抗烧结钙基吸收剂同时捕集CO_2/SO_2的循环反应特性及动力学研究
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摘要
控制和减缓工业生产过程中CO_2的排放对于缓解全球变暖和温室效应具有重要意义。探索高效、抗烧结钙基吸收剂，并利用其吸碳/煅烧循环反应捕集CO_2是是控制CO_2排放的重要途径，而合成高性能吸收剂是其中的方法之一。目前对于合成钙基吸收剂的制备方法均较为复杂，应探索一种简单的方法制备高性能吸收剂；在对合成吸收剂循环吸收性能考察方面，需深入考察SO_2存在时，吸收剂同时捕集CO_2/SO_2的循环反应特性；在动力学方面，吸碳过程中快速反应与慢速反应的分界、合成吸收剂吸碳动力学、煅烧动力学以及反应过程中的本征动力学等问题都有待于进一步研究探讨。针对以上科学问题展开研究，可为钙基吸收剂循环吸收CO_2/SO_2的应用和深入探索奠定理论基础，具有重要的学术意义和应用前景。
本文针对抗烧结钙基吸收剂捕集CO_2研究的不足，采用湿法混合的方法制备新型钙基吸收剂，考察了含钙前驱物、添加剂前驱物等因素对合成吸收剂的循环吸收CO_2反应能力及循环稳定性的影响规律，获得了循环反应性能较好的抗烧结钙基吸收剂；实验研究了其同时捕集CO_2/SO_2的反应特性，分析了SO_2存在对钙基吸收剂循环吸收CO_2反应性能的影响规律。对钙基吸收剂循环吸收CO_2反应宏观动力学特性进行了研究，探讨了吸碳反应时快速反应和慢速反应阶段的动力学模型，分析了吸碳及煅烧阶段的宏观动力学的关键参数。深入研究了钙基吸收剂吸碳反应的本征动力学特性，分析了不同反应驱动力作用下吸收剂的本征动力学常数及活化能，探讨了变级数反应的控制机理。
考察了葡萄糖酸钙、乳酸钙和甲酸钙等有机物作为前驱物制备的钙基吸收剂的循环吸收CO_2特性，研究表明，由葡萄糖酸钙作为前驱物制得的G-CaO吸收剂具有最高的循环吸收率和循环稳定性。通过对添加剂元素和种类的考察发现，添加Mg元素可有效提高吸收剂的循环吸收率，而添加Al元素则可以大幅改善吸收剂的循环稳定性。经多循环测试，采用湿法混合制得的G(Ca)-G(Mg)75吸收剂的循环吸收率最高，而G(Ca)-L(Al)75循环稳定性最好，两种吸收剂为捕集CO_2的高性能吸收剂。吸收剂表现出不同的反应特性与其比表面积和孔容积有关，大的比表面积和孔容积有利于保持较高的反应活性。
研究了合成钙基吸收剂同时捕捉CO_2/SO_2时的循环反应特性，观测了SO_2引起的吸收剂微观结构的变化。研究表明，SO_2的存在严重阻碍了吸收剂对CO_2的捕集，随循环次数的增加，吸收剂循环吸收CO_2的转化率降低，累积吸收SO_2的转化率增加，总的Ca的利用率先降低后不断增加，煅烧分解速率降低；SO_2存在时，随循环次数的增加，吸收剂颗粒团聚加剧，其比表面积迅速降低，出现严重烧结的大孔，是造成吸收剂吸收CO_2能力快速下降的主要原因；SO2浓度越高，吸收剂吸收CO_2能力下降的越快，吸收SO2的转化率越高。
在对钙基吸收剂吸碳/煅烧循环宏观动力学研究中，提出在吸碳反应快速阶段采用Logistic方程拟合转化率随时间的变化曲线，并获得了钙基吸收剂的动力学模型方程；在慢速反应阶段采用Avrami方程能较好地描述吸收剂转化率随时间的变化；采用非等温法获得了吸收剂在煅烧反应阶段的关键动力参数；通过对吸收剂转化率随循环次数的分析预测，G(Ca)-G(Mg)75和G(Ca)-L(Al)75吸收剂经200次循环后转化率分别稳定在0.813和0.735。
深入研究了钙基吸收剂吸碳反应的本征动力学特性，探讨了变级数反应的控制机理。研究表明，在本征动力学控制阶段，在不同反应驱动力(P_(CO_2) P_(CO_2,eq))下，吸收剂出现变级数反应，在(PCO_2PCO_2,eq)<10kPa时，吸碳反应为1级反应；在(PCO_2PCO_2,eq)≥10kPa时吸碳反应级数趋近于零；钙基吸收剂的本征反应速率常数与(PC O2PCO_2,eq)有关，而G(Ca)-G(Mg)75和G(Ca)-L(Al)75吸收剂在本征反应阶段的活化能分别为24.9kJ/mol和21.12kJ/mol；反应级数的变化说明了控制机理的变化，当反应级数为1时，吸碳反应受CaO+CO_2CaO·CO_2控制；当反应级数为0时，吸碳反应受CaO CO_2CaCO_3控制。
本文较系统地研究了钙基吸收剂的制备及其循环吸收CO_2、同时捕集CO_2/SO_2的循环反应特性，得到了抗烧结、高性能的钙基吸收剂，探讨了其在同时捕集CO_2/SO2时的反应特性和规律，获得了吸碳/煅烧循环反应的动力学模型和关键参数，弄清了钙基吸收剂在本征动力学阶段变级数反应的控制机理。有助于推进钙基吸收剂循环吸收CO_2/SO2的深入研究，充实和丰富了CO_2捕集领域的研究成果，可为钙基吸收剂循环吸收CO_2/SO2的应用和深入探索提供理论支撑和依据。
It is significant to control and reduce CO2emissions in industrial processes forpreventing global warming and green house effect. Calcium-based sorbents with theircarbonation/calcinations cycles are widely employed as one of most importantapproaches for CO2capture. High efficiency and anti-sintering calcium-based sorbentsare pursed to improve cyclic reaction capacity. So far, most of methods for synthesizingcalcium-based sorbents are complex. A new simple method to produce high capacitysorbents should be found. For new synthesized sorbents, cyclic reaction characteristicfor co-capture CO2/SO_2should be investigated. The separation of rapid and slowreaction step for carbonation process, carbonation kinetics for calcium-based sorbents,calcination kinetics and intrinsic kinetics for carbonation should be further studied. Theabove scientific questions are focused and studied. The results can provide theoreticalsupport for co-capture CO2/SO_2with calcium-based sorbents. The research hasimportant academic value and application prospect.
Current situation for CO2capture with calcium-based sorbents were concerned. Asimple wet mixing method for producing new sorbents was used. Effects ofcalcium-precursors, additives on cyclic CO2absorption capacity and stability wereinvestigated. The anti-sintering and high efficiency calcium-based sorbents weresynthesized. The co-capture CO2/SO_2characteristic for synthesized sorbents wasstudied. Effects of SO_2on cyclic CO2capture capacity of calcium-based sorbents wereanalyzed. Carbonation/carbonation kinetics for calcium-based sorbents was investigated.Models of rapid and slow reaction steps in carbonation were discussed. The key kineticparameters were obtained. The intrinsic kinetic for calcium-based sorbents wasspecially investigated. The reaction rate constant and activation energy in differentdriving power were analyzed. The control mechanism of variation reaction order wasdiscussed.
The calcium-based sorbents produced from organic precursors such as calciumgluconate, calcium lactate and calcium formate were investigated for cyclic CO2capture.The results show that G-CaO sorbent produced from calcium gluconate exhibits thehighest cyclic absorption and stability. According to experimental study on additiveelements and categories, Mg elements can effectively improve cyclic absorptioncapacity while Al elements can improve cyclic stability. After many cycles tests, G(Ca)-G(Mg)75shows the best cyclic absorption efficiency while G(Ca)-L(Al)75has the highest cyclic stability. The two sorbents are high-efficiency calcium-based sorbents for CO2capture. The reaction characteristic for synthesized sorbents related to specific surface area and pore volume. The absorption reaction can be benefited on higher specific surface area and pore volume.
Cyclic characteristic of co-capture CO2/SO2with synthesized calcium-based sorbents were investigated. The micro-structure changes of calcium-based sorbents caused by SO2were observed. The results show that SO2seriously impedes CO2capture by calcium-based sorbents. When number of cycles increase, CO2absorption capacity decreases while cumulative SO2absorption capacity increases. Total calcium utilization ratio first decreases and then increases while calcination decomposition ratio decreases with number of cycles. In co-capture CO2/SO2process, grains reunite becomes seriously with number of cycles, specific surface area decreases rapidly. Bigger pores caused by sintering were emerged. The above are major reasons for rapid decrease of CO2capture capacity. The CO2capture capacity decreases more quickly with higher SO2concentrations while cumulative SO2conversion ratio becomes much higher.
In carbonation/calcination cycle kinetics study, Logistic equation was employed to fit conversion ration curve as a function of time at the rapid reaction step. Avrami equation can well describe the conversion ration variation with time. The key kinetic parameters in calcination stage were obtained by a non-isothermal method. According to conversion ration variation with number of cycles, conversion rations of G(Ca)-G(Mg)75and G(Ca)-L(Al)75stabilize after200cycles, with their value0.813and0.735respectively.
In the intrinsic kinetics study of carbonation for calcium-based sorbents, the variable reaction order was found. The intrinsic reaction order changed abruptly from first-order to zero-order when the driving force (PCO2-PCO2,eq) exceeded an equilibrium value about lOkPa in this work. The intrinsic reaction rate constants were relative to (PCO2-PCO2,eq).The activation energies were found to be24.9kJ/mol and21.12kJ/mol for G(Ca)-G(Mg)75and G(Ca)-L(Al)75, respectively. The transition of reaction order suggested a shift of control mechanism. When the order was first, carbonation was controlled by whereas, controlled by when the order was zero. In this thesis work, a series of investigations for calcium-based sorbents was taken systematically, such as preparation of synthesis sorbents and cyclic reactioncharacteristics for CO_2capture and simultaneous CO_2/SO_2capture. Anti-sinteringcalcium-based sorbents were obtained with high reaction capacity. The reactioncharacteristics and pattern for simultaneous CO_2/SO_2capture were also concluded. Thekinetic model and key parameters were achieved for carbonation/calcination cyclicreaction. Besides, the control mechanism of variable order reaction for intrinsic surfacereaction stage was studied. This thesis work could help advancing the further researchfor simultaneous CO_2/SO_2capture and enriching the research findings for CO_2capture,and also gives a theory support for the utilization of calcium-based sorbents whensimultaneously capturing CO_2/SO_2.
本文针对抗烧结钙基吸收剂捕集CO_2研究的不足，采用湿法混合的方法制备新型钙基吸收剂，考察了含钙前驱物、添加剂前驱物等因素对合成吸收剂的循环吸收CO_2反应能力及循环稳定性的影响规律，获得了循环反应性能较好的抗烧结钙基吸收剂；实验研究了其同时捕集CO_2/SO_2的反应特性，分析了SO_2存在对钙基吸收剂循环吸收CO_2反应性能的影响规律。对钙基吸收剂循环吸收CO_2反应宏观动力学特性进行了研究，探讨了吸碳反应时快速反应和慢速反应阶段的动力学模型，分析了吸碳及煅烧阶段的宏观动力学的关键参数。深入研究了钙基吸收剂吸碳反应的本征动力学特性，分析了不同反应驱动力作用下吸收剂的本征动力学常数及活化能，探讨了变级数反应的控制机理。
考察了葡萄糖酸钙、乳酸钙和甲酸钙等有机物作为前驱物制备的钙基吸收剂的循环吸收CO_2特性，研究表明，由葡萄糖酸钙作为前驱物制得的G-CaO吸收剂具有最高的循环吸收率和循环稳定性。通过对添加剂元素和种类的考察发现，添加Mg元素可有效提高吸收剂的循环吸收率，而添加Al元素则可以大幅改善吸收剂的循环稳定性。经多循环测试，采用湿法混合制得的G(Ca)-G(Mg)75吸收剂的循环吸收率最高，而G(Ca)-L(Al)75循环稳定性最好，两种吸收剂为捕集CO_2的高性能吸收剂。吸收剂表现出不同的反应特性与其比表面积和孔容积有关，大的比表面积和孔容积有利于保持较高的反应活性。
研究了合成钙基吸收剂同时捕捉CO_2/SO_2时的循环反应特性，观测了SO_2引起的吸收剂微观结构的变化。研究表明，SO_2的存在严重阻碍了吸收剂对CO_2的捕集，随循环次数的增加，吸收剂循环吸收CO_2的转化率降低，累积吸收SO_2的转化率增加，总的Ca的利用率先降低后不断增加，煅烧分解速率降低；SO_2存在时，随循环次数的增加，吸收剂颗粒团聚加剧，其比表面积迅速降低，出现严重烧结的大孔，是造成吸收剂吸收CO_2能力快速下降的主要原因；SO2浓度越高，吸收剂吸收CO_2能力下降的越快，吸收SO2的转化率越高。
在对钙基吸收剂吸碳/煅烧循环宏观动力学研究中，提出在吸碳反应快速阶段采用Logistic方程拟合转化率随时间的变化曲线，并获得了钙基吸收剂的动力学模型方程；在慢速反应阶段采用Avrami方程能较好地描述吸收剂转化率随时间的变化；采用非等温法获得了吸收剂在煅烧反应阶段的关键动力参数；通过对吸收剂转化率随循环次数的分析预测，G(Ca)-G(Mg)75和G(Ca)-L(Al)75吸收剂经200次循环后转化率分别稳定在0.813和0.735。
深入研究了钙基吸收剂吸碳反应的本征动力学特性，探讨了变级数反应的控制机理。研究表明，在本征动力学控制阶段，在不同反应驱动力(P_(CO_2) P_(CO_2,eq))下，吸收剂出现变级数反应，在(PCO_2PCO_2,eq)<10kPa时，吸碳反应为1级反应；在(PCO_2PCO_2,eq)≥10kPa时吸碳反应级数趋近于零；钙基吸收剂的本征反应速率常数与(PC O2PCO_2,eq)有关，而G(Ca)-G(Mg)75和G(Ca)-L(Al)75吸收剂在本征反应阶段的活化能分别为24.9kJ/mol和21.12kJ/mol；反应级数的变化说明了控制机理的变化，当反应级数为1时，吸碳反应受CaO+CO_2CaO·CO_2控制；当反应级数为0时，吸碳反应受CaO CO_2CaCO_3控制。
本文较系统地研究了钙基吸收剂的制备及其循环吸收CO_2、同时捕集CO_2/SO_2的循环反应特性，得到了抗烧结、高性能的钙基吸收剂，探讨了其在同时捕集CO_2/SO2时的反应特性和规律，获得了吸碳/煅烧循环反应的动力学模型和关键参数，弄清了钙基吸收剂在本征动力学阶段变级数反应的控制机理。有助于推进钙基吸收剂循环吸收CO_2/SO2的深入研究，充实和丰富了CO_2捕集领域的研究成果，可为钙基吸收剂循环吸收CO_2/SO2的应用和深入探索提供理论支撑和依据。
It is significant to control and reduce CO2emissions in industrial processes forpreventing global warming and green house effect. Calcium-based sorbents with theircarbonation/calcinations cycles are widely employed as one of most importantapproaches for CO2capture. High efficiency and anti-sintering calcium-based sorbentsare pursed to improve cyclic reaction capacity. So far, most of methods for synthesizingcalcium-based sorbents are complex. A new simple method to produce high capacitysorbents should be found. For new synthesized sorbents, cyclic reaction characteristicfor co-capture CO2/SO_2should be investigated. The separation of rapid and slowreaction step for carbonation process, carbonation kinetics for calcium-based sorbents,calcination kinetics and intrinsic kinetics for carbonation should be further studied. Theabove scientific questions are focused and studied. The results can provide theoreticalsupport for co-capture CO2/SO_2with calcium-based sorbents. The research hasimportant academic value and application prospect.
Current situation for CO2capture with calcium-based sorbents were concerned. Asimple wet mixing method for producing new sorbents was used. Effects ofcalcium-precursors, additives on cyclic CO2absorption capacity and stability wereinvestigated. The anti-sintering and high efficiency calcium-based sorbents weresynthesized. The co-capture CO2/SO_2characteristic for synthesized sorbents wasstudied. Effects of SO_2on cyclic CO2capture capacity of calcium-based sorbents wereanalyzed. Carbonation/carbonation kinetics for calcium-based sorbents was investigated.Models of rapid and slow reaction steps in carbonation were discussed. The key kineticparameters were obtained. The intrinsic kinetic for calcium-based sorbents wasspecially investigated. The reaction rate constant and activation energy in differentdriving power were analyzed. The control mechanism of variation reaction order wasdiscussed.
The calcium-based sorbents produced from organic precursors such as calciumgluconate, calcium lactate and calcium formate were investigated for cyclic CO2capture.The results show that G-CaO sorbent produced from calcium gluconate exhibits thehighest cyclic absorption and stability. According to experimental study on additiveelements and categories, Mg elements can effectively improve cyclic absorptioncapacity while Al elements can improve cyclic stability. After many cycles tests, G(Ca)-G(Mg)75shows the best cyclic absorption efficiency while G(Ca)-L(Al)75has the highest cyclic stability. The two sorbents are high-efficiency calcium-based sorbents for CO2capture. The reaction characteristic for synthesized sorbents related to specific surface area and pore volume. The absorption reaction can be benefited on higher specific surface area and pore volume.
Cyclic characteristic of co-capture CO2/SO2with synthesized calcium-based sorbents were investigated. The micro-structure changes of calcium-based sorbents caused by SO2were observed. The results show that SO2seriously impedes CO2capture by calcium-based sorbents. When number of cycles increase, CO2absorption capacity decreases while cumulative SO2absorption capacity increases. Total calcium utilization ratio first decreases and then increases while calcination decomposition ratio decreases with number of cycles. In co-capture CO2/SO2process, grains reunite becomes seriously with number of cycles, specific surface area decreases rapidly. Bigger pores caused by sintering were emerged. The above are major reasons for rapid decrease of CO2capture capacity. The CO2capture capacity decreases more quickly with higher SO2concentrations while cumulative SO2conversion ratio becomes much higher.
In carbonation/calcination cycle kinetics study, Logistic equation was employed to fit conversion ration curve as a function of time at the rapid reaction step. Avrami equation can well describe the conversion ration variation with time. The key kinetic parameters in calcination stage were obtained by a non-isothermal method. According to conversion ration variation with number of cycles, conversion rations of G(Ca)-G(Mg)75and G(Ca)-L(Al)75stabilize after200cycles, with their value0.813and0.735respectively.
In the intrinsic kinetics study of carbonation for calcium-based sorbents, the variable reaction order was found. The intrinsic reaction order changed abruptly from first-order to zero-order when the driving force (PCO2-PCO2,eq) exceeded an equilibrium value about lOkPa in this work. The intrinsic reaction rate constants were relative to (PCO2-PCO2,eq).The activation energies were found to be24.9kJ/mol and21.12kJ/mol for G(Ca)-G(Mg)75and G(Ca)-L(Al)75, respectively. The transition of reaction order suggested a shift of control mechanism. When the order was first, carbonation was controlled by whereas, controlled by when the order was zero. In this thesis work, a series of investigations for calcium-based sorbents was taken systematically, such as preparation of synthesis sorbents and cyclic reactioncharacteristics for CO_2capture and simultaneous CO_2/SO_2capture. Anti-sinteringcalcium-based sorbents were obtained with high reaction capacity. The reactioncharacteristics and pattern for simultaneous CO_2/SO_2capture were also concluded. Thekinetic model and key parameters were achieved for carbonation/calcination cyclicreaction. Besides, the control mechanism of variable order reaction for intrinsic surfacereaction stage was studied. This thesis work could help advancing the further researchfor simultaneous CO_2/SO_2capture and enriching the research findings for CO_2capture,and also gives a theory support for the utilization of calcium-based sorbents whensimultaneously capturing CO_2/SO_2.
引文
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