生物质焦油均相转化及其在焦炭中异相脱除的实验研究
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摘要
我国农村具有丰富的秸秆资源。随着经济的发展，农村对能源的需求不断提高，开发以村为单位的小型生物质气化发电系统是解决这一矛盾的有效途径。当前焦油含量过高是制约生物质气化技术商业应用的瓶颈，二段式下吸气化炉具有气化效率高、焦油含量低的特点，但是，焦油在该炉内的转化及脱除机理仍不清楚，缺乏科学的设计理论和方法。因此，本文将针对二段式气化炉中焦油的转化和脱除机理展开深入研究，构建焦油均相转化路线图和焦油异相催化脱除机理。以揭示二段式气化炉焦油含量低的根本原因，为二段式气化炉工艺优化和运行提供理论依据和实践指导。
二段式气化炉采用部分氧化和炭层转化相分离的工艺来实现焦油的分步转化和脱除，但焦油的脱除是一个系统工程，其脱除不仅受焦油自身生成、转化规律的影响，同时还与转化气氛和起催化脱除作用的焦炭的化学活性密切相关。因此，为了研究热解段及喉口处焦油的生成及均相转化规律，本文针对气化炉内运行条件，在改进的固定床反应器中研究了热解段焦油的生成规律，以及喉口处不同气氛及含量对焦油的均相转化规律。结果表明热解温度及生物质种类是影响热解焦油成分的主要因素，热解焦油一般在500℃之前析出，其焦油成分以酚类、醛类、酮类、呋喃类等含氧类为主。与稻秆相比，松木所产生的焦油中含有较高比例的大分子量初级焦油，而稻秆所产生的焦油中含有较高比例的三级焦油，其原因是稻秆原料中含有更多的碱金属，对初级焦油具有催化转化作用。热解焦油在喉口处的均相转化中，热裂解是最基本的影响因素，而气氛对热解焦油的均相转化具有促进作用。苯、甲苯、苯乙烯、苯酚、萘是典型的均相转化产物，在热解焦油的均相转化产物中占有重要比例（35~80%）。热裂解转化中取代基及杂原子官能团转化的主要温度区间在700~900℃，温度的升高会促进多环芳烃含量的提高，其中萘占主要成分。喉口处喷入O_2、H_2O和CO_2有利于活性自由基O、OH、OH_2等形成，促进焦油的裂解转化，H_2O对焦油转化受H_2O/C比值的影响，浓度过量后效果增长不明显。CO_2对焦油的脱除效果则随浓度的升高而增强，对多环芳烃的脱除作用也越明显。基于实验结果及现有的理论，构建了热解焦油生成及其均相转化路线图。
为了探索生物质焦反应活性在炉内的演变规律，本文在大热重实验台中对影响生物质焦反应活性的三个主要因素即微观物理结构、微观化学结构以及灰分组成及含量演变规律进行了针对性研究。结果表明温度的升高有利于稻秆焦中比表面积的增大，这一变化在500~600℃范围内尤其显著，并在700℃左右达到最大值，随着温度的进一步升高，稻秆焦由于收缩作用比表面积逐渐下降。高温条件下生物质焦微孔占主导地位。喉口对已热解焦炭的影响主要是微孔含量明显增长，孔隙分形维数与比表面积变化规律基本一致，且温度的升高有利于稻秆焦孔隙空间复杂程度的增大，但超过700℃后其分形维数逐渐下降，且过高的温度会降低孔隙表面不规则度。温度的升高使生物质焦中含氧、含氮等活性官能团逐步转化和消失，而含C=C的芳香结构增多，焦炭微观化学结构向芳香化转化，反应活性下降。生物质焦中的碱金属含量和生物质种类密切相关，稻秆具有比松木高得多的K、Na等碱金属含量。随着热解温度的升高，挥发份集中在中前期析出，而碱金属则更多的在中后期析出，因此前期挥发份析出速率较高，整体表现为碱金属相对浓度的不断增大，并在500℃时达到最大，随后碱金属析出速率增大，而焦炭析出逐步停滞，从而碱金属相对浓度逐渐下降。
为了揭示生物质焦催化脱除焦油的作用机理，利用自行搭建的微反应器固定床实验台深入研究了生物质焦对焦油模型化合物萘的脱除规律。结果表明，萘的热裂解产物主要包括甲苯、二甲苯（包含临、间、对）及苯乙烷几种成分。萘在800℃逐渐有炭黑生成，900℃时积炭已很严重。稻秆焦由于积炭失活，对萘的转化率随反应时间的延长而逐渐下降。反应温度和萘浓度的升高会促进催化剂表面的积炭过程。生物质焦积炭主要发生在微孔区域，中、大孔积炭不太明显，新生成的积炭具有比普通生物质焦更高的气化反应特性，且随着积炭含量的增长，气化反应活性也增大，但一旦积炭使微孔堵塞，气化反应活性迅速下降。在有氧化性或重整性气氛存在时，焦炭中催化剂可促进炭的气化反应，进而抑制其结焦过程。根据实验结果及现有的文献理论，构建了生物质焦催化脱除焦油的作用机理。
生物质焦脱除焦油效率随温度的升高而迅速增强，全焦油经焦炭脱除后成分以甲苯为主，二甲苯、苯乙烷及萘其次，其它成分较少。焦炭对多环芳烃类焦油的脱除具有选择性，对多环芳烃类（除萘外）可实现完全脱除。焦炭粒径对焦油转化有明显影响，颗粒越小，对焦油的脱除效率越高，提高炭层高度有利于提高焦油转化率。焦炭对焦油的催化转化随焦炭碱金属含量及比表面积的升高而增大。揭示了二段式气化炉焦油含量低的根本原因在于有效分离了对焦油的脱除具有互补性的均相转化与异相脱除过程。最后提出了二段式气化炉的工艺优化方法。
There is a large number of agriculture residue as crop straw resources in China, alarge parts of them are abandoned without effectively utilizing, on the other side, witheconomic development, rural energy requirement growth continuous. Developing asmall-scale biomass gasification power generation based on distributed energysupplying system is an effective way to resolve this contradiction due to its flexibilityand efficiency. However, high tar content in the syngas is the bottle neck in restrictingthe commercial application of biomass gasification power generation technology. Incurrently, two-stage downdraft gasifier is one of the best gasifier which with higherefficiency, lower tar content than others. However, tar conversion mechanism underhomogeneous and heterogeneous catalytic decomposition remains unclear in the gasifier,which limits its further improvement and utilization.
Tar decomposition processes in the gasifier are interrelated, tar removal is not onlyaffected by the tar formation and conversion properties, but also related to theconversion conditions such as atmosphere and the catalytics. Therefore, the aim of thispaper is to investigate tar conversion and removal mechanism in two-stage downdraftgasifier, by means of constructing the probable road map of tar formation, homogeneousconversion and heterogeneous decomposition, and reveal the catalytic mechanism ofbiomass char decompose tar, provide a theoretical guideline for optimizing tarconversion and removal processes, and optimize the design of the two-stage gasifier.
Pyrolysis tar formation and homogeneous conversion properties wereexperimentally investigated in an improved two-stage fixed bed reactor, includingpyrolysis tar formation factors as pyrolysis temperature, biomass species, particle size,as well as carrying gas flow rate, combined with the feasibility study of throat injectingreforming gas for the tar removal process, and explored the different atmosphere withreforming agents such as H_2O, CO_2and O_2on tar homogeneous conversion properties.There are three kinds of tar analysis methods including qualitative analysis, GC/MScomponent analysis and typical tar component of the GC/MS quantitative analysis. Tarcompounds vary in the formation, conversion process have been studied intensively, and results show that the pyrolysis temperature and the biomass species are the main factorsinfluence of pyrolysis tar composition,400-500℃is a reasonable pyrolysis temperaturerange for tar release. Phenols, aldehydes, ketones and furans consist a major proportionof the pyrolysis tar. In pyrolysis tar homogeneous conversion process, temperature playa significant role, O_2can promote tar cracking by forming active free radicals, thepresence of H_2O can contribute a significant reduction both in tar species and in total.Meanwhile, high concentration of CO_2atmosphere is almost completely transformedpyrolysis tar. Organic mass spectrometry analytical method can effectively analyze thetar thermal cracking pathes. By synthesis analyzing of experimental results and currenttheories, a possible roadmap of pyrolysis tar formation and conversion was constructed.
Three main aspects effect the char reactivity have been investigated in this paper,including micro-physical structure, micro-chemical structure, as well as metallic speciesand content. Evolution properties of micro-physical structure in biomass char vary insurface area, pore size and pore volume with different conditions. The result shows thattemperature has a strong effect in promoting the formation of char porosity, but highertemperature will induce char shrinking and reduce pore content. In porous biomass char,micro pore accounts for the main component, moreover, the fractal dimension values ofchar can be more effective in reflect the complexity of matrix structure than surface area,and the char activity. Micro-chemical structure of oxygen, nitrogen, sugar and aliphaticfunctional groups gradually transformed with preparation temperature increasing, andthe aromatic hydrocarbon structure-containing C=C gradually increased, formingdifferent kinds of aromatic, char chemical reactivity decreased. Alkali metal and alkaliearth metal(AAEM) content depends on biomass species and preparation temperature,the alkali metal concentration in the char has a first increase and then drop, with amaximum value at500℃. Along with the pyrolysis temperature increasing, the totalalkali metal monotonically decrease.
In order to reveal the mechanism and conversion property of biomass char catalyticremoval of tar, an intensive study have been made with biomass char reduce the tarmodel compound as naphthalene in a self-designed bench scale fixed bed micro-reactor.The results show that naphthalene began to yield coke at800℃, and carbon depositionsignificantly improved at900℃. Rice straw char on naphthalene conversion rategradually decreased with time on stream. Increase reaction temperature or naphthaleneconcentration will promote the carbon deposition process on the char active site whichmeans catalyst surface. Low naphthalene concentration8.25g/Nm~3and with charpyrolysis temperature in the600-900℃, rice straw char in the deactivation process can removal naphthalene rate of0.036g/grice straw. Biomass char coke formation occursmainly in the microspore region, less obvious on the macropore region. Coke formedchar with CO_2gasification will be more active than those without coke formed char, butgasification reactivity will be rapidly decreased or even inactivated for char continuescoking exceeds a certain range. Char catalytic mechanism in decomposition tar wasrevealed based on experimental results and exiting theories.
Biomass char catalytic removal of homogeneous converted raw tar compoundshave been concerned. The results indicate that tar species was selectively decomposedin biomass char, such as PAHs species almost completely converted, but parts of onering aromatic tar removal property is less effective. Biomass char can removal the rawtar and the composition of yields tar dominated by toluene, xylene, ethylbenzene andnaphthalene, few other components at900℃. With the same temperature conditions,biomass char can be7~12%higher than thermal cracking in gravimetric tar removalefficiency. Tar removal efficiency will be further improved with higher alkali and alkaliearth metal content in char, smaller particle and longer residence time. Temperature isone of the most significant factors in promoting biomass char removal tar. Toluene is animportant converted product between tar and biomass char interaction. Oxidation orreforming atmosphere exist, biomass char catalyst can also promote the carbongasification reaction, and thus inhibit the coking process. The results reveal the primarycause of low tar contents of syngas in a two-stage downdraft gasifier is the effectivelysegregation and coupling of tar homogeneous conversion process and heterogeneousdecomposition process, which are converted the tar into aromatic one and selectivelydecomposed the aromatic tar, especially PAHs(Polycyclic Aromatic Hydrocarbons).Finally, some suggestions in optimizing process for two-stage downdraft gasifier havebeen proposed.
二段式气化炉采用部分氧化和炭层转化相分离的工艺来实现焦油的分步转化和脱除，但焦油的脱除是一个系统工程，其脱除不仅受焦油自身生成、转化规律的影响，同时还与转化气氛和起催化脱除作用的焦炭的化学活性密切相关。因此，为了研究热解段及喉口处焦油的生成及均相转化规律，本文针对气化炉内运行条件，在改进的固定床反应器中研究了热解段焦油的生成规律，以及喉口处不同气氛及含量对焦油的均相转化规律。结果表明热解温度及生物质种类是影响热解焦油成分的主要因素，热解焦油一般在500℃之前析出，其焦油成分以酚类、醛类、酮类、呋喃类等含氧类为主。与稻秆相比，松木所产生的焦油中含有较高比例的大分子量初级焦油，而稻秆所产生的焦油中含有较高比例的三级焦油，其原因是稻秆原料中含有更多的碱金属，对初级焦油具有催化转化作用。热解焦油在喉口处的均相转化中，热裂解是最基本的影响因素，而气氛对热解焦油的均相转化具有促进作用。苯、甲苯、苯乙烯、苯酚、萘是典型的均相转化产物，在热解焦油的均相转化产物中占有重要比例（35~80%）。热裂解转化中取代基及杂原子官能团转化的主要温度区间在700~900℃，温度的升高会促进多环芳烃含量的提高，其中萘占主要成分。喉口处喷入O_2、H_2O和CO_2有利于活性自由基O、OH、OH_2等形成，促进焦油的裂解转化，H_2O对焦油转化受H_2O/C比值的影响，浓度过量后效果增长不明显。CO_2对焦油的脱除效果则随浓度的升高而增强，对多环芳烃的脱除作用也越明显。基于实验结果及现有的理论，构建了热解焦油生成及其均相转化路线图。
为了探索生物质焦反应活性在炉内的演变规律，本文在大热重实验台中对影响生物质焦反应活性的三个主要因素即微观物理结构、微观化学结构以及灰分组成及含量演变规律进行了针对性研究。结果表明温度的升高有利于稻秆焦中比表面积的增大，这一变化在500~600℃范围内尤其显著，并在700℃左右达到最大值，随着温度的进一步升高，稻秆焦由于收缩作用比表面积逐渐下降。高温条件下生物质焦微孔占主导地位。喉口对已热解焦炭的影响主要是微孔含量明显增长，孔隙分形维数与比表面积变化规律基本一致，且温度的升高有利于稻秆焦孔隙空间复杂程度的增大，但超过700℃后其分形维数逐渐下降，且过高的温度会降低孔隙表面不规则度。温度的升高使生物质焦中含氧、含氮等活性官能团逐步转化和消失，而含C=C的芳香结构增多，焦炭微观化学结构向芳香化转化，反应活性下降。生物质焦中的碱金属含量和生物质种类密切相关，稻秆具有比松木高得多的K、Na等碱金属含量。随着热解温度的升高，挥发份集中在中前期析出，而碱金属则更多的在中后期析出，因此前期挥发份析出速率较高，整体表现为碱金属相对浓度的不断增大，并在500℃时达到最大，随后碱金属析出速率增大，而焦炭析出逐步停滞，从而碱金属相对浓度逐渐下降。
为了揭示生物质焦催化脱除焦油的作用机理，利用自行搭建的微反应器固定床实验台深入研究了生物质焦对焦油模型化合物萘的脱除规律。结果表明，萘的热裂解产物主要包括甲苯、二甲苯（包含临、间、对）及苯乙烷几种成分。萘在800℃逐渐有炭黑生成，900℃时积炭已很严重。稻秆焦由于积炭失活，对萘的转化率随反应时间的延长而逐渐下降。反应温度和萘浓度的升高会促进催化剂表面的积炭过程。生物质焦积炭主要发生在微孔区域，中、大孔积炭不太明显，新生成的积炭具有比普通生物质焦更高的气化反应特性，且随着积炭含量的增长，气化反应活性也增大，但一旦积炭使微孔堵塞，气化反应活性迅速下降。在有氧化性或重整性气氛存在时，焦炭中催化剂可促进炭的气化反应，进而抑制其结焦过程。根据实验结果及现有的文献理论，构建了生物质焦催化脱除焦油的作用机理。
生物质焦脱除焦油效率随温度的升高而迅速增强，全焦油经焦炭脱除后成分以甲苯为主，二甲苯、苯乙烷及萘其次，其它成分较少。焦炭对多环芳烃类焦油的脱除具有选择性，对多环芳烃类（除萘外）可实现完全脱除。焦炭粒径对焦油转化有明显影响，颗粒越小，对焦油的脱除效率越高，提高炭层高度有利于提高焦油转化率。焦炭对焦油的催化转化随焦炭碱金属含量及比表面积的升高而增大。揭示了二段式气化炉焦油含量低的根本原因在于有效分离了对焦油的脱除具有互补性的均相转化与异相脱除过程。最后提出了二段式气化炉的工艺优化方法。
There is a large number of agriculture residue as crop straw resources in China, alarge parts of them are abandoned without effectively utilizing, on the other side, witheconomic development, rural energy requirement growth continuous. Developing asmall-scale biomass gasification power generation based on distributed energysupplying system is an effective way to resolve this contradiction due to its flexibilityand efficiency. However, high tar content in the syngas is the bottle neck in restrictingthe commercial application of biomass gasification power generation technology. Incurrently, two-stage downdraft gasifier is one of the best gasifier which with higherefficiency, lower tar content than others. However, tar conversion mechanism underhomogeneous and heterogeneous catalytic decomposition remains unclear in the gasifier,which limits its further improvement and utilization.
Tar decomposition processes in the gasifier are interrelated, tar removal is not onlyaffected by the tar formation and conversion properties, but also related to theconversion conditions such as atmosphere and the catalytics. Therefore, the aim of thispaper is to investigate tar conversion and removal mechanism in two-stage downdraftgasifier, by means of constructing the probable road map of tar formation, homogeneousconversion and heterogeneous decomposition, and reveal the catalytic mechanism ofbiomass char decompose tar, provide a theoretical guideline for optimizing tarconversion and removal processes, and optimize the design of the two-stage gasifier.
Pyrolysis tar formation and homogeneous conversion properties wereexperimentally investigated in an improved two-stage fixed bed reactor, includingpyrolysis tar formation factors as pyrolysis temperature, biomass species, particle size,as well as carrying gas flow rate, combined with the feasibility study of throat injectingreforming gas for the tar removal process, and explored the different atmosphere withreforming agents such as H_2O, CO_2and O_2on tar homogeneous conversion properties.There are three kinds of tar analysis methods including qualitative analysis, GC/MScomponent analysis and typical tar component of the GC/MS quantitative analysis. Tarcompounds vary in the formation, conversion process have been studied intensively, and results show that the pyrolysis temperature and the biomass species are the main factorsinfluence of pyrolysis tar composition,400-500℃is a reasonable pyrolysis temperaturerange for tar release. Phenols, aldehydes, ketones and furans consist a major proportionof the pyrolysis tar. In pyrolysis tar homogeneous conversion process, temperature playa significant role, O_2can promote tar cracking by forming active free radicals, thepresence of H_2O can contribute a significant reduction both in tar species and in total.Meanwhile, high concentration of CO_2atmosphere is almost completely transformedpyrolysis tar. Organic mass spectrometry analytical method can effectively analyze thetar thermal cracking pathes. By synthesis analyzing of experimental results and currenttheories, a possible roadmap of pyrolysis tar formation and conversion was constructed.
Three main aspects effect the char reactivity have been investigated in this paper,including micro-physical structure, micro-chemical structure, as well as metallic speciesand content. Evolution properties of micro-physical structure in biomass char vary insurface area, pore size and pore volume with different conditions. The result shows thattemperature has a strong effect in promoting the formation of char porosity, but highertemperature will induce char shrinking and reduce pore content. In porous biomass char,micro pore accounts for the main component, moreover, the fractal dimension values ofchar can be more effective in reflect the complexity of matrix structure than surface area,and the char activity. Micro-chemical structure of oxygen, nitrogen, sugar and aliphaticfunctional groups gradually transformed with preparation temperature increasing, andthe aromatic hydrocarbon structure-containing C=C gradually increased, formingdifferent kinds of aromatic, char chemical reactivity decreased. Alkali metal and alkaliearth metal(AAEM) content depends on biomass species and preparation temperature,the alkali metal concentration in the char has a first increase and then drop, with amaximum value at500℃. Along with the pyrolysis temperature increasing, the totalalkali metal monotonically decrease.
In order to reveal the mechanism and conversion property of biomass char catalyticremoval of tar, an intensive study have been made with biomass char reduce the tarmodel compound as naphthalene in a self-designed bench scale fixed bed micro-reactor.The results show that naphthalene began to yield coke at800℃, and carbon depositionsignificantly improved at900℃. Rice straw char on naphthalene conversion rategradually decreased with time on stream. Increase reaction temperature or naphthaleneconcentration will promote the carbon deposition process on the char active site whichmeans catalyst surface. Low naphthalene concentration8.25g/Nm~3and with charpyrolysis temperature in the600-900℃, rice straw char in the deactivation process can removal naphthalene rate of0.036g/grice straw. Biomass char coke formation occursmainly in the microspore region, less obvious on the macropore region. Coke formedchar with CO_2gasification will be more active than those without coke formed char, butgasification reactivity will be rapidly decreased or even inactivated for char continuescoking exceeds a certain range. Char catalytic mechanism in decomposition tar wasrevealed based on experimental results and exiting theories.
Biomass char catalytic removal of homogeneous converted raw tar compoundshave been concerned. The results indicate that tar species was selectively decomposedin biomass char, such as PAHs species almost completely converted, but parts of onering aromatic tar removal property is less effective. Biomass char can removal the rawtar and the composition of yields tar dominated by toluene, xylene, ethylbenzene andnaphthalene, few other components at900℃. With the same temperature conditions,biomass char can be7~12%higher than thermal cracking in gravimetric tar removalefficiency. Tar removal efficiency will be further improved with higher alkali and alkaliearth metal content in char, smaller particle and longer residence time. Temperature isone of the most significant factors in promoting biomass char removal tar. Toluene is animportant converted product between tar and biomass char interaction. Oxidation orreforming atmosphere exist, biomass char catalyst can also promote the carbongasification reaction, and thus inhibit the coking process. The results reveal the primarycause of low tar contents of syngas in a two-stage downdraft gasifier is the effectivelysegregation and coupling of tar homogeneous conversion process and heterogeneousdecomposition process, which are converted the tar into aromatic one and selectivelydecomposed the aromatic tar, especially PAHs(Polycyclic Aromatic Hydrocarbons).Finally, some suggestions in optimizing process for two-stage downdraft gasifier havebeen proposed.
引文
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