烟草废弃物热解和气化的实验及机理研究
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摘要
众所周知，合理开发利用清洁的可再生能源是解决日益严峻的化石能源形势和日趋恶化的生态环境的重要手段。生物质能作为目前唯一一种可存储和运输的可再生能源，其资源化利用备受世界瞩目。烟草行业是我国重要经济支柱产业，卷烟加工会产生近30%烟草废弃物，如何将这些废弃物高效、清洁转化利用，不仅对地区经济社会的发展和环境保护有着重要意义，而且有益于当地建立持续发展的能源系统。生物质热化学转化技术是实现其能量转化最有效的方式，尤其是热解和气化将其转化为高品位的气体燃料。然而产品气中的高焦油含量居高不下严重限制了气化产品气的应用，生物质的催化热解和水蒸气催化气化被认为是减少其产品气中焦油含量最有效的办法。本文以烟草废弃物为研究对象，对其催化热解和水蒸气气化技术展开了系统的研究，对于揭示生物质热解和气化机理具有重要的意义。
本文中热解和气化实验所使用的烟草废弃物原料，由于原料的原始形状和颗粒大小通常不一致，为了能得到不同粒径大小的样品，便于实验和分析测试，首先要对原材料进行干燥、破碎和筛分。样品理化分析结果表明：烟草废弃物相对煤而言有较低的固定碳含量，较高的挥发份含量。而且原料中元素N和S含量极低，灰分含量小于4%，因此，烟草废弃物是一种环境友好的生物质能源。同时，本文还自制了负载型纳米镍基催化剂，以纳米氧化镍为活性成分，纳米氧化粉体先采用均匀沉淀法制备，再利用沉淀——沉积法将其负载到γ-Al_2O_3载体上得到NiO/γ-Al_2O_3催化剂，并利用APSP2020、SEM、EDX等手段对其进行了表征和分析。结果表明：催化剂有比较高的外表面积和比表面积，其中NiO负载量超过13wt.%，而且活性组分NiO主要集中在催化剂的表面，这种结构有利于NiO的催化作用，同时还能节约成本。
利用TGA-DSC对烟草废弃物热解特性进行了系统的研究，并分析了TG-DTG和DSC曲线了解样品的热失重行为和热解特征参数，同时研究升温速率、颗粒大小和催化剂对生物质热解特性的影响，还利用Doyle和Friedman两种动力学模型计算出生物质热解反应动力学参数E和A。结果表明：样品的热裂解过程分为脱水、烘焙、热解和炭化四个阶段。升温速率的提高和催化剂对烟草废弃物的热解反应速率都有显著提高的作用。
采用TG-GC相结合的方法，开展了烟草废弃物水蒸气催化气化的实验研究，探讨了以NiO和白云石为催化剂，在水蒸气气氛下的烟草废弃物的挥发份析出特性，半焦的气化特性、气化反应动力学特性以及催化剂对气体产物特性的影响。结果表明：样品在水蒸气气氛下的失重过程表现出明显的“两段性”，第一段为挥发分析出阶段，温度范围为217~357℃，水蒸气对此阶段的影响很小，可以忽略不计；第二段为水蒸气与第一阶段剩余的焦炭发生气化反应的阶段，温度范围为717~805℃。气化反应中热解阶段视为一级反应，半焦气化视为缩核反应。催化剂对气化反应有促进作用，提高了气体产物的产量和品质，合成气的产量有明显增加，而焦油的裂解被明显加强。添加NiO时，H2的产率最大，达到34mol/kg；添加白云石时，CO的产率最大，达到23mol/kg。
为了进一步了解烟草废弃物热解机理和热解产物的特性，采用管式电加热炉配合气相色谱仪对烟草废弃物热解产物的分布进行了详细研究，主要考查了热解终温、固相停留时间和催化剂的添加对气体产物特性的影响。研究发现高温有利于H2和CO的产生。在NiO/γ-Al_2O_3催化剂的作用下，在850℃气体产率达到1.52Nm3/kg，H2的含量达到38.6vol.%，气体产物的热值约为15MJ/m3，可以直接用于燃气轮机、引擎和锅炉的燃烧。同时，对整个热解系统在900℃下干燥烟草废弃物的热解过程进行了能量和能量平衡计算分析，结果表明：热解系统建立的质量平衡的误差为1%；因为烟草废弃物热解过程中每一个环节都会存在一定的能量损失，而且原料中存储的化学能也不可能完全转化热解产物的化学能，所以此热解系统的制气效率、能源回收率和能耗比分别为42.16%、89.01%和2.49。
在连续进料的方式下利用实验室规模的鼓泡流化床气化系统，对烟草废弃物水蒸气气化进行了深入研究，主要考查反应温度和S/B对气体产物特性的影响。实验结果表明：随着气化温度从700℃升高至850℃，气体中H2的含量从50.5增加至54.4%，CO的含量从14.3%提高到18.5%，而CO_2和CH_4呈现相反的变化趋势；随着S/B的升高H2的产量先从0.037kg/kg大幅增加到0.07kg/kg，再缓慢增加到0.095kg/kg，最后慢慢趋于平稳甚至减小，所以水蒸气最佳通入量为1.32（S/B）。
此外，由于烟草废弃物水蒸气气化反应的计算结果与实验结果有一定的偏差，因此需要对热力学模型进行适当的修正，从而使得模型计算结果与实验结果更加匹配。模型计算结果表明：各组分气体在几种气化炉温度和S/B工况下的变化趋势与实验结果相似，两者之间RMS误差平均值达到2.990，但模型添加修正系数以后，两者之间的RMS误差平均值降低到1.985，说明修正以后的计算结果跟实验结果更加匹配。
As is known to all, exploring novel energy resource and clean conversion technologieshave become an important and timely research way to solve the excessive use of fossilfuels and the concerns over environmental protection. At present, biomass, as the onlyrenewable energy which can be stored and transported has attracted increasing worldwideinterest. Tobacco has been considered as one of the most important agricultural products inChina. However, tobacco wastes accounted for more than30%of the tobacco plantsproduction which counld not be used for cigarwtte production. Thus, how to treat thistremendous amount of wastes by novel and clean technologies, can promote thedevelopment of social economy, improve ecological environment and establish sustainableenergy system. Biomass thermochemical conversion is considered to be one of the mostefficient ways for converting biomass to bio-oil and bio-char especially for fuel gas whichhas high quality. However, high yield of tar in fuel gas prodution inhibits the furtherdevelopment and commercialization of biomass thermochemical conversion. Catalyticpyrolysis and steam gasification are considered as the most potent technique to decrease taryield, thus to improve the quality of fuel gas. In this study, we carried out an in-depthresearch on tobacco wastes catalytic pyrolysis and steam gasification, which were essentialto understand the fundamentals and mechanisms involved in biomass pyrolysis andgasification.
This study primarily focused on tobacco wastes as feedstock. For analyzing and labresearch, the tobacco wastes needed to be dried, crashed and sieved in different particlesizes so as to get raw materials. The physicochemical property of the feedstock revealedthat tobacco wastes contained lower fixed carbon and more valatiles comparing to coal andthe harmful elements N and S were less than4%, which were of very low contents infeedstock. Thus, tobacco wastes are environment-friendly bioenergy sources. Meanwhile, the NiO/γ-Al_2O_3catalyst was developed in the study. NiO particles which were prepared byhomogeneous precipitation method were an active componet loaded on commercialγ-Al_2O_3carriers in this work. Based on above work, the supported NiO/γ-Al_2O_3catalystsinvolving γ-Al_2O_3as carrier were further exploited by deposition-precipitation Method.Different analytical methods such as APSP2020, SEM and EDX were used to characterizeand analysis the catalysts. The loaded capacity of active component NiO was more than13wt%. The active component NiO were only concentrated on the surface of the catalystswhich can promote catalytic activity and save cost.
Pyrolysis characteristics and kinetics of tobacco wastes were investigated in TGAcoupled with DSC and their kinetics parameters were detemined by using Friedman andDoyle methods, simultaneously, the influence of particle size, heating rate and catalysts onbiomass pyrolysis was analyzed. It was observed that four stage pyrolysis mechanism oftobacco wastes, the first being dehydration, the second at a temperature range oftorrefaction, the third at the pyrolysis temperature range and the fourth stage at thetemperature range of graphitisation. In addition, increasing heating rate and the presence ofcatalysts showed great influence on accelerating thermal degradation.
Tobacco wastes gasification experiments were carried out using thermogravimetricanalyzer and gas chromatographic analyzer (TG-GC). Under the catalytic and non-catalyticcondition, the pyrolysis characteristics, gasification characteristics and kinetics of tobaccowastes were investigated in nitrogen-steam atmosphere. The TGA data indicated the weightloss behavior of the sample in nitrogen-steam mixture was divided into two regions(217~357℃and717~805℃). The volumetric model was used in modeling pyrolysis ofbiomass and the shrinking model was applied for investigating the gasification of pyrolysischars. Both NiO and dolomite could decrease the gasification temperature and enhancewater gas shift reactions. The H2yield (34mol/kg) of tobacco wastes gasification with NiOwas the most. The dolomite had more remarkable effect on improving CO yield (23mol/kg).
For the further information of the characteristics of gas products, tar and charcoal frombiomass pyrolysis, the pyrolysis of tobacco wastes was carried out in fixed-bed reactor withgas chromatograph. The effect of three important reaction parameters such as hearthtemperature, gas/solid residence time and catalysts on the gas product property was focusedon this study. The results showed that higher temperature is favorable for H2and COcontents. With presence of NiO/γ-Al_2O_3catalyst, the yield of fuel gas product reached1.52Nm3/kg with38.6vol.%H2. The calorific value of the fuel gas generated in the process wasabout15MJ/m3, which can be used directly for gas turbine, engine and boiler. Moreover,according to the mass and energy balance evaluation of pyrolysis process of dried tobaccowastes at900℃, the error of mass balance evaluation of dried tobacco wastes is1%. Byenergy evaluation, gas production efficiency, energy recovery and energy consumptionratio of this pyrolysis system were42.16%、89.01%and2.49, respectively.
Furthermore, steam gasification of tobacco wastes was investigated by a home designedbubbling fluidized bed system with continuous feeding. The influence of various technicalparameters such as reactor temperature and Steam/Biomass (S/B) on fuel gas yield andcomposition was analyzed experimentally. It was found that H2and CO contents increasedsteadily from50.5%to54.4%and14.3%to18.5%as the temperature increased from700to850℃, while CO_2and CH_4contents exhibited the opposite tendencies. The yield of H2first increased shaply from0.037kg/kg to0.07kg/kg as the S/B increased to0.5, then itincreased slightly to0.095kg/kg as the S/B continuously increased, finally it trend to astable value or decreased. Thus, the optimum quantity of adding vapour is1.32(S/B).
Moreover, a thermodynamics equilibrium model based on equilibrium constant andmaterial balance has been developed to predict the gas composition which has beencompared with experimental results. Calibration of the model with appropriate modelingcoefficients was necessary to achieve close resemblance with the experimental values. Theresults indicated that the trend of changing the gas compositions with temperature and S/Bwas matching with the experimental results and the average RMS error was2.990. To fit the experimental result, the pre-factor were used to calibrate the equilibrium model. It wasobserved that the average RMS value decreases to1.985. So the modified model predictsthe gas composition much closer to the experimental value.
本文中热解和气化实验所使用的烟草废弃物原料，由于原料的原始形状和颗粒大小通常不一致，为了能得到不同粒径大小的样品，便于实验和分析测试，首先要对原材料进行干燥、破碎和筛分。样品理化分析结果表明：烟草废弃物相对煤而言有较低的固定碳含量，较高的挥发份含量。而且原料中元素N和S含量极低，灰分含量小于4%，因此，烟草废弃物是一种环境友好的生物质能源。同时，本文还自制了负载型纳米镍基催化剂，以纳米氧化镍为活性成分，纳米氧化粉体先采用均匀沉淀法制备，再利用沉淀——沉积法将其负载到γ-Al_2O_3载体上得到NiO/γ-Al_2O_3催化剂，并利用APSP2020、SEM、EDX等手段对其进行了表征和分析。结果表明：催化剂有比较高的外表面积和比表面积，其中NiO负载量超过13wt.%，而且活性组分NiO主要集中在催化剂的表面，这种结构有利于NiO的催化作用，同时还能节约成本。
利用TGA-DSC对烟草废弃物热解特性进行了系统的研究，并分析了TG-DTG和DSC曲线了解样品的热失重行为和热解特征参数，同时研究升温速率、颗粒大小和催化剂对生物质热解特性的影响，还利用Doyle和Friedman两种动力学模型计算出生物质热解反应动力学参数E和A。结果表明：样品的热裂解过程分为脱水、烘焙、热解和炭化四个阶段。升温速率的提高和催化剂对烟草废弃物的热解反应速率都有显著提高的作用。
采用TG-GC相结合的方法，开展了烟草废弃物水蒸气催化气化的实验研究，探讨了以NiO和白云石为催化剂，在水蒸气气氛下的烟草废弃物的挥发份析出特性，半焦的气化特性、气化反应动力学特性以及催化剂对气体产物特性的影响。结果表明：样品在水蒸气气氛下的失重过程表现出明显的“两段性”，第一段为挥发分析出阶段，温度范围为217~357℃，水蒸气对此阶段的影响很小，可以忽略不计；第二段为水蒸气与第一阶段剩余的焦炭发生气化反应的阶段，温度范围为717~805℃。气化反应中热解阶段视为一级反应，半焦气化视为缩核反应。催化剂对气化反应有促进作用，提高了气体产物的产量和品质，合成气的产量有明显增加，而焦油的裂解被明显加强。添加NiO时，H2的产率最大，达到34mol/kg；添加白云石时，CO的产率最大，达到23mol/kg。
为了进一步了解烟草废弃物热解机理和热解产物的特性，采用管式电加热炉配合气相色谱仪对烟草废弃物热解产物的分布进行了详细研究，主要考查了热解终温、固相停留时间和催化剂的添加对气体产物特性的影响。研究发现高温有利于H2和CO的产生。在NiO/γ-Al_2O_3催化剂的作用下，在850℃气体产率达到1.52Nm3/kg，H2的含量达到38.6vol.%，气体产物的热值约为15MJ/m3，可以直接用于燃气轮机、引擎和锅炉的燃烧。同时，对整个热解系统在900℃下干燥烟草废弃物的热解过程进行了能量和能量平衡计算分析，结果表明：热解系统建立的质量平衡的误差为1%；因为烟草废弃物热解过程中每一个环节都会存在一定的能量损失，而且原料中存储的化学能也不可能完全转化热解产物的化学能，所以此热解系统的制气效率、能源回收率和能耗比分别为42.16%、89.01%和2.49。
在连续进料的方式下利用实验室规模的鼓泡流化床气化系统，对烟草废弃物水蒸气气化进行了深入研究，主要考查反应温度和S/B对气体产物特性的影响。实验结果表明：随着气化温度从700℃升高至850℃，气体中H2的含量从50.5增加至54.4%，CO的含量从14.3%提高到18.5%，而CO_2和CH_4呈现相反的变化趋势；随着S/B的升高H2的产量先从0.037kg/kg大幅增加到0.07kg/kg，再缓慢增加到0.095kg/kg，最后慢慢趋于平稳甚至减小，所以水蒸气最佳通入量为1.32（S/B）。
此外，由于烟草废弃物水蒸气气化反应的计算结果与实验结果有一定的偏差，因此需要对热力学模型进行适当的修正，从而使得模型计算结果与实验结果更加匹配。模型计算结果表明：各组分气体在几种气化炉温度和S/B工况下的变化趋势与实验结果相似，两者之间RMS误差平均值达到2.990，但模型添加修正系数以后，两者之间的RMS误差平均值降低到1.985，说明修正以后的计算结果跟实验结果更加匹配。
As is known to all, exploring novel energy resource and clean conversion technologieshave become an important and timely research way to solve the excessive use of fossilfuels and the concerns over environmental protection. At present, biomass, as the onlyrenewable energy which can be stored and transported has attracted increasing worldwideinterest. Tobacco has been considered as one of the most important agricultural products inChina. However, tobacco wastes accounted for more than30%of the tobacco plantsproduction which counld not be used for cigarwtte production. Thus, how to treat thistremendous amount of wastes by novel and clean technologies, can promote thedevelopment of social economy, improve ecological environment and establish sustainableenergy system. Biomass thermochemical conversion is considered to be one of the mostefficient ways for converting biomass to bio-oil and bio-char especially for fuel gas whichhas high quality. However, high yield of tar in fuel gas prodution inhibits the furtherdevelopment and commercialization of biomass thermochemical conversion. Catalyticpyrolysis and steam gasification are considered as the most potent technique to decrease taryield, thus to improve the quality of fuel gas. In this study, we carried out an in-depthresearch on tobacco wastes catalytic pyrolysis and steam gasification, which were essentialto understand the fundamentals and mechanisms involved in biomass pyrolysis andgasification.
This study primarily focused on tobacco wastes as feedstock. For analyzing and labresearch, the tobacco wastes needed to be dried, crashed and sieved in different particlesizes so as to get raw materials. The physicochemical property of the feedstock revealedthat tobacco wastes contained lower fixed carbon and more valatiles comparing to coal andthe harmful elements N and S were less than4%, which were of very low contents infeedstock. Thus, tobacco wastes are environment-friendly bioenergy sources. Meanwhile, the NiO/γ-Al_2O_3catalyst was developed in the study. NiO particles which were prepared byhomogeneous precipitation method were an active componet loaded on commercialγ-Al_2O_3carriers in this work. Based on above work, the supported NiO/γ-Al_2O_3catalystsinvolving γ-Al_2O_3as carrier were further exploited by deposition-precipitation Method.Different analytical methods such as APSP2020, SEM and EDX were used to characterizeand analysis the catalysts. The loaded capacity of active component NiO was more than13wt%. The active component NiO were only concentrated on the surface of the catalystswhich can promote catalytic activity and save cost.
Pyrolysis characteristics and kinetics of tobacco wastes were investigated in TGAcoupled with DSC and their kinetics parameters were detemined by using Friedman andDoyle methods, simultaneously, the influence of particle size, heating rate and catalysts onbiomass pyrolysis was analyzed. It was observed that four stage pyrolysis mechanism oftobacco wastes, the first being dehydration, the second at a temperature range oftorrefaction, the third at the pyrolysis temperature range and the fourth stage at thetemperature range of graphitisation. In addition, increasing heating rate and the presence ofcatalysts showed great influence on accelerating thermal degradation.
Tobacco wastes gasification experiments were carried out using thermogravimetricanalyzer and gas chromatographic analyzer (TG-GC). Under the catalytic and non-catalyticcondition, the pyrolysis characteristics, gasification characteristics and kinetics of tobaccowastes were investigated in nitrogen-steam atmosphere. The TGA data indicated the weightloss behavior of the sample in nitrogen-steam mixture was divided into two regions(217~357℃and717~805℃). The volumetric model was used in modeling pyrolysis ofbiomass and the shrinking model was applied for investigating the gasification of pyrolysischars. Both NiO and dolomite could decrease the gasification temperature and enhancewater gas shift reactions. The H2yield (34mol/kg) of tobacco wastes gasification with NiOwas the most. The dolomite had more remarkable effect on improving CO yield (23mol/kg).
For the further information of the characteristics of gas products, tar and charcoal frombiomass pyrolysis, the pyrolysis of tobacco wastes was carried out in fixed-bed reactor withgas chromatograph. The effect of three important reaction parameters such as hearthtemperature, gas/solid residence time and catalysts on the gas product property was focusedon this study. The results showed that higher temperature is favorable for H2and COcontents. With presence of NiO/γ-Al_2O_3catalyst, the yield of fuel gas product reached1.52Nm3/kg with38.6vol.%H2. The calorific value of the fuel gas generated in the process wasabout15MJ/m3, which can be used directly for gas turbine, engine and boiler. Moreover,according to the mass and energy balance evaluation of pyrolysis process of dried tobaccowastes at900℃, the error of mass balance evaluation of dried tobacco wastes is1%. Byenergy evaluation, gas production efficiency, energy recovery and energy consumptionratio of this pyrolysis system were42.16%、89.01%and2.49, respectively.
Furthermore, steam gasification of tobacco wastes was investigated by a home designedbubbling fluidized bed system with continuous feeding. The influence of various technicalparameters such as reactor temperature and Steam/Biomass (S/B) on fuel gas yield andcomposition was analyzed experimentally. It was found that H2and CO contents increasedsteadily from50.5%to54.4%and14.3%to18.5%as the temperature increased from700to850℃, while CO_2and CH_4contents exhibited the opposite tendencies. The yield of H2first increased shaply from0.037kg/kg to0.07kg/kg as the S/B increased to0.5, then itincreased slightly to0.095kg/kg as the S/B continuously increased, finally it trend to astable value or decreased. Thus, the optimum quantity of adding vapour is1.32(S/B).
Moreover, a thermodynamics equilibrium model based on equilibrium constant andmaterial balance has been developed to predict the gas composition which has beencompared with experimental results. Calibration of the model with appropriate modelingcoefficients was necessary to achieve close resemblance with the experimental values. Theresults indicated that the trend of changing the gas compositions with temperature and S/Bwas matching with the experimental results and the average RMS error was2.990. To fit the experimental result, the pre-factor were used to calibrate the equilibrium model. It wasobserved that the average RMS value decreases to1.985. So the modified model predictsthe gas composition much closer to the experimental value.
引文
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