩散动力学传质规律,致密晶粒内的固态离子传质规律,以及气-固传质扩散的耦合控制模式等方面展开研究,以期为提高脱硫效率提供理论支撑。主要研究内容及成果如下:
(1)为探索近似CFB条件对脱硫剂煅烧分解后结构特性的影响,对DTU-2A型热天平进行了技术改造。实验发现:气氛中CO_2浓度增大易导致碳酸化;水蒸气对石灰石分解起到一定的催化作用;温度升高会加快石灰石分解过程,但会加剧石灰石煅烧产物的烧结;杂质导致石灰石最终分解转化率降低。多种因素造成脱硫剂颗粒具有非线性结构。
(2)分形维数是表征微粒结构特性的重要参数。研究表明:用SEM图像法和压汞仪法均能有效测定颗粒试样的分形维数。同时发现:脱硫剂随温度升高或杂质增加,烧结现象愈严重,脱硫剂分形维数降低。并提出一种测定石灰石煅烧颗粒微观形貌多重分形谱的方法。
(3)通过建立三维空间粘附方程,进行了晶粒团聚融合的计算机模拟研究,并与压汞仪实验数据进行定性对比分析,发现:石灰石在高温煅烧过程中,存在晶粒融合现象,会导致CaO颗粒分形维数、孔隙率、比表面积的降低。本文利用晶粒团聚体的概念,对产物层进行了二级划分,即:颗粒产物层和晶粒产物层,在颗粒产物层内传质过程服从气体扩散机制,在晶粒产物层内传质过程服从固态离子扩散机制。
(4)压汞仪实验发现颗粒产物层内的孔隙尺寸在5-2000nm范围内,Knudsen数很大,基本处于K n>0.1区域,反应气体SO_2分子在其内部的扩散存在稀薄气体效应,产物层中孔隙的分形结构导致扩散能力下降,计算出了颗粒产物层内的气体扩散系数,分析了反应气体在颗粒产物层内沿径向的浓度分布规律。
(5)利用扫描电镜能谱分析功能研究晶粒产物层内离子扩散流,发现:Ca~(2+)离子“向外生长”扩散方式是晶粒产物层内的主要扩散形式,且属于电中性扩散,扩散驱动力来自产物表层的缺陷飘移;利用电导率补偿效应获得CaSO_4产物层的Arrhenius特征温度680K,特征电导率10-5.722S,采用差热分析法推定脱硫剂晶粒产物层内的固态离子扩散活化能为223.98KJ/mol,并计算出了固态离子扩散系数。
(6)建立了颗粒系统硫化反应物质流的耦合扩散方程,对照TGA实验数据进行定性比较。研究发现:硫化反应扩散过程是由气体扩散与固态离子扩散两种扩散形式耦合作用的结果;固态离子扩散过程对整体硫化进程的控制作用是非常重要的,尤其是在反应初期的控制作用往往被忽视。
Recent study on the release control of SO_2 has become the most important focus in the study of clean coal combustion. Ca-based sorbent (limestone) has been widely applied in dry desulfurization technology, and still, its desulfurization efficiency and calcium utilizable efficiency are both low. In order to attain the theoretical supports for enhancing the efficiency of sulfur removal, the main research contents in this paper include: the main causes of micro-pore structure in sorbent particle, the fractal property of micro-pore structure in sorbent particle, the adhesion and fusion rule of grain aggregates, the reaction gas kinetics diffusion rule inside pores, the solid-state ion mass transfer law inside compact grain, the gas-solid mass diffusion’s coupling control model. The details and results are as follows:
(1) The technical improvement of DTU-2A thermal gravity analyzer (TGA) has been made to explore the influence of different CFB calcination conditions on sorbent’s microstructure property. The TGA experiments show that, high concentration of CO_2 is liable to lead to carbonation, H2O steam promote limestone decomposition, high temperature accelerates limestone decomposition and causes sintering and aggravated micro-pore structure, and the impurities reduce the final conversion rate of limestone decomposition.
(2) Fractal dimension is an important parameter for representing micro-particle structure properties. Comparison experiments show, both image analysis technology and mercury intrusion method can efficiently survey particle sample’s fractal dimension. Also, more impurities or higher temperature lead to lower fractal dimension because of sintering. A determination method of multi-fractal spectrum about limestone calcination particle morphology is presented in this chapter.
(3) The adhesion equation in three-dimension space was found to simulate the CaO grain’s aggregation and fusion process in computer. The results were compared with experiment data from mercury injection apparatus. During limestone high-temperature calcinations, the appearance of grain fusion caused the decrease of fractal dimension, porosity, specific surface area. The concept of grains aggregate is presented in this chapter. According to this accept, the product layer is divided into two layers, one is the product layer of gas diffusion mechanism inside particle, and the other one is the product layer of solid-state ion exchange mechanism inside grain.
(4) The experiment results on mercury injection apparatus show that, the size of pores in the CaO particle is 5-2000nm, their Knudsen values are high in the rang of K n>0.1. The diffusion of gaseous reaction SO_2 molecular inside particle layer occur rarefied gas effect. The fractal structure inside particle product layer leads to the decrease of gas diffusion capacity. The coefficient of gas diffusion inside particle product layer has been calculated out in this part, and also the concentration of reaction gas has been analyzed along the direction of diameter in the particle.
(5) Through the energy spectrum analysis of scanning electron microscopy, ion diffusion flow was studied inside the product layer of grain. The Ca~(2+) ion diffusion model of growth outward is the main form of the mass diffusion inside the grain product layer, which is neutral diffusion, the driving force for diffusion comes from defect drift in the surface of grain. Using the compensation effect of conductivity in CaSO_4 product layer, it is obtained that the characteristic temperature of Arrhenius is 600 K, characteristic conductivity is 10-5.722S. The activity energy of solid-state ion diffusion inside grain product layer is 223.98KJ/mol by a different-heat analysis. The coefficient of solid-state ion diffusion inside compact grain product layer has been calculated out in this chapter.
(6) The coupling control equation of sulfur reaction mass flow has been found, which results compared with the data from TGA experiments. It is shown that, the diffusion process of the sulfur reaction is coupled of two processes, one is gas diffusion process, and the other is solid-state ion diffusion process. The one of two processes, which diffusion rate is slower, controls the whole desulphurization process. The control effect of solid-state ion diffusion to the whole sulfur process is extremely important, especially during the beginning of reaction, which had been ignored by people in the past.
(1)为探索近似CFB条件对脱硫剂煅烧分解后结构特性的影响,对DTU-2A型热天平进行了技术改造。实验发现:气氛中CO_2浓度增大易导致碳酸化;水蒸气对石灰石分解起到一定的催化作用;温度升高会加快石灰石分解过程,但会加剧石灰石煅烧产物的烧结;杂质导致石灰石最终分解转化率降低。多种因素造成脱硫剂颗粒具有非线性结构。
(2)分形维数是表征微粒结构特性的重要参数。研究表明:用SEM图像法和压汞仪法均能有效测定颗粒试样的分形维数。同时发现:脱硫剂随温度升高或杂质增加,烧结现象愈严重,脱硫剂分形维数降低。并提出一种测定石灰石煅烧颗粒微观形貌多重分形谱的方法。
(3)通过建立三维空间粘附方程,进行了晶粒团聚融合的计算机模拟研究,并与压汞仪实验数据进行定性对比分析,发现:石灰石在高温煅烧过程中,存在晶粒融合现象,会导致CaO颗粒分形维数、孔隙率、比表面积的降低。本文利用晶粒团聚体的概念,对产物层进行了二级划分,即:颗粒产物层和晶粒产物层,在颗粒产物层内传质过程服从气体扩散机制,在晶粒产物层内传质过程服从固态离子扩散机制。
(4)压汞仪实验发现颗粒产物层内的孔隙尺寸在5-2000nm范围内,Knudsen数很大,基本处于K n>0.1区域,反应气体SO_2分子在其内部的扩散存在稀薄气体效应,产物层中孔隙的分形结构导致扩散能力下降,计算出了颗粒产物层内的气体扩散系数,分析了反应气体在颗粒产物层内沿径向的浓度分布规律。
(5)利用扫描电镜能谱分析功能研究晶粒产物层内离子扩散流,发现:Ca~(2+)离子“向外生长”扩散方式是晶粒产物层内的主要扩散形式,且属于电中性扩散,扩散驱动力来自产物表层的缺陷飘移;利用电导率补偿效应获得CaSO_4产物层的Arrhenius特征温度680K,特征电导率10-5.722S,采用差热分析法推定脱硫剂晶粒产物层内的固态离子扩散活化能为223.98KJ/mol,并计算出了固态离子扩散系数。
(6)建立了颗粒系统硫化反应物质流的耦合扩散方程,对照TGA实验数据进行定性比较。研究发现:硫化反应扩散过程是由气体扩散与固态离子扩散两种扩散形式耦合作用的结果;固态离子扩散过程对整体硫化进程的控制作用是非常重要的,尤其是在反应初期的控制作用往往被忽视。
Recent study on the release control of SO_2 has become the most important focus in the study of clean coal combustion. Ca-based sorbent (limestone) has been widely applied in dry desulfurization technology, and still, its desulfurization efficiency and calcium utilizable efficiency are both low. In order to attain the theoretical supports for enhancing the efficiency of sulfur removal, the main research contents in this paper include: the main causes of micro-pore structure in sorbent particle, the fractal property of micro-pore structure in sorbent particle, the adhesion and fusion rule of grain aggregates, the reaction gas kinetics diffusion rule inside pores, the solid-state ion mass transfer law inside compact grain, the gas-solid mass diffusion’s coupling control model. The details and results are as follows:
(1) The technical improvement of DTU-2A thermal gravity analyzer (TGA) has been made to explore the influence of different CFB calcination conditions on sorbent’s microstructure property. The TGA experiments show that, high concentration of CO_2 is liable to lead to carbonation, H2O steam promote limestone decomposition, high temperature accelerates limestone decomposition and causes sintering and aggravated micro-pore structure, and the impurities reduce the final conversion rate of limestone decomposition.
(2) Fractal dimension is an important parameter for representing micro-particle structure properties. Comparison experiments show, both image analysis technology and mercury intrusion method can efficiently survey particle sample’s fractal dimension. Also, more impurities or higher temperature lead to lower fractal dimension because of sintering. A determination method of multi-fractal spectrum about limestone calcination particle morphology is presented in this chapter.
(3) The adhesion equation in three-dimension space was found to simulate the CaO grain’s aggregation and fusion process in computer. The results were compared with experiment data from mercury injection apparatus. During limestone high-temperature calcinations, the appearance of grain fusion caused the decrease of fractal dimension, porosity, specific surface area. The concept of grains aggregate is presented in this chapter. According to this accept, the product layer is divided into two layers, one is the product layer of gas diffusion mechanism inside particle, and the other one is the product layer of solid-state ion exchange mechanism inside grain.
(4) The experiment results on mercury injection apparatus show that, the size of pores in the CaO particle is 5-2000nm, their Knudsen values are high in the rang of K n>0.1. The diffusion of gaseous reaction SO_2 molecular inside particle layer occur rarefied gas effect. The fractal structure inside particle product layer leads to the decrease of gas diffusion capacity. The coefficient of gas diffusion inside particle product layer has been calculated out in this part, and also the concentration of reaction gas has been analyzed along the direction of diameter in the particle.
(5) Through the energy spectrum analysis of scanning electron microscopy, ion diffusion flow was studied inside the product layer of grain. The Ca~(2+) ion diffusion model of growth outward is the main form of the mass diffusion inside the grain product layer, which is neutral diffusion, the driving force for diffusion comes from defect drift in the surface of grain. Using the compensation effect of conductivity in CaSO_4 product layer, it is obtained that the characteristic temperature of Arrhenius is 600 K, characteristic conductivity is 10-5.722S. The activity energy of solid-state ion diffusion inside grain product layer is 223.98KJ/mol by a different-heat analysis. The coefficient of solid-state ion diffusion inside compact grain product layer has been calculated out in this chapter.
(6) The coupling control equation of sulfur reaction mass flow has been found, which results compared with the data from TGA experiments. It is shown that, the diffusion process of the sulfur reaction is coupled of two processes, one is gas diffusion process, and the other is solid-state ion diffusion process. The one of two processes, which diffusion rate is slower, controls the whole desulphurization process. The control effect of solid-state ion diffusion to the whole sulfur process is extremely important, especially during the beginning of reaction, which had been ignored by people in the past.
引文
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