澳大利亚小桉树流化床快速热解的研究
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摘要
生物质热解是当前国际上生物质能研究的前沿技术之一。流化床快速热解技术由于具有高传热速率,一致的床层温度,较短的气相停留时间,可以抑制热解蒸气的二次裂解等优点,有利于提高生物油产量,因而受到广泛应用。该技术能以连续进料的工艺将生物质转化为高品质的易储存、易运输、能量密度高且使用方便的代用液体燃料(生物油)。小桉树是澳大利亚西澳州用于治理土地盐渍化而广泛种植在小麦条带间的一种灌木桉树,其具有耐干旱、成材迅速、产量大等优点。
在以往的生物质热解实验研究中,人们更多的将研究的重点放在油产率的最大化,但是考虑到生物油的最终用途及其对油品质的要求,本文同时也研究了生物质热解的产物分布、热解生成的生物油的性质及化学组成。在实际工业生产中,包含植物的各部分(木质部分和树叶)的小桉树将会被整体送入反应装置中热解制油,因此分别研究清楚小桉树的木质部分和树叶的热解行为,以及各部分热解所生成的生物油的性质非常必要。
基于此本论文依托澳大利亚第二代生物能源技术政府科研基金项目,在流化床热解反应器上较系统地研究了热解参数(热解温度、生物质粒度、生物质中碱金属和碱土金属的含量等)对小桉树各部分(木质部分和树叶)热解产物产率以及生物油化学组成的影响。主要包括以下研究内容和结论：
1.本文在实验室规模流化床热解反应器上研究了温度(350-580℃)对小桉树木质部分热解产物的产率的影响,并通过热重分析、扫描电镜、生物油粘度测试、生物油元素分析、生物油的水含量测试、生物油热值测试等方法对小桉树木质部分原料和热解油进行了分析,探讨了温度对小桉树木质部分热解汕的物理性质和化学组成的影响,得出以下结论：热解温度对热解产物的产率有显著影响,热解温度在450℃时,生物汕的产率达到最大值(65%)；在生物油产率最高的温度范围热解制得的生物油中木质素衍生的聚合物的含量最高,并且生物油的水含量最低,使得生物油的粘度最高,同时生物油的热值最高,品质最好,即获得生物油产率最高的热解温度范围与获得较高品质的生物油的温度范围完全吻合；在350-500℃的温度范围内,生物油产率随热解温度升高而增大主要是由生物油中的木质素聚合物(不溶于水不但溶于二氯甲烷组分)产率升高引起的。
2.采用生物质流化床快速热解装置研究了生物质粒度对小桉树木质部分热解产率和热解油的组成及化学性质的影响,通过热重分析、生物油粘度测试、生物油的水含量测试、冷水萃取法、紫外荧光光谱方法等方法和技术对小桉树木质部分热解油进行了分析,得出以下结论：当生物质粒度从0.38mm增大到1.7mmm时,生物油的产率明显降低(约11-13%),生物焦和热解气的产率明显升高,分别升高8%和6%；当生物质的粒度从1.7mm继续增大到5.38mm时,生物质热解产物产率不再发生明显变化。生物油的粘度随粒径的变化规律正好与油产率的变化相一致,均随着生物质粒度的增大而降低；生物油中水含量随生物质粒度的增大而升高以及生物油中分子量较高的木质素聚合物的含量随生物质粒度的增大而降低是油粘度变化的原因；通过对不同粒度生物质热解制得的生物油的TGA族组分分析得到,生物质粒度越大,生物质热解油中轻组分产率越高,重组分产率越低。
3.采用流化床快速热解装置研究了碱金属和碱土金属的脱除对小桉树木质部分热解产物产率和热解油的组成及化学性质的影响,通过热重分析、生物油粘度测试、生物油的水含量测试、冷水萃取法、紫外荧光光谱方法等方法和技术对小桉树木质部分热解油进行了分析,得出以下结论：生物质中的AAEM在生物质中以水可脱除的和水不可脱除但酸可脱除两种形式存在；经过水洗和酸洗预处理的后生物质热解产率均没有明显变化,但是生物油的组成却发生明显变化,尤其是水不可脱除但酸可脱除的AAEM对生物油组成的影响显著；生物质中的AAEM的脱除(尤其是水不可脱除但酸可脱除的AAEM),会导致生物油中糖类和木质素聚合物等重组分的含量增加,以及水和轻组分含量的下降,造成生物油粘度增加,使生物油变“重”。
4.由于树叶热解制得的蒸气与最终冷凝所得的生物汕与木质部分热解所得的蒸气及生物油相比,具有更高的粘结性,很容易造成生物油冷凝和收集系统的堵塞。针对这个问题,本实验对原装置的冷凝系统进行了设计和改造。
在改造后的反应器上对小桉树树叶在不同温度下(300-580℃)的热解行为进行了研究。采用Karl-Fisher水分测定仪、冷水萃取法、旋转粘度计、热重分析仪、傅里叶变换红外光谱、气相色谱-质谱联用、紫外荧光光谱等对生物质油进行分析。实验结果表明小桉树的树叶和木质部分均可通过热解实现较高的油产率,成为生物能源的优质原料。小桉树树叶在各温度下热解油产率均低于小桉树木质部分热解油产率。小桉树树叶热解油的产率在热解温度为400-450℃达到最大值,为52.6%。树叶热解油中的水不溶组分含量远高于木质部分热解油。桉脑油是桉树树叶热解液体产物中特有的且含量最丰富的单体化合物。在小桉树树叶热解油中源自纤维素和半纤维素的化合物(左旋葡聚糖、酸类和醛类)产率也低于木质部分热解油中相应化合物。树叶热解的生物焦产率高于木质部分,原因是由于桉树树叶中含量较高的“萃取物”所致。小桉树树叶热解油的芳香性随着热解温度的升高而增加。
Biomass pyrolysis is one of the cutting-edge technologies for the research of bio-energy in the world. Fluidised-bed fast pyrolysis technology has advantages such as high heat transfer rate, uniform bed temperature, short residence time to inhibit second cracking, etc. so has been widely used in the biomass pyrolysis research to obtain high bio-oil yield. Fluidised-bed fast pyrolysis technology can convert biomass into high quality liquid fuel (bio-oil) using continual feeding. Mallee biomass is grown in Australia to combat the existing salinity problem in the Western Australian wheat belt, due to its performance in fast growing, high yield and drought tolerance.
In the past research on biomass pyrolysis, a lot of work has been done in maximizing bio-oil yield. However, considering the final use and its request for the oil quality, pyrolysis products distribution, property and chemical composition of bio-oil have been intensively studied in this thesis. For practical production facility, the entire tree (including woody trunk and leaves) will be delivered in the reactor to produce biofuels. Understanding the pyrolysis behaviour of woody trunk and leaves would thus be an important aspect of the biofuel technology development. Based on above described necessarity, the effects of pyrolysis parameters (temperature, particle size of biomass, the removal of AAEM) on mallee woody trunk and leaves pyrolysis products yield and bio-oil composition have been systematically studied. The main research work and conclusions are listed as following:
1. This paper presents an investigation of the effect of temperature on yield of pyrolysis products and bio-oil property through characterization method of thermogravimetric analysis, scanning electron microscope, viscosity analysis, elemental analysis, water content analysis and heating value analysis. The research results show that the yields of pyrolysis products were significantly influenced by the pyrolysis temperature. The maximum yield of bio-oil and minimum content of water in bio-oil were achieved at the same pyrolysis temperature range (450-475℃). It was shown that the conditions for maximizing bio-oil yield also led to the formation of the largest amounts of small lignin-derived oligomers as a part of bio-oil, resulting in a bio-oil with the highest viscosity and highest heating value. The increases in oil yield with increasing temperature from350to500℃were mainly due to the increases in the production of lignin-derived oligomers insoluble in water but soluble in CH2C12.
2. The effect of particle size on yield of pyrolysis products and bio-oil propoty was studied in a fluidized-bed reactor, and the bio-oil was analyzed by technologies/method of thermogravimetric analysis, UV-fluorescence spectroscopy, viscosity analysis, water content analysis and cold water precipitation analysis. The research results show that the yield of bio-oil decreased as the average biomass particle size was increased from0.3to about1.5mm. Further increases in biomass particle size failed result in any further decreases in the pyrolysis products yield. The viscosity of bio-oil decrease with increasing particle size as well, which paralled the changing trend of bio-oil yield. The increase of water content in bio-oil and and the decrease of the content lignin derived oligmor with increasing particle size could explain the changing trend of bio-oil viscosity. It can be learned from the TGA analysis of the bio-oil that the biomass with larger particle size could result in higer yield of light components in bio-oil.
3. The effects of inorganic species in biomass, especially the alkali and alkaline earth metallic (AAEM) species (K, Na, Mg and Ca) on the yield and property of bio-oil from the pyrolysis of biomass was investiated. The bio-oil was characterized by thermogravimetric analysis, UV-fluorescence spectroscopy, viscosity analysis, water content analysis and cold water precipitation analysis. The research results show that AAEM species exist in the wood in two different forms:water-soluble and water-insoluble but acid-soluble. The removal of AAEM species did not result in significant changes in the yields of bio-oil and bio-char. However, the bio-oil properties, e.g.viscosity, were drastically affected by the removal of AAEM species. The water-soluble AAEM species were not as important as the waterinsoluble but acid-soluble AAEM species in influencing the bio-oil composition and properties. It is believed that the acid-soluble AAEM species (especially Ca) were more closely linked with the organic matter in biomass and thus were closely involved in the reactions during pyrolysis. The removal of AAEM species, especially the acid-soluble AAEM species, led to very significant increases in the yields of sugars and lignin-derived oligomers, accompanied by decreases in the yields of water and light organic compounds in the bio-oil.
4. The viscous nature of the bio-oil from the pyrolysis of leaves cause the bio-oil condensation and collection system to block easily, necessitating modifications to ensure uninterrupted pyrolysis experiments.
The pyrolysis behaviour of mallee leaves at different temperatures has been studied using a modified fluidised-bed reactor. The bio-oils have been characterised with Karl Fischer titration, TGA, UV-fluorescence spectroscopy, FTIR spectroscopy and GC-MS. These results show that the yields and composition/properties of bio-oils from leaves are quite different from those obtained from the pyrolysis of the woody fraction of the same mallee tree species. Both wood and leaves give good yields of bio-oils and therefore are suitable feedstocks for biofuel production. Notably, the amount of water-insoluble compounds present in leaf bio-oils occur in much higher concentration than in wood bio-oils. Eucalyptol is the most abundant simple compound identified in the liquid product. Char yields of leaves are also higher than the woody fraction, partly due to the increased fraction of "extractives", which include other compounds not included in the usual classification of woody biomass.
在以往的生物质热解实验研究中,人们更多的将研究的重点放在油产率的最大化,但是考虑到生物油的最终用途及其对油品质的要求,本文同时也研究了生物质热解的产物分布、热解生成的生物油的性质及化学组成。在实际工业生产中,包含植物的各部分(木质部分和树叶)的小桉树将会被整体送入反应装置中热解制油,因此分别研究清楚小桉树的木质部分和树叶的热解行为,以及各部分热解所生成的生物油的性质非常必要。
基于此本论文依托澳大利亚第二代生物能源技术政府科研基金项目,在流化床热解反应器上较系统地研究了热解参数(热解温度、生物质粒度、生物质中碱金属和碱土金属的含量等)对小桉树各部分(木质部分和树叶)热解产物产率以及生物油化学组成的影响。主要包括以下研究内容和结论：
1.本文在实验室规模流化床热解反应器上研究了温度(350-580℃)对小桉树木质部分热解产物的产率的影响,并通过热重分析、扫描电镜、生物油粘度测试、生物油元素分析、生物油的水含量测试、生物油热值测试等方法对小桉树木质部分原料和热解油进行了分析,探讨了温度对小桉树木质部分热解汕的物理性质和化学组成的影响,得出以下结论：热解温度对热解产物的产率有显著影响,热解温度在450℃时,生物汕的产率达到最大值(65%)；在生物油产率最高的温度范围热解制得的生物油中木质素衍生的聚合物的含量最高,并且生物油的水含量最低,使得生物油的粘度最高,同时生物油的热值最高,品质最好,即获得生物油产率最高的热解温度范围与获得较高品质的生物油的温度范围完全吻合；在350-500℃的温度范围内,生物油产率随热解温度升高而增大主要是由生物油中的木质素聚合物(不溶于水不但溶于二氯甲烷组分)产率升高引起的。
2.采用生物质流化床快速热解装置研究了生物质粒度对小桉树木质部分热解产率和热解油的组成及化学性质的影响,通过热重分析、生物油粘度测试、生物油的水含量测试、冷水萃取法、紫外荧光光谱方法等方法和技术对小桉树木质部分热解油进行了分析,得出以下结论：当生物质粒度从0.38mm增大到1.7mmm时,生物油的产率明显降低(约11-13%),生物焦和热解气的产率明显升高,分别升高8%和6%；当生物质的粒度从1.7mm继续增大到5.38mm时,生物质热解产物产率不再发生明显变化。生物油的粘度随粒径的变化规律正好与油产率的变化相一致,均随着生物质粒度的增大而降低；生物油中水含量随生物质粒度的增大而升高以及生物油中分子量较高的木质素聚合物的含量随生物质粒度的增大而降低是油粘度变化的原因；通过对不同粒度生物质热解制得的生物油的TGA族组分分析得到,生物质粒度越大,生物质热解油中轻组分产率越高,重组分产率越低。
3.采用流化床快速热解装置研究了碱金属和碱土金属的脱除对小桉树木质部分热解产物产率和热解油的组成及化学性质的影响,通过热重分析、生物油粘度测试、生物油的水含量测试、冷水萃取法、紫外荧光光谱方法等方法和技术对小桉树木质部分热解油进行了分析,得出以下结论：生物质中的AAEM在生物质中以水可脱除的和水不可脱除但酸可脱除两种形式存在；经过水洗和酸洗预处理的后生物质热解产率均没有明显变化,但是生物油的组成却发生明显变化,尤其是水不可脱除但酸可脱除的AAEM对生物油组成的影响显著；生物质中的AAEM的脱除(尤其是水不可脱除但酸可脱除的AAEM),会导致生物油中糖类和木质素聚合物等重组分的含量增加,以及水和轻组分含量的下降,造成生物油粘度增加,使生物油变“重”。
4.由于树叶热解制得的蒸气与最终冷凝所得的生物汕与木质部分热解所得的蒸气及生物油相比,具有更高的粘结性,很容易造成生物油冷凝和收集系统的堵塞。针对这个问题,本实验对原装置的冷凝系统进行了设计和改造。
在改造后的反应器上对小桉树树叶在不同温度下(300-580℃)的热解行为进行了研究。采用Karl-Fisher水分测定仪、冷水萃取法、旋转粘度计、热重分析仪、傅里叶变换红外光谱、气相色谱-质谱联用、紫外荧光光谱等对生物质油进行分析。实验结果表明小桉树的树叶和木质部分均可通过热解实现较高的油产率,成为生物能源的优质原料。小桉树树叶在各温度下热解油产率均低于小桉树木质部分热解油产率。小桉树树叶热解油的产率在热解温度为400-450℃达到最大值,为52.6%。树叶热解油中的水不溶组分含量远高于木质部分热解油。桉脑油是桉树树叶热解液体产物中特有的且含量最丰富的单体化合物。在小桉树树叶热解油中源自纤维素和半纤维素的化合物(左旋葡聚糖、酸类和醛类)产率也低于木质部分热解油中相应化合物。树叶热解的生物焦产率高于木质部分,原因是由于桉树树叶中含量较高的“萃取物”所致。小桉树树叶热解油的芳香性随着热解温度的升高而增加。
Biomass pyrolysis is one of the cutting-edge technologies for the research of bio-energy in the world. Fluidised-bed fast pyrolysis technology has advantages such as high heat transfer rate, uniform bed temperature, short residence time to inhibit second cracking, etc. so has been widely used in the biomass pyrolysis research to obtain high bio-oil yield. Fluidised-bed fast pyrolysis technology can convert biomass into high quality liquid fuel (bio-oil) using continual feeding. Mallee biomass is grown in Australia to combat the existing salinity problem in the Western Australian wheat belt, due to its performance in fast growing, high yield and drought tolerance.
In the past research on biomass pyrolysis, a lot of work has been done in maximizing bio-oil yield. However, considering the final use and its request for the oil quality, pyrolysis products distribution, property and chemical composition of bio-oil have been intensively studied in this thesis. For practical production facility, the entire tree (including woody trunk and leaves) will be delivered in the reactor to produce biofuels. Understanding the pyrolysis behaviour of woody trunk and leaves would thus be an important aspect of the biofuel technology development. Based on above described necessarity, the effects of pyrolysis parameters (temperature, particle size of biomass, the removal of AAEM) on mallee woody trunk and leaves pyrolysis products yield and bio-oil composition have been systematically studied. The main research work and conclusions are listed as following:
1. This paper presents an investigation of the effect of temperature on yield of pyrolysis products and bio-oil property through characterization method of thermogravimetric analysis, scanning electron microscope, viscosity analysis, elemental analysis, water content analysis and heating value analysis. The research results show that the yields of pyrolysis products were significantly influenced by the pyrolysis temperature. The maximum yield of bio-oil and minimum content of water in bio-oil were achieved at the same pyrolysis temperature range (450-475℃). It was shown that the conditions for maximizing bio-oil yield also led to the formation of the largest amounts of small lignin-derived oligomers as a part of bio-oil, resulting in a bio-oil with the highest viscosity and highest heating value. The increases in oil yield with increasing temperature from350to500℃were mainly due to the increases in the production of lignin-derived oligomers insoluble in water but soluble in CH2C12.
2. The effect of particle size on yield of pyrolysis products and bio-oil propoty was studied in a fluidized-bed reactor, and the bio-oil was analyzed by technologies/method of thermogravimetric analysis, UV-fluorescence spectroscopy, viscosity analysis, water content analysis and cold water precipitation analysis. The research results show that the yield of bio-oil decreased as the average biomass particle size was increased from0.3to about1.5mm. Further increases in biomass particle size failed result in any further decreases in the pyrolysis products yield. The viscosity of bio-oil decrease with increasing particle size as well, which paralled the changing trend of bio-oil yield. The increase of water content in bio-oil and and the decrease of the content lignin derived oligmor with increasing particle size could explain the changing trend of bio-oil viscosity. It can be learned from the TGA analysis of the bio-oil that the biomass with larger particle size could result in higer yield of light components in bio-oil.
3. The effects of inorganic species in biomass, especially the alkali and alkaline earth metallic (AAEM) species (K, Na, Mg and Ca) on the yield and property of bio-oil from the pyrolysis of biomass was investiated. The bio-oil was characterized by thermogravimetric analysis, UV-fluorescence spectroscopy, viscosity analysis, water content analysis and cold water precipitation analysis. The research results show that AAEM species exist in the wood in two different forms:water-soluble and water-insoluble but acid-soluble. The removal of AAEM species did not result in significant changes in the yields of bio-oil and bio-char. However, the bio-oil properties, e.g.viscosity, were drastically affected by the removal of AAEM species. The water-soluble AAEM species were not as important as the waterinsoluble but acid-soluble AAEM species in influencing the bio-oil composition and properties. It is believed that the acid-soluble AAEM species (especially Ca) were more closely linked with the organic matter in biomass and thus were closely involved in the reactions during pyrolysis. The removal of AAEM species, especially the acid-soluble AAEM species, led to very significant increases in the yields of sugars and lignin-derived oligomers, accompanied by decreases in the yields of water and light organic compounds in the bio-oil.
4. The viscous nature of the bio-oil from the pyrolysis of leaves cause the bio-oil condensation and collection system to block easily, necessitating modifications to ensure uninterrupted pyrolysis experiments.
The pyrolysis behaviour of mallee leaves at different temperatures has been studied using a modified fluidised-bed reactor. The bio-oils have been characterised with Karl Fischer titration, TGA, UV-fluorescence spectroscopy, FTIR spectroscopy and GC-MS. These results show that the yields and composition/properties of bio-oils from leaves are quite different from those obtained from the pyrolysis of the woody fraction of the same mallee tree species. Both wood and leaves give good yields of bio-oils and therefore are suitable feedstocks for biofuel production. Notably, the amount of water-insoluble compounds present in leaf bio-oils occur in much higher concentration than in wood bio-oils. Eucalyptol is the most abundant simple compound identified in the liquid product. Char yields of leaves are also higher than the woody fraction, partly due to the increased fraction of "extractives", which include other compounds not included in the usual classification of woody biomass.
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