微波辅助热解污泥机理与试验研究
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摘要
微波辅助热解污泥可使污泥中的有机物发生化学裂解,生成生物油、合成气和炭基吸附剂,有利于污泥的资源化利用,并且污染物排放可有效控制。本研究构建了一套5 kg处理能力的干化污泥微波装置。基于此装置,开展了试验研究与分析,着重分析了微波辐照条件(如微波加热功率、微波加热时间以及最终加热温度)和催化剂的应用对产物产量和质量的影响,并探讨了微波辅助热解污泥的反应机理。
微波辐照条件对热解污泥过程分析发现,微波加热功率和最终加热温度是影响微波升温过程的关键因素。微波辅助热解污泥制备生物油主要在150-400°C加热温度区域生成,生物油产率最高的温度范围为250-300°C。合成气产率最大化发生在250°C-320°C,产率在320°C以后开始下降。炭基吸附剂的最佳炭化温度约为600°C,当最终炭化温度达到700°C,会引起剧烈裂解反应,从而引起炭产量和质量的下降。总的来说,微波加热功率的增加有利于生物油和合成气质量的提高。
催化剂对微波辅助热解污泥实验研究表明,除催化剂FeSO4和ZnCl2的添加能提高合成气的产率外,其他催化剂的添加均降低了生物油、合成气和炭基吸附剂的产率。催化剂的添加对生物油、合成气和炭基吸附剂的质量均有显著性影响。对生物油而言,依据制备的生物油的卡路里值、密度、粘度和C含量分析,催化剂KOH、H2SO4、H3BO3和FeSO4的添加显著提高了生物油的质量,催化剂ZnCl2降低了生物油的质量。对合成气而言,污泥经酸化处理(添加H3PO4和H3BO3)明显降低了CO和CO2的生成,但增加了H2的生成量。对炭基吸附剂而言,催化剂的添加可促进生成炭基吸附剂的孔结构发育。
考虑到污泥热解过程及影响其过程因素的多种复杂性,分别运用三种统计推断方法(即神经网络、支持向量机、逐步聚类回归)建立基于统计的动力学预测模型,以实现在不同工况条件下分别对温度升高和产油过程的预报。研究结果表明,发现预测效果最好的为支持向量机预测模型,其预测精度的R2值达0.8以上,可以较好地用于污泥热解过程分析,从而实现对温度和产油速率变化的预报。
微波辅助热解污泥产物质量分配评估得出,炭基吸附剂、生物油和合成气质量分别占污泥原质量的65.0–68.9%、10.1–15.3%和11.8–13.4%。微波辅助热解污泥产物能量分配评估显示,每公斤污泥微波辅助热解产生的炭基吸附剂、生物油和合成气的热值分别为5.21–6.71 MJ、3.70–5.34 MJ和1.35–1.60 MJ。催化剂的添加增加了炭基吸附剂的能量储存,但降低了生物油的能量贮存。
Microwave-heating-based pyrolysis for sewage sludge can produce bio-oil, syngas and carbonaceous adsorbent, which is beneficial to resource recovery of wastes and emission mitigation of pollutants. In this study, a pilot-scale microwave heating equipment with the processing capacity of 5 kg solid waste was constructed. Using the equipment, the effects of important microwave-related processing parameters were investigated such as heating rate, final pyrolysis temperature and radiation time, as well as catalyst usage on the yield and quality of bio-oil, syngas and carbonaceous adsorbent. Moreover, the mechanisms and kinetics of resources recovery from sewage sludge pyrolysis using microwave heating was explored by analyzing the components and properties of resultant products.
By analyzing the impacts of microwave heating conditions on sewage sludge pyrolysis, it was found that microwave power and final temperature are the crucial factors during the temperature rising process. The generation of bio-oil occurred mainly in the range of 150-400°C, and the maximum bio-oil generation rate was researched at the temperature between 250-300°C. The syngas generation rate occurred at the temperature between 250°C-320°C. However, it decreased when the temperature was higher than 320°C. During the process of carbonaceous adsorbent production, the optimum carbonization temperature was approximately 600°C. When the temperature reached 700°C, violent pyrolysis reactions took place, leading to the decrease of carbon quantity and quality. In general, an increase in the microwave power was beneficial to enhancement of the bio-oil and syngas quality.
The impacts of catalysts on the pyrolysis process were further examined. Results showed that catalysts had significant impacts on the generation of bio-oil, syngas and carbonaceous adsorbent.The catalysts decreased the quantity of resultant products except that FeSO4 and ZnCl2 increased the quantity of syngas.KOH、H2SO4、H3BO3和FeSO4 significantly increased the quality of bio-oil, while ZnCl2 decreased. For the syngas, acidified sewage sludge added with H3PO4 or H3BO3 decreased CO and CO2 production rate, but increased the generation rate of H2.Regarding carbonaceous adsorbent, the catalysts can stimulate the formation of porous structure of SBAs. There is much complexity existing in the process of sewage sludge pyrolysis as well as its impact factors. This leads to the difficulty in investigating the mechanisms and kinetics of the pyrolysis process using traditional first-principle models. Therefore, three statistical inference methods were employed instead for modeling and forecasting of temperature-rise and bio-oil production processes. The results revealed that support vector machine achieved the best forecasting performance, with their R-square values higher than 0.8. Despite the first attempt, it was desired that further studies be undertaken to improve the accuracy of the statistical methods and extend them for modeling the kinetics of other processes such as gas synthesis and carbonaceous adsorption.
Moreover, energy and mass balance analysis was conducted. The results showed that the mass of the carbonaceous adsorbent, bio-oil and syngas accounts for 65–68.9%、10.1–15.3%, and 11.8–13.4% of the sewage sludge mass, respectively. The heat values of the carbonaceous adsorbent, bio-oil and syngas produced from each kilogram sewage sludge were 5.21 MJ–6.71 MJ、3.70 MJ–5.34 MJ和1.35 MJ–1.60 MJ, respectively. In addition, it was found that the addition of catalyst increased energy storage capacity of the carbonaceous adsorbent, but lowered that of the bio-oil.
微波辐照条件对热解污泥过程分析发现,微波加热功率和最终加热温度是影响微波升温过程的关键因素。微波辅助热解污泥制备生物油主要在150-400°C加热温度区域生成,生物油产率最高的温度范围为250-300°C。合成气产率最大化发生在250°C-320°C,产率在320°C以后开始下降。炭基吸附剂的最佳炭化温度约为600°C,当最终炭化温度达到700°C,会引起剧烈裂解反应,从而引起炭产量和质量的下降。总的来说,微波加热功率的增加有利于生物油和合成气质量的提高。
催化剂对微波辅助热解污泥实验研究表明,除催化剂FeSO4和ZnCl2的添加能提高合成气的产率外,其他催化剂的添加均降低了生物油、合成气和炭基吸附剂的产率。催化剂的添加对生物油、合成气和炭基吸附剂的质量均有显著性影响。对生物油而言,依据制备的生物油的卡路里值、密度、粘度和C含量分析,催化剂KOH、H2SO4、H3BO3和FeSO4的添加显著提高了生物油的质量,催化剂ZnCl2降低了生物油的质量。对合成气而言,污泥经酸化处理(添加H3PO4和H3BO3)明显降低了CO和CO2的生成,但增加了H2的生成量。对炭基吸附剂而言,催化剂的添加可促进生成炭基吸附剂的孔结构发育。
考虑到污泥热解过程及影响其过程因素的多种复杂性,分别运用三种统计推断方法(即神经网络、支持向量机、逐步聚类回归)建立基于统计的动力学预测模型,以实现在不同工况条件下分别对温度升高和产油过程的预报。研究结果表明,发现预测效果最好的为支持向量机预测模型,其预测精度的R2值达0.8以上,可以较好地用于污泥热解过程分析,从而实现对温度和产油速率变化的预报。
微波辅助热解污泥产物质量分配评估得出,炭基吸附剂、生物油和合成气质量分别占污泥原质量的65.0–68.9%、10.1–15.3%和11.8–13.4%。微波辅助热解污泥产物能量分配评估显示,每公斤污泥微波辅助热解产生的炭基吸附剂、生物油和合成气的热值分别为5.21–6.71 MJ、3.70–5.34 MJ和1.35–1.60 MJ。催化剂的添加增加了炭基吸附剂的能量储存,但降低了生物油的能量贮存。
Microwave-heating-based pyrolysis for sewage sludge can produce bio-oil, syngas and carbonaceous adsorbent, which is beneficial to resource recovery of wastes and emission mitigation of pollutants. In this study, a pilot-scale microwave heating equipment with the processing capacity of 5 kg solid waste was constructed. Using the equipment, the effects of important microwave-related processing parameters were investigated such as heating rate, final pyrolysis temperature and radiation time, as well as catalyst usage on the yield and quality of bio-oil, syngas and carbonaceous adsorbent. Moreover, the mechanisms and kinetics of resources recovery from sewage sludge pyrolysis using microwave heating was explored by analyzing the components and properties of resultant products.
By analyzing the impacts of microwave heating conditions on sewage sludge pyrolysis, it was found that microwave power and final temperature are the crucial factors during the temperature rising process. The generation of bio-oil occurred mainly in the range of 150-400°C, and the maximum bio-oil generation rate was researched at the temperature between 250-300°C. The syngas generation rate occurred at the temperature between 250°C-320°C. However, it decreased when the temperature was higher than 320°C. During the process of carbonaceous adsorbent production, the optimum carbonization temperature was approximately 600°C. When the temperature reached 700°C, violent pyrolysis reactions took place, leading to the decrease of carbon quantity and quality. In general, an increase in the microwave power was beneficial to enhancement of the bio-oil and syngas quality.
The impacts of catalysts on the pyrolysis process were further examined. Results showed that catalysts had significant impacts on the generation of bio-oil, syngas and carbonaceous adsorbent.The catalysts decreased the quantity of resultant products except that FeSO4 and ZnCl2 increased the quantity of syngas.KOH、H2SO4、H3BO3和FeSO4 significantly increased the quality of bio-oil, while ZnCl2 decreased. For the syngas, acidified sewage sludge added with H3PO4 or H3BO3 decreased CO and CO2 production rate, but increased the generation rate of H2.Regarding carbonaceous adsorbent, the catalysts can stimulate the formation of porous structure of SBAs. There is much complexity existing in the process of sewage sludge pyrolysis as well as its impact factors. This leads to the difficulty in investigating the mechanisms and kinetics of the pyrolysis process using traditional first-principle models. Therefore, three statistical inference methods were employed instead for modeling and forecasting of temperature-rise and bio-oil production processes. The results revealed that support vector machine achieved the best forecasting performance, with their R-square values higher than 0.8. Despite the first attempt, it was desired that further studies be undertaken to improve the accuracy of the statistical methods and extend them for modeling the kinetics of other processes such as gas synthesis and carbonaceous adsorption.
Moreover, energy and mass balance analysis was conducted. The results showed that the mass of the carbonaceous adsorbent, bio-oil and syngas accounts for 65–68.9%、10.1–15.3%, and 11.8–13.4% of the sewage sludge mass, respectively. The heat values of the carbonaceous adsorbent, bio-oil and syngas produced from each kilogram sewage sludge were 5.21 MJ–6.71 MJ、3.70 MJ–5.34 MJ和1.35 MJ–1.60 MJ, respectively. In addition, it was found that the addition of catalyst increased energy storage capacity of the carbonaceous adsorbent, but lowered that of the bio-oil.
引文
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