生物质与煤共热解气化行为特性及动力学研究
摘要
生物质与煤共热解是一项极具开发潜力的技术，在国内外仍属较新领域，其核心是共热解中协同反应效应的相关问题。本论文研究在现有实验室条件下，全面分析了六种形式的生物质与煤共热解过程，考察其中的协同反应效应，利用分布活化能法（DAEM）研究生物质与煤的共热解动力学特性，得出共热解动力学相关参数，为实现生物质与煤高效协同共热解反应寻找更为有效的途径。主要内容和研究成果归纳如下：
1.生物质与煤慢速共热解行为研究
采用TG-FTIR联用的分析方法对生物质与煤单独热解及共热解过程进行分析。结果发现，生物质与煤共热解的实际热失重过程较理论计算值程度有所加深，褐煤与生物质的共热解效果最好；共热解协同作用主要体现在较高温段生物质对煤的催化作用。根据TG-FTIR的实验结果推测，生物质中的Fe、Ca、Mg、Si等微量元素的氧化物，在共热解过程中破坏煤胶质体的形成，使得煤炭热解初期的产物气体得以逸出，从而增加共热解过程气体产率，降低液体产率；自制的镍铁白云石基双金属催化剂进一步促进了共热解反应发生的深度，提高了共热解过程中碳的转化率和原料利用率。
2.生物质与煤快速共热解行为研究
在小型固定床反应器上，对生物质与煤快速共热解过程进行研究，发现：温度对生物质与煤快速共热解反应影响比较明显，温度越高，产气率和H2含量越大，固体得率越低，气体和固体得率及气体组分理论值与实际值的偏差，说明快速共热解过程中存在协同反应；生物质与煤快速共热解产气量随生物质在原料中掺混比例的增加而增加；生物质与煤快速共热解反应有利于产生富氢热解气，尤其是木屑与烟煤在B:C=2:8(Wt/Wt)的条件下生成的热解气中H2所占比例达42.53%，CO产率随着生物质在原料中所占比例的增加而降低，CO2实际产率低于理论计算值，CH_4产率随着煤化程度和生物质在原料中所占比例的增加逐渐降低，其他烃类的产量增加。
3.生物质与煤快速共气化行为研究
在小型固定床反应器上，采用快速升温的方式，考察生物质与煤水蒸气快速共气化和加水快速共气化两种方式对共气化过程及产物的影响。生物质与煤水蒸气快速共气化反应可生产富氢产物气，明显降低CO及烃类气体产率，H_2/CO可达3-4，对CO_2产量影响不是很明显；生物质与煤加水快速共气化气体产量也有显著增加，随着加水共气化终温的升高，气体产物中H_2组分所占比例明显增加，而CO组分所占比例略有下降。两种共气化方式相比，水蒸气共气化法产生富氢气体，适用于合成液体燃料，尤其是作为甲醇合成的原料气；而直接加水气化得到较多的可燃气体，燃气热值较高，可用来燃烧、发电及供气。
4.烘焙生物质与煤共热解行为研究
采用TG和小型固定床两种反应器形式分别对烘焙生物质与煤慢速共热解和快速共热解过程及产物进行研究。通过慢速共热解研究，发现250℃和30min是一个比较合适的生物质原料预处理温度。烘焙预处理有利于生物质与褐煤快速共热解气体产物的生成。各气体组分中，H2含量减少很多，CO含量略有增加，CO_2含量增加，CmHn含量增加较多，但气体热值总体变化不大。生物质经烘焙预处理后与煤快速共热解反应能有效降低焦油产量。
5.生物质与煤共热解及焦油催化裂解动力学研究
分别采用Coats-Redfern法和DAEM法对生物质与煤共热解过程的动力学特性加以分析。Coats-Redfern法中，升温速率对活化能影响不大，对频率因子有一定的影响。Coats-Redfern法将共热解过程分为多段的单一反应，求出的活化能值较低，且为整个共热解过程活化能的平均值，不能全面准确的表达生物质、煤单独热解或两者混合物的共热解活化能和实际过程，因而不适宜于模拟共热解等复杂反应体系；DAEM模型求得的活化能是随转化率变化的一个函数，呈现升高-平稳-升高的变化趋势，指前因子随活化能的增大而增大，补偿了由于活化能增大而造成的速度常数减少。DAEM法的Gaussian拟合相关性较好，充分证明了DAEM模型对共热解过程的适用性较好。实验得到的共热解活化能小于加权计算方法得到的共热解活化能，进一步验证了在共热解过程中协同反应效应的真实存在。
以萘为模型化合物模拟焦油的催化裂解反应可以看做是平推流反应形式。在自制的镍铁白云石基双金属复合催化剂上，950℃时萘的转化率达到93%以上，求得的表观活化能为63.96kJ/mol，为目前所能检索到的最小。以萘为模型化合物的焦油催化裂解本征动力学方程为：r_A=396.2×exp(-925.34×1/T)C_A
Biomass and coal co-pyrolysis is a great potential technology and a relative new researchfield in the world. Its core problem is the synergistic effect of co-pyrolysis. Under ourlaboratory conditions, the co-pyrolysis synergistic effect of6kinds of biomasses and coalswere studied and investigated in this thesis. Distribution activation energy method (DAEM)was introduced into this thesis to study the co-pyrolysis kinetics of biomass and coal, and to getthe co-pyrolysis related kinetics parameters. The aim of this thesis is to find more effectiveways to achieve the synergistic effect in biomass and coal co-pyrolysis. This main researchcontents and results are summarized as follows:
1. Slow co-pyrolysis behavior of biomass and coal
Mono-pyrolysis and co-pyrolysis of biomass and coal were studied by using the TG-FTIRtechnology. It is found that the actual co-pyrolysis degrees are deeper than the theoretical ones.The effect of biomass and lignite co-pyrolysis is the best with actual results deviatingtheoretical value greatly. The synergistic effects are expressed as the biomass catalytic effect oncoal at high temperature region. According to results of the TG-FTIR, it can be concluded thatthe oxides of Fe, Ca, Mg, Si, and other trace elements in biomass inhibit the formation of coalcolloid, and make the initial gas product of coal pyrolysis be able to escape. Synergistic effectaccelerates coal pyrolysis to produce gas and decrease liquid products. The bimetallic dolomitebased catalyst further promotes the co-pyrolysis reaction, and improves the carbon conversionrates and utilization of raw materials in the co-pyrolysis process.
2. Fast co-pyrolysis behavior of biomass and coal
Fast co-pyrolysis process of biomass and coal were studied in a small fixed-bed reactor. Itis found that the pyrolysis temperature impact on fast co-pyrolysis of biomass and coalsignificantly. The synergistic effect is more obvious in the higher temperature. With theincrease of temperature, the H_2content and gas product yields increase, and the solid productyields greatly decrease. The deviation of theoretical value and actual value of co-pyrolysis gas and solid yields fully prove that the synergistic effect in fast co-pyrolysis process. Gasproductions increase with incremental biomass ratio in blending raw material. Biomass andcoal fast co-pyrolysis reaction can obtain hydrogen-rich gaseous products. Especially, when theratio of sawdust to bituminous is2to8, fast co-pyrolysis reactions get highest H2content of42.53%. The CO production decreases in higher biomass mixing ratio. The CO_2actual yield islower than the theoretical value. The CH_4yield decrease with the coal rank and biomass to coalratio increase. However, co-pyrolysis process effectively improves the production of otherhydrocarbons.
3. Fast co-gasification behavior of biomass and coal
Steam fast co-gasification and mixing water fast co-gasification processes were studied ina small fixed-bed reactor by fast heating-up mode. Steam fast co-gasification of biomass andcoal can produce hydrogen-rich gaseous products, and promote the H_2/CO to3-4, butsignificantly reduces the yield of CO and hydrocarbon. CO_2production change of this processis not very remarkable. Mixing water fast co-gasification process of biomass and coal canpromote the synergistic effect occur. The gaseous product yield of biomass and coal mixingwater fast co-gasification significantly increases. With the co-gasification reaction temperaturerise, the H2content increases significantly, while a slight decrease for the CO content occurs.Comparing the two methods of co-gasification, it can be concluded that steam fastco-gasification get the hydrogen-rich gas which is suitable for synthesizing liquid fuels,especially as the raw gas of methanol synthesis, while mixing water fast co-gasification getmuch higher heat value combustible gas which can be used for burning, power generation andgas supply.
4. Co-pyrolysis behavior of torrefaction biomass and coal
The process and product of slow and fast co-pyrolysis of torrefied biomass and coal werestudied by TG analysis technique and a small fixed-bed reactor respectively. In the slowco-pyrolysis research, it can be concluded that250℃and30min is a suitable torrefactioncondition for biomass. The torrefaction of biomass is better for biomass and lignite fast co-pyrolysis to get more gaseous product. Fast co-pyrolysis reactions of torrefaction biomassand coal have the effect of reducing H2content significantly, increasing CO content a bit andaccruing CO2and CmHncontent vastly. However, the heat values of gaseous product arechanged slightly. Fast co-pyrolysis of torrefied biomass and coal has a positive effect onlowering tar yield.
5. Kinetic analysis of biomass and coal co-pyrolysis and tar catalytic cracking
In this part, Coats-Redfern and DAEM methods were used to analyze the dynamiccharacteristics of biomass and coal co-pyrolysis. In Coats-Redfern method, heating rates haveless effect on the activation energy, but have some influences on pre-exponential factor. Theco-pyrolysis process is divided into some single reactions, and lower activation energy which isan average value of whole pyrolysis process is obtained. Average activation energy is difficultto describe the whole co-pyrolysis process. So Coats-Redfern is not the most effective methodto simulate co-pyrolysis kinetics. An activation energy function that change with theconversion rate is obtained by DAEM mode. The activation energy fuction shows an increased-smooth-increased trend. When using DAEM method to simulate the whole co-pyrolysisprocess, pre-exponential factors go up with the increase of activation energy and showcompensation effect. The Gaussian fitting for co-pyrolysis process has good correlations whichprove the excellent applicability of the DAEM for co-pyrolysis process. The test co-pyrolysisactivation energy values are lower than the calculated ones which further verify the existenceof synergistic effect in the co-pyrolysis process.
The catalytic characterizations were tested with tar simulated by naphthalene.93%naphthalene is decomposed at950℃. Activation energy of63.96kJ/mol and pre-exponentialfactor of396.2/s are calculated, which shows the lowest apparent activation energy in allreferrences. A first order apparent kinetic model is developed.r_A=396.2×exp(-925.34×1/T)C_A
1.生物质与煤慢速共热解行为研究
采用TG-FTIR联用的分析方法对生物质与煤单独热解及共热解过程进行分析。结果发现，生物质与煤共热解的实际热失重过程较理论计算值程度有所加深，褐煤与生物质的共热解效果最好；共热解协同作用主要体现在较高温段生物质对煤的催化作用。根据TG-FTIR的实验结果推测，生物质中的Fe、Ca、Mg、Si等微量元素的氧化物，在共热解过程中破坏煤胶质体的形成，使得煤炭热解初期的产物气体得以逸出，从而增加共热解过程气体产率，降低液体产率；自制的镍铁白云石基双金属催化剂进一步促进了共热解反应发生的深度，提高了共热解过程中碳的转化率和原料利用率。
2.生物质与煤快速共热解行为研究
在小型固定床反应器上，对生物质与煤快速共热解过程进行研究，发现：温度对生物质与煤快速共热解反应影响比较明显，温度越高，产气率和H2含量越大，固体得率越低，气体和固体得率及气体组分理论值与实际值的偏差，说明快速共热解过程中存在协同反应；生物质与煤快速共热解产气量随生物质在原料中掺混比例的增加而增加；生物质与煤快速共热解反应有利于产生富氢热解气，尤其是木屑与烟煤在B:C=2:8(Wt/Wt)的条件下生成的热解气中H2所占比例达42.53%，CO产率随着生物质在原料中所占比例的增加而降低，CO2实际产率低于理论计算值，CH_4产率随着煤化程度和生物质在原料中所占比例的增加逐渐降低，其他烃类的产量增加。
3.生物质与煤快速共气化行为研究
在小型固定床反应器上，采用快速升温的方式，考察生物质与煤水蒸气快速共气化和加水快速共气化两种方式对共气化过程及产物的影响。生物质与煤水蒸气快速共气化反应可生产富氢产物气，明显降低CO及烃类气体产率，H_2/CO可达3-4，对CO_2产量影响不是很明显；生物质与煤加水快速共气化气体产量也有显著增加，随着加水共气化终温的升高，气体产物中H_2组分所占比例明显增加，而CO组分所占比例略有下降。两种共气化方式相比，水蒸气共气化法产生富氢气体，适用于合成液体燃料，尤其是作为甲醇合成的原料气；而直接加水气化得到较多的可燃气体，燃气热值较高，可用来燃烧、发电及供气。
4.烘焙生物质与煤共热解行为研究
采用TG和小型固定床两种反应器形式分别对烘焙生物质与煤慢速共热解和快速共热解过程及产物进行研究。通过慢速共热解研究，发现250℃和30min是一个比较合适的生物质原料预处理温度。烘焙预处理有利于生物质与褐煤快速共热解气体产物的生成。各气体组分中，H2含量减少很多，CO含量略有增加，CO_2含量增加，CmHn含量增加较多，但气体热值总体变化不大。生物质经烘焙预处理后与煤快速共热解反应能有效降低焦油产量。
5.生物质与煤共热解及焦油催化裂解动力学研究
分别采用Coats-Redfern法和DAEM法对生物质与煤共热解过程的动力学特性加以分析。Coats-Redfern法中，升温速率对活化能影响不大，对频率因子有一定的影响。Coats-Redfern法将共热解过程分为多段的单一反应，求出的活化能值较低，且为整个共热解过程活化能的平均值，不能全面准确的表达生物质、煤单独热解或两者混合物的共热解活化能和实际过程，因而不适宜于模拟共热解等复杂反应体系；DAEM模型求得的活化能是随转化率变化的一个函数，呈现升高-平稳-升高的变化趋势，指前因子随活化能的增大而增大，补偿了由于活化能增大而造成的速度常数减少。DAEM法的Gaussian拟合相关性较好，充分证明了DAEM模型对共热解过程的适用性较好。实验得到的共热解活化能小于加权计算方法得到的共热解活化能，进一步验证了在共热解过程中协同反应效应的真实存在。
以萘为模型化合物模拟焦油的催化裂解反应可以看做是平推流反应形式。在自制的镍铁白云石基双金属复合催化剂上，950℃时萘的转化率达到93%以上，求得的表观活化能为63.96kJ/mol，为目前所能检索到的最小。以萘为模型化合物的焦油催化裂解本征动力学方程为：r_A=396.2×exp(-925.34×1/T)C_A
Biomass and coal co-pyrolysis is a great potential technology and a relative new researchfield in the world. Its core problem is the synergistic effect of co-pyrolysis. Under ourlaboratory conditions, the co-pyrolysis synergistic effect of6kinds of biomasses and coalswere studied and investigated in this thesis. Distribution activation energy method (DAEM)was introduced into this thesis to study the co-pyrolysis kinetics of biomass and coal, and to getthe co-pyrolysis related kinetics parameters. The aim of this thesis is to find more effectiveways to achieve the synergistic effect in biomass and coal co-pyrolysis. This main researchcontents and results are summarized as follows:
1. Slow co-pyrolysis behavior of biomass and coal
Mono-pyrolysis and co-pyrolysis of biomass and coal were studied by using the TG-FTIRtechnology. It is found that the actual co-pyrolysis degrees are deeper than the theoretical ones.The effect of biomass and lignite co-pyrolysis is the best with actual results deviatingtheoretical value greatly. The synergistic effects are expressed as the biomass catalytic effect oncoal at high temperature region. According to results of the TG-FTIR, it can be concluded thatthe oxides of Fe, Ca, Mg, Si, and other trace elements in biomass inhibit the formation of coalcolloid, and make the initial gas product of coal pyrolysis be able to escape. Synergistic effectaccelerates coal pyrolysis to produce gas and decrease liquid products. The bimetallic dolomitebased catalyst further promotes the co-pyrolysis reaction, and improves the carbon conversionrates and utilization of raw materials in the co-pyrolysis process.
2. Fast co-pyrolysis behavior of biomass and coal
Fast co-pyrolysis process of biomass and coal were studied in a small fixed-bed reactor. Itis found that the pyrolysis temperature impact on fast co-pyrolysis of biomass and coalsignificantly. The synergistic effect is more obvious in the higher temperature. With theincrease of temperature, the H_2content and gas product yields increase, and the solid productyields greatly decrease. The deviation of theoretical value and actual value of co-pyrolysis gas and solid yields fully prove that the synergistic effect in fast co-pyrolysis process. Gasproductions increase with incremental biomass ratio in blending raw material. Biomass andcoal fast co-pyrolysis reaction can obtain hydrogen-rich gaseous products. Especially, when theratio of sawdust to bituminous is2to8, fast co-pyrolysis reactions get highest H2content of42.53%. The CO production decreases in higher biomass mixing ratio. The CO_2actual yield islower than the theoretical value. The CH_4yield decrease with the coal rank and biomass to coalratio increase. However, co-pyrolysis process effectively improves the production of otherhydrocarbons.
3. Fast co-gasification behavior of biomass and coal
Steam fast co-gasification and mixing water fast co-gasification processes were studied ina small fixed-bed reactor by fast heating-up mode. Steam fast co-gasification of biomass andcoal can produce hydrogen-rich gaseous products, and promote the H_2/CO to3-4, butsignificantly reduces the yield of CO and hydrocarbon. CO_2production change of this processis not very remarkable. Mixing water fast co-gasification process of biomass and coal canpromote the synergistic effect occur. The gaseous product yield of biomass and coal mixingwater fast co-gasification significantly increases. With the co-gasification reaction temperaturerise, the H2content increases significantly, while a slight decrease for the CO content occurs.Comparing the two methods of co-gasification, it can be concluded that steam fastco-gasification get the hydrogen-rich gas which is suitable for synthesizing liquid fuels,especially as the raw gas of methanol synthesis, while mixing water fast co-gasification getmuch higher heat value combustible gas which can be used for burning, power generation andgas supply.
4. Co-pyrolysis behavior of torrefaction biomass and coal
The process and product of slow and fast co-pyrolysis of torrefied biomass and coal werestudied by TG analysis technique and a small fixed-bed reactor respectively. In the slowco-pyrolysis research, it can be concluded that250℃and30min is a suitable torrefactioncondition for biomass. The torrefaction of biomass is better for biomass and lignite fast co-pyrolysis to get more gaseous product. Fast co-pyrolysis reactions of torrefaction biomassand coal have the effect of reducing H2content significantly, increasing CO content a bit andaccruing CO2and CmHncontent vastly. However, the heat values of gaseous product arechanged slightly. Fast co-pyrolysis of torrefied biomass and coal has a positive effect onlowering tar yield.
5. Kinetic analysis of biomass and coal co-pyrolysis and tar catalytic cracking
In this part, Coats-Redfern and DAEM methods were used to analyze the dynamiccharacteristics of biomass and coal co-pyrolysis. In Coats-Redfern method, heating rates haveless effect on the activation energy, but have some influences on pre-exponential factor. Theco-pyrolysis process is divided into some single reactions, and lower activation energy which isan average value of whole pyrolysis process is obtained. Average activation energy is difficultto describe the whole co-pyrolysis process. So Coats-Redfern is not the most effective methodto simulate co-pyrolysis kinetics. An activation energy function that change with theconversion rate is obtained by DAEM mode. The activation energy fuction shows an increased-smooth-increased trend. When using DAEM method to simulate the whole co-pyrolysisprocess, pre-exponential factors go up with the increase of activation energy and showcompensation effect. The Gaussian fitting for co-pyrolysis process has good correlations whichprove the excellent applicability of the DAEM for co-pyrolysis process. The test co-pyrolysisactivation energy values are lower than the calculated ones which further verify the existenceof synergistic effect in the co-pyrolysis process.
The catalytic characterizations were tested with tar simulated by naphthalene.93%naphthalene is decomposed at950℃. Activation energy of63.96kJ/mol and pre-exponentialfactor of396.2/s are calculated, which shows the lowest apparent activation energy in allreferrences. A first order apparent kinetic model is developed.r_A=396.2×exp(-925.34×1/T)C_A
引文
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