以CaO为吸收体的生物质无氧气化制氢的机理与试验研究
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摘要
化石燃料是当今世界的主要能源。然而,化石燃料不仅面临日益短缺的问题,其利用还带来了严重的环境污染并加剧了温室效应。充分利用可再生能源,开发清洁、高效、低碳排放的先进能源利用技术尤为重要。以CaO为吸收体的生物质无氧气化制氢技术是近年来兴起的一种新型制氢方法。利用该技术不但可以利用可再生的生物质资源制取高纯度H2、构建高效的能源利用系统,而且能同时获得高浓度的CO2气体、便于实现温室气体CO2的运输和储存。本文主要针对该技术开展相关的机理和试验研究。
研究高CaO/C摩尔比条件下的生物质热解机理对分析生物质无氧气化反应物的分布具有重要意义,也有助于分析CaO对CO2和生物质焦油析出的影响规律。利用热重-傅里叶变换红外光谱联用方法进行了不同CaO添加量、不同升温速率下麦秆热解特性的试验研究。研究表明,在高CaO/C摩尔比条件下添加CaO后麦秆热解呈现出两个不同的阶段。在热解第一阶段(主要阶段),添加CaO明显降低了热解挥发分包括H2O、CO、CO2、CH4以及焦油类物质甲苯、间二甲苯、苯酚、蚁酸等的析出,该阶段热解失重量相应减少。CaO在麦秆热解中起到了CO2吸收剂和焦油分解催化剂的双重作用。动力学计算表明添加CaO还降低了麦秆热解反应的活化能。添加CaO后麦秆热解第二阶段主要是第一阶段所生成的CaCO3煅烧分解重新释放出CO2的过程,在实际气化过程中应该防止热解第二阶段的发生。
加压不仅有利于提高气化强度,还将促进CaO碳酸化反应的进行,从而有利于进一步促进水煤气反应和水煤气变换反应。利用加压热重分析仪研究了不同总压、不同CO2浓度条件下CaO碳酸化反应的动力学特性。结果表明,提高总压和提高CO2浓度均能提高碳酸化初始阶段的反应速率和CaO的最终转化率。采用收缩核机理模型进行了等温反应动力学研究。发现CaO碳酸化反应的活化能随着压力的升高而逐渐降低。提出了综合考虑反应温度和CO2分压的CaO碳酸化反应速率经验方程。
CaO的循环碳酸化反应活性对系统的经济性至关重要。利用加压热重分析仪考查了不同煅烧压力对CaO循环碳酸化反应活性的影响,同时研究了常压蒸馏水活化和加压水蒸汽活化两种方法对CaO循环碳酸化活性改进的效果。结合扫描电镜技术分析了CaO循环反应活性变化的原因。结果表明,低压煅烧时获得的吸收剂具有更高的孔隙率,其碳酸化活性随循环次数增加而降低的程度较加压煅烧时要低。两种活化方法均有效改善了CaO的孔隙结构,经过6次“煅烧-碳酸化”循环CaO的碳酸化平均活性分别提高了约22%和27%。
流化床运行条件下气化操作变量的变化将对所研究的技术产生重要影响。利用自行搭建的常压流化床研究了CaO/C摩尔比、H2O/C摩尔比以及气化温度T对木屑无氧气化制氢过程的影响。结果表明,在研究范围内(CaO/C：0～2；H2O/C：1.2～2.18,T：489～740℃),CaO/C摩尔比、H20/C摩尔比和气化温度的提高均有利于提高合成气中H2的产量和浓度。在CaO/C摩尔比为1、H2O/C摩尔比为2.18、温度为740℃的条件下获得了H2浓度达62%的气化合成气,H2产量达72g/kg生物质。与先前其他生物质气化实验结果的对比验证了该技术在制取含高浓度H2和低浓度CO2的合成气方面具有优势。
为开展加压条件下生物质无氧气化制氢的试验研究,自行设计、搭建了一台最大工作压力为1.0MPa的加压双循环流化床反应装置。在冷态试验的基础上,利用该试验台进行了加压条件下木屑无氧气化制氢的热态试验研究(反应压力1～4bar,反应温度530～760℃,CaO/C摩尔比0～1.2,H20/C摩尔比0.72～0.89)。结果表明：加压有利于提高合成气中H2的浓度和产量。与常压试验相比,加压反应进一步降低了合成气中CO2的浓度、减少了水蒸汽的消耗量,并提高了生物质气化的碳转化率和冷煤气效率。在反应压力为4bar、反应温度为680℃、H2O/C摩尔比为0.89、CaO/C摩尔比为1.2的条件下,合成气中H2的浓度和产量分别达到了67.7%、68g/kg木屑。
为了全面获得系统的运行特性,为下一步试验研究提供理论指导,建立了以CaO为吸收体的生物质无氧气化制氢系统的动力学模型。模型考虑了气化炉和燃烧炉的物质和能量平衡,包含了生物质热解、生物质热解产物气化、CaO碳酸化、生物质半焦燃烧以及CaCO3煅烧等重要的反应过程。利用该模型全面预测了压力、温度、反应气氛对系统运行特性的影响。预测结果表明,比较合理的反应条件为：气化和煅烧压力～1MPa、气化温度～973K、燃烧温度～1173K。在典型工况计算条件下,系统达到了较合理的运行特性和制氢效果。
Fossil fuels are the main energy sources in the world. However, fossil fuels will be in large shortage in the near future. Moreover, the utilization of fossil fuels makes great challenge in environment protection and aggravates the global warming. As a result, it is rather significant to use renewable energy and develop advanced energy utilization technologies, which are clean, highly efficient and with low carbon emission. The CaO sorption enhanced biomass anaerobic gasification is a novel technology to produce hydrogen, which can not only produce syngas with high purity hydrogen using renewable biomass resource, but also be capable to obtain flue gases with high CO2concentration. The development of this technology will helps to construct high efficiency energy utilization system and be beneficical for CO2transport and storage. This thesis focuses on both mechanism and experimental studies relating to CaO sorption enhanced biomass anaerobic gasification.
The study on biomass pyrolysis mechanism in the presence of abundant CaO is important to analyze reactant distributions prior to biomass anaerobic gasification and examine the influences of CaO additives on the evolution of CO2and biomass tar species. Using thermogravimetric Fourier transform infrared (TG-FTIR) analysis, wheat-straw pyrolysis experiments were conducted under different CaO addition amounts and heating rates. Results show that wheat-straw pyrolysis exhibits two stages in the presence of CaO. In the first and also the main stage, the addition of CaO apparently reduces the yields of H2O、CO、CO2、CH4and biomass tar species such as toluene, p-xylene, phenol and formic acid, and the total mass loss in this stage correspondingly decreases. CaO plays dual roles of both CO2sorbent and tar reduction catalyst in this stage. Kinetic calculation reveals that the addition of CaO can also lower the activation energy of biomass pyrolysis. The second stage is caused by the decomposition of CaCO3at high temperatures and should be avoided during realistic gasification operations.
Pressurized operation implies great benefit for CaO carbonation and plays a key role to enhance hydrogen production reactions. The kinetic reaction properties of CaO carbonation under high pressure were examined using a pressurized thermogravimetric analyzer. Experiments were performed at different total pressures and different CO2concentrations. It is found that the increase in total pressure and CO2concentration both accelerate the initial reaction rate of CaO carbonation and increase the final conversion of CaO sorbents. The shrinking core model is adopted for the isothermal kinetic analysis. Results of kinetic calculation show that the activation energy of CaO carbonation decreases with increasing pressures. An empirical reaction rate equation for CaO carbonation is proposed coupling both reaction temperature and CO2partial pressure.
The cyclic carbonation reactivity of CaO sorbents is critical for the economic of the whole system. Using a pressurized thermogravimetric analyzer and Scanning Electron Microscopy (SEM) technology, the effect of calcination pressure on CaO cyclic carbonation reactivity was examined. Meanwhile, the reactivation of CaO sorbents during cyclic calcination-carbonation (CC) reactions was also surveyed using distilled water hydration at atmospheric pressure and saturated steam hydration at high pressure. It is found that CaO sorbents calcined under lower CO2partial pressure exhibit higher porosity and lose reactivity more slowly with increasing cycle number than those calcined at high pressure. Both two hydration methods efficiently improve the CaO reactivity during cyclic CC reactions as a result of the promoted surface area and porosity. The mean values of reactivity increase for water hydration and steam hydration after6cycles were～22%and～27%respectively.
The change of gasification operating variables under realistic fluidized bed conditions will have large influences on the investigated technology. The effects of CaO to carbon mole ratio (CaO/C), H2O to carbon mole ratio (H2O/C) and gasification temperature (T) on hydrogen production from sawdust anaerobic gasification were examined at atmospheric pressure, using a self-design bubbling fluidized bed reactor. Results show that, over the ranges examined in this study (CaO/C:0-2; H2O/C:1.2-2.18, T:489-740℃), the increase of CaO/C, H2O/C and T are all favorable for promoting H2production. A maximum H2output with a concentration of62%and a yield of72g/kg-biomass is achieved at CaO/C=1, H2O/C=2.18and T=740℃. The comparison with previous studies on fluidized bed biomass gasification reveals that this method has the advantage of being capable to produce a syngas with high H2concentration and low CO2concentration.
In order to investigate the effects of reaction pressure on CaO sorption enhanced biomass anaerobic gasification, a pressurized dual circulating fluidized beds reactor was designed and constructed, which can be operated at pressures up to1.0MPa. After the cold state tests, hydrogen production experiments were performed in this facility using sawdust anaerobic gasification within the following experimental ranges: pressure (P)1-4bar, T530-760℃, CaO/C0-1.2and H2O/C0.72-0.89. Results show that pressurized operations are beneficial to increase both H2concentration and H2yield. Compared with the atmospheric runs, pressurized gasification further decreases the CO2concentration in syngas, reduces the consumption of steam and promotes the biomass carbon conversion and cold gas efficiency. H2output with a concentration of67.7%and a yield of68g/kg-sawdust was achieved at P=4bar, CaO/C=1.2, H2O/C=0.89and T=680℃.
To get systematic operation properties of the whole H2production system and provide theoretical guide for the realistic dual fluidized bed runs in next step, a kinetic model for CaO sorption enhanced biomass anaerobic gasification was established. This model involves in five key reaction processes, i.e., biomass pyrolysis, gasification of the pyrolysis products, CaO carbonation, biomass char combustion and CaCO3calcination. Using this model, effects of reaction pressure, temperature and reaction atmosphere on system operation properties were systematically predicted. According to the calculation results, the suitable operation conditions are:gasification and calcination pressure1MPa, gasification temperature973K, calcination temperature1173K. At a typical calculation condition, the whole system achieves reasonable operation properties and H2output.
研究高CaO/C摩尔比条件下的生物质热解机理对分析生物质无氧气化反应物的分布具有重要意义,也有助于分析CaO对CO2和生物质焦油析出的影响规律。利用热重-傅里叶变换红外光谱联用方法进行了不同CaO添加量、不同升温速率下麦秆热解特性的试验研究。研究表明,在高CaO/C摩尔比条件下添加CaO后麦秆热解呈现出两个不同的阶段。在热解第一阶段(主要阶段),添加CaO明显降低了热解挥发分包括H2O、CO、CO2、CH4以及焦油类物质甲苯、间二甲苯、苯酚、蚁酸等的析出,该阶段热解失重量相应减少。CaO在麦秆热解中起到了CO2吸收剂和焦油分解催化剂的双重作用。动力学计算表明添加CaO还降低了麦秆热解反应的活化能。添加CaO后麦秆热解第二阶段主要是第一阶段所生成的CaCO3煅烧分解重新释放出CO2的过程,在实际气化过程中应该防止热解第二阶段的发生。
加压不仅有利于提高气化强度,还将促进CaO碳酸化反应的进行,从而有利于进一步促进水煤气反应和水煤气变换反应。利用加压热重分析仪研究了不同总压、不同CO2浓度条件下CaO碳酸化反应的动力学特性。结果表明,提高总压和提高CO2浓度均能提高碳酸化初始阶段的反应速率和CaO的最终转化率。采用收缩核机理模型进行了等温反应动力学研究。发现CaO碳酸化反应的活化能随着压力的升高而逐渐降低。提出了综合考虑反应温度和CO2分压的CaO碳酸化反应速率经验方程。
CaO的循环碳酸化反应活性对系统的经济性至关重要。利用加压热重分析仪考查了不同煅烧压力对CaO循环碳酸化反应活性的影响,同时研究了常压蒸馏水活化和加压水蒸汽活化两种方法对CaO循环碳酸化活性改进的效果。结合扫描电镜技术分析了CaO循环反应活性变化的原因。结果表明,低压煅烧时获得的吸收剂具有更高的孔隙率,其碳酸化活性随循环次数增加而降低的程度较加压煅烧时要低。两种活化方法均有效改善了CaO的孔隙结构,经过6次“煅烧-碳酸化”循环CaO的碳酸化平均活性分别提高了约22%和27%。
流化床运行条件下气化操作变量的变化将对所研究的技术产生重要影响。利用自行搭建的常压流化床研究了CaO/C摩尔比、H2O/C摩尔比以及气化温度T对木屑无氧气化制氢过程的影响。结果表明,在研究范围内(CaO/C：0～2；H2O/C：1.2～2.18,T：489～740℃),CaO/C摩尔比、H20/C摩尔比和气化温度的提高均有利于提高合成气中H2的产量和浓度。在CaO/C摩尔比为1、H2O/C摩尔比为2.18、温度为740℃的条件下获得了H2浓度达62%的气化合成气,H2产量达72g/kg生物质。与先前其他生物质气化实验结果的对比验证了该技术在制取含高浓度H2和低浓度CO2的合成气方面具有优势。
为开展加压条件下生物质无氧气化制氢的试验研究,自行设计、搭建了一台最大工作压力为1.0MPa的加压双循环流化床反应装置。在冷态试验的基础上,利用该试验台进行了加压条件下木屑无氧气化制氢的热态试验研究(反应压力1～4bar,反应温度530～760℃,CaO/C摩尔比0～1.2,H20/C摩尔比0.72～0.89)。结果表明：加压有利于提高合成气中H2的浓度和产量。与常压试验相比,加压反应进一步降低了合成气中CO2的浓度、减少了水蒸汽的消耗量,并提高了生物质气化的碳转化率和冷煤气效率。在反应压力为4bar、反应温度为680℃、H2O/C摩尔比为0.89、CaO/C摩尔比为1.2的条件下,合成气中H2的浓度和产量分别达到了67.7%、68g/kg木屑。
为了全面获得系统的运行特性,为下一步试验研究提供理论指导,建立了以CaO为吸收体的生物质无氧气化制氢系统的动力学模型。模型考虑了气化炉和燃烧炉的物质和能量平衡,包含了生物质热解、生物质热解产物气化、CaO碳酸化、生物质半焦燃烧以及CaCO3煅烧等重要的反应过程。利用该模型全面预测了压力、温度、反应气氛对系统运行特性的影响。预测结果表明,比较合理的反应条件为：气化和煅烧压力～1MPa、气化温度～973K、燃烧温度～1173K。在典型工况计算条件下,系统达到了较合理的运行特性和制氢效果。
Fossil fuels are the main energy sources in the world. However, fossil fuels will be in large shortage in the near future. Moreover, the utilization of fossil fuels makes great challenge in environment protection and aggravates the global warming. As a result, it is rather significant to use renewable energy and develop advanced energy utilization technologies, which are clean, highly efficient and with low carbon emission. The CaO sorption enhanced biomass anaerobic gasification is a novel technology to produce hydrogen, which can not only produce syngas with high purity hydrogen using renewable biomass resource, but also be capable to obtain flue gases with high CO2concentration. The development of this technology will helps to construct high efficiency energy utilization system and be beneficical for CO2transport and storage. This thesis focuses on both mechanism and experimental studies relating to CaO sorption enhanced biomass anaerobic gasification.
The study on biomass pyrolysis mechanism in the presence of abundant CaO is important to analyze reactant distributions prior to biomass anaerobic gasification and examine the influences of CaO additives on the evolution of CO2and biomass tar species. Using thermogravimetric Fourier transform infrared (TG-FTIR) analysis, wheat-straw pyrolysis experiments were conducted under different CaO addition amounts and heating rates. Results show that wheat-straw pyrolysis exhibits two stages in the presence of CaO. In the first and also the main stage, the addition of CaO apparently reduces the yields of H2O、CO、CO2、CH4and biomass tar species such as toluene, p-xylene, phenol and formic acid, and the total mass loss in this stage correspondingly decreases. CaO plays dual roles of both CO2sorbent and tar reduction catalyst in this stage. Kinetic calculation reveals that the addition of CaO can also lower the activation energy of biomass pyrolysis. The second stage is caused by the decomposition of CaCO3at high temperatures and should be avoided during realistic gasification operations.
Pressurized operation implies great benefit for CaO carbonation and plays a key role to enhance hydrogen production reactions. The kinetic reaction properties of CaO carbonation under high pressure were examined using a pressurized thermogravimetric analyzer. Experiments were performed at different total pressures and different CO2concentrations. It is found that the increase in total pressure and CO2concentration both accelerate the initial reaction rate of CaO carbonation and increase the final conversion of CaO sorbents. The shrinking core model is adopted for the isothermal kinetic analysis. Results of kinetic calculation show that the activation energy of CaO carbonation decreases with increasing pressures. An empirical reaction rate equation for CaO carbonation is proposed coupling both reaction temperature and CO2partial pressure.
The cyclic carbonation reactivity of CaO sorbents is critical for the economic of the whole system. Using a pressurized thermogravimetric analyzer and Scanning Electron Microscopy (SEM) technology, the effect of calcination pressure on CaO cyclic carbonation reactivity was examined. Meanwhile, the reactivation of CaO sorbents during cyclic calcination-carbonation (CC) reactions was also surveyed using distilled water hydration at atmospheric pressure and saturated steam hydration at high pressure. It is found that CaO sorbents calcined under lower CO2partial pressure exhibit higher porosity and lose reactivity more slowly with increasing cycle number than those calcined at high pressure. Both two hydration methods efficiently improve the CaO reactivity during cyclic CC reactions as a result of the promoted surface area and porosity. The mean values of reactivity increase for water hydration and steam hydration after6cycles were～22%and～27%respectively.
The change of gasification operating variables under realistic fluidized bed conditions will have large influences on the investigated technology. The effects of CaO to carbon mole ratio (CaO/C), H2O to carbon mole ratio (H2O/C) and gasification temperature (T) on hydrogen production from sawdust anaerobic gasification were examined at atmospheric pressure, using a self-design bubbling fluidized bed reactor. Results show that, over the ranges examined in this study (CaO/C:0-2; H2O/C:1.2-2.18, T:489-740℃), the increase of CaO/C, H2O/C and T are all favorable for promoting H2production. A maximum H2output with a concentration of62%and a yield of72g/kg-biomass is achieved at CaO/C=1, H2O/C=2.18and T=740℃. The comparison with previous studies on fluidized bed biomass gasification reveals that this method has the advantage of being capable to produce a syngas with high H2concentration and low CO2concentration.
In order to investigate the effects of reaction pressure on CaO sorption enhanced biomass anaerobic gasification, a pressurized dual circulating fluidized beds reactor was designed and constructed, which can be operated at pressures up to1.0MPa. After the cold state tests, hydrogen production experiments were performed in this facility using sawdust anaerobic gasification within the following experimental ranges: pressure (P)1-4bar, T530-760℃, CaO/C0-1.2and H2O/C0.72-0.89. Results show that pressurized operations are beneficial to increase both H2concentration and H2yield. Compared with the atmospheric runs, pressurized gasification further decreases the CO2concentration in syngas, reduces the consumption of steam and promotes the biomass carbon conversion and cold gas efficiency. H2output with a concentration of67.7%and a yield of68g/kg-sawdust was achieved at P=4bar, CaO/C=1.2, H2O/C=0.89and T=680℃.
To get systematic operation properties of the whole H2production system and provide theoretical guide for the realistic dual fluidized bed runs in next step, a kinetic model for CaO sorption enhanced biomass anaerobic gasification was established. This model involves in five key reaction processes, i.e., biomass pyrolysis, gasification of the pyrolysis products, CaO carbonation, biomass char combustion and CaCO3calcination. Using this model, effects of reaction pressure, temperature and reaction atmosphere on system operation properties were systematically predicted. According to the calculation results, the suitable operation conditions are:gasification and calcination pressure1MPa, gasification temperature973K, calcination temperature1173K. At a typical calculation condition, the whole system achieves reasonable operation properties and H2output.
引文
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