煤、生物质及其混合物的快速热解及过程中氮的迁移
摘要
热解不仅是热化学转化的一种直接方法,也是燃烧和气化过程的重要阶段。在气流床气化炉中,气化原料喷入气化炉后首先发生快速热解,由于气流床气化炉内反应温度高,物料的平均停留时间较短,快速热解产物的分布和焦的气化特性是影响后续气化反应的重要条件。尤其对转化速率较慢的含氮化合物,快速热解中氮的迁移对最终含氮污染物的形成影响很大。因此,对煤和生物质的快速热解产物分布、快速热解焦的气化特性和氮元素的迁移进行研究对煤和生物质的高效清洁利用具有重要意义。
本文将高频感应加热方法用于热解实验,设计了一种独特的高频炉快速热解装置,利用该装置对煤和生物质的单独快速热解以及煤/生物质共快速热解(600～1200℃)时气固相产物的分布、焦的结构和气化特性进行了研究。同时考察了煤、生物质单独快速热解和共快速热解过程中氮元素的迁移特性,应用量子化学方法和模型化合物快速热解实验相结合的方法对煤和生物质快速热解时氮的逸出机理进行了分析。主要内容如下：
(1)对内蒙南露天褐煤、神府烟煤和遵义无烟煤快速热解时产物的分布进行了考察。结果表明,煤快速热解相比慢速热解能析出更多的挥发分。热解温度的升高能显著提高热解气产率,降低焦产率。煤阶的升高使焦产率上升,热解气产率降低。热解气主要成分为H2和CO,其次为CH4和CO2,还有少量气态烃(C2～C3)。热解温度的升高使H2和CO产率升高,CO2产率下降,CH4等气态烃大多呈先上升后下降的趋势。热解气低位热值均随热解温度的升高逐步下降。
(2)分析了热解条件对煤快速热解焦理化结构及最终气化特性的影响。结果表明,褐煤焦具有粗糙的表面和丰富的孔隙结构；烟煤焦在热解时发生了严重的熔融,形成了光滑的表面,但焦的内部孔隙结构发达；无烟煤焦仅在表面可见少量裂缝。因此,随煤阶的升高,孔隙率和比表面积降低,而煤焦有序化程度则逐步升高,导致气化反应活性下降。褐煤和烟煤的气化反应速率在气化时先升高后迅速下降,导致随机孔模型的拟合效果较差,而变换后的修正随机孔模型能得到较好的拟合效果。
(3)对煤快速热解时氮的迁移进行了考察。结果表明,大部分氮保留在焦中,N2是主要的气相含氮产物,NH3是主要的含氮污染物,HCN的产率较低。HCN和NH3均可以在热解的初始阶段直接生成。利用量子化学方法和模型化合物快速热解实验对煤中氮的逸出机理进行分析时发现,N-6在快速热解时会倾向于以-CN基的形式逸出并产生较多的HCN, N-5在快速热解时会倾向于以-NH基的形式逸出并主要转化为NH3, N-Q在快速热解的剧烈热冲击条件下可能会以N自由基的形式逸出并转化为NH3。HCN受二次反应程度的影响最为明显。
(4)对稻草、树叶和木屑快速热解产物分布进行了考察。生物质有机质转化率顺序为松木屑>稻草>梧桐树叶。快速热解焦的产率较低,因此灰分的含量在一定程度影响了焦的产率。生物质有机质向热解气的转化率可达到80%以上。热解气主要成分为CO和H2,二者的产率均随着热解温度的升高而升高；CH4等烃类的产率则先升高后下降；高温条件下CO2的产率很低。随热解温度的升高,热解气的低位热值先升高后下降。
(5)对三种生物质快速热解焦的结构及气化特性进行了考察。结果表明,热解温度的升高使生物质焦的有序化程度升高,并导致气化活性的下降。稻草和梧桐树叶快速热解焦基本保持了原始结构,而松木屑发生软化和熔缩,导致孔隙结构的破坏,进而导致其气化反应活性的显著下降。随机孔模型在多数情况下能较好地描述生物质焦的气化反应动力学。但当气化反应速率在高转化率范围内仍较高或者急剧下降时,修正随机孔模型的的拟合效果更好。
(6)对生物质快速热解时氮的迁移进行了考察。生物质快速热解时残留在焦中的氮很少,氮主要转化为了N2,热解温度的提高会降低含氮污染物的生成,促使更多的氮转化为N2。蛋白质、氨基酸和含氮碱基快速热解时,含氮污染物以NH3为主。而三种农林生物质快速热解时HCN的产率远高于NH3,且HCN的产率随生物质木质素含量的升高而升高。木质素构成的微腔结构可能会在热解初期导致蛋白质、氨基酸等含氮物质与生物质有机组分发生缩聚反应而生成含氮杂环,并导致HCN的大量生成。
(7)高频炉在煤/生物质共热解过程中既能保证样品较好的接触,又能使其达到高的升温速率,在这种条件下共热解能发生明显的协同作用,导致焦产率的降低,热解气产率的升高。生物质的堆积密度及其在热解过程中碳骨架的变化是影响协同作用的重要因素。生物质焦与煤焦共气化时气化活性有所升高,而生物质与煤共热解所得焦的活性并未明显提高,生物质与煤共热解时发生的相互粘附及研磨时孔隙结构的阻塞是导致上述现象的原因。这两个因素又导致共热解焦具有较高的均一性,使其气化反应速率随转化率的变化较为平缓。
(8)对生物质与煤共快速热解时氮的迁移进行了研究。生物质与煤混合样品的堆积密度以及生物质碳骨架在热解过程中的坍塌特性,是影响混合样品升温速率及其最终含氮产物分布的重要条件。生物质与烟煤共热解能明显降低焦-N产率,提高挥发分-N的产率,降低(NH3+HCN)-N的产率。NH3-N的产率的实验值在所有条件下均低于叠加值。HCN-N产率的实验值在高温条件下均低于叠加值,但在600～700℃条件下,HCN-N的产率却明显提高。
Pyrolysis is not only one of the thermal conversion method, but also an important process in combustion and gasification. In the entrained-flow gasifier, rapid pyrolysis happens immediately when the fuels are injected into the gasifier. As reaction temperature in entrained-flow gasifier is very high and average residence time of reactants is very short, product distribution of the rapid pyrolysis and gasification characteristics of the pyrolysis char are important factors of the subsequent gasification reactions. Especially for the nitrogen containing compounds whose conversion rates are relatively low, thus nitrogen evolution during rapid pyrolysis greatly affects the yields of the final nitrogen pollutants. Therefore, investigation on product distribution and nitrogen evolution during rapid pyrolysis of coal and biomass and gasification characteristics of the derived char has important significances for clean and efficient utilization of coal and biomass.
In this study, high-frequency inductive heating method was employed to the pyrolysis experiments, and a high-frequency furnace which has innovation significance was designed. Yields of gaseous and solid products during rapid pyrolysis (600～1200℃) of coal, biomass, and their blends, structure and gasification characteristics of the residual char were investigated. Nitrogen evolution during individual pyrolysis and co-pyrolysis of biomass and coal was also studied. Nitrogen release mechanisms during rapid pyrolysis were analyzed by integrating the results of quantum chemical calculation and nitrogen containing model compound pyrolysis. Main contents and results are summarized as the follows:
(1) Product distributions during rapid pyrolysis of the Inner Mongolia Nanlutian lignite, Shenfu bituminous, and Zunyi anthracite were investigated. Results show that, more volatiles released under rapid pyrolysis than slow pyrolysis. The increasing temperature increased the yields of gas but decreased the char yields. The increasing coal rank decreased the gas yields and increased the char yields. H2 and CO were the main components of the pyrolysis gas, followed by CH4 and CO2, some gaseous hydrocarbons (C2～C3) were also formed. As the temperature increased, yields of H2 and CO increased, yields of CO2 decreased, and yields of CH4 and the other gaseous hydrocarbons mainly increased first and deceased then. Low heating values of all the pyrolysis gas decreased with the increasing temperature.
(2) Effects of pyrolysis conditions on morphologic and instinct chemical structures and further on gasification characteristics of the char derived from coal pyrolysis were studied. Lignite char presents a very coarse surface and rich porosity. Serious melting happened to the bituminous char which resulted in smooth surfaces but rich internal porosity. Just some gaps formed on the anthracite char. Thus as the coal rank increased, specific areas of the char decrease, graphitization degrees of the char also increased with the coal rank. Therefore, gasification reactivity decreased with the increasing coal rank. During gasification of lignite char and bituminous char, reaction rates increased first and decreased sharply then, which resulted in unsatisfied fitting results of random pore model (RPM). But the shifted modified random pore model (S-M-RPM) could obtain very good fitting results.
(3) Nitrogen evolution during rapid pyrolysis of the three coals was investigated. Most of the fuel-N was retained in char after pyrolysis, N2 was the main gaseous nitrogen product, and NH3 was the main nitrogen pollutant. Both HCN and NH3 could be formed in the primary stage of rapid pyrolysis. With the results of quantum chemical calculations and pyrolysis of nitrogen-containing model compound, it was found that N-6 tended to release as -CN radicals and formed HCN mainly, N-5 tended to release as -NH radicals and formed NH3 mainly, and N-Q tended to release as N radicals under the drastic heat impact and formed NH3 mainly. HCN has the highest sensitivity to the secondary reactions.
(4) Product distributions under rapid pyrolysis of rice straw, chinar leaves, and pine sawdust were investigated. During pyrolysis order the organic matter conversions are pine sawdust>rice straw>chinar leaves. Conversion of the organic matters to gas could reach as high as 80%. Char yields were very low after rapid pyrolysis of biomass at high temperature, therefore ash contents had important affected on the char yields. CO and H2 were the main components of the pyrolysis gas, which increased with the increasing temperature. As the temperature increased, yields of CH4 increased first and decreased then, those of CO2 decreased gradually to a very low value in the high temperature. Low heating values of the pyrolysis gas increased first and decreased then.
(5) Morphologic and instinct chemical structures of the biomass char and their effect on the gasification characteristics were studied. Graphitization degrees of the char increased with the increasing pyrolysis temperature and led to the decrease of gasification reactivity. Char derived from rapid pyrolysis of rice straw and chinar leaves almost remained the original structures. Serious melting happened to the pine sawdust, and resulted in the destruction of the pore structures and low reactivity. RPM performed well under most of the conditions to describe the gasification rates. But under the condition that high gasification rates were remained or drastic decrease of the gasification rates happened in the high conversion range, the S-M-RPM performed better.
(6) Nitrogen evolution during rapid pyrolysis of biomass was investigated. Little nitrogen retained in char after pyrolysis of biomass, and most of the nitrogen converted to N2. The increasing temperature could decrease the yields of nitrogen pollutants and promote nitrogen conversion to N2. NH3 was the main nitrogen pollutant during rapid pyrolysis of protein, amino acids, and nucleobases. While yields of HCN were much higher than those of NH3 during rapid pyrolysis of the 3 agriculture and forestry biomass, and the yields of HCN increased with the lignin contents of biomass. The reason might be that "Microcells" composed by the lignin could result in the polymerization reactions between protein, amino acids, etc. and the organic compositions (cellulose, hemicellulose, and lignin) to form heterocyclic nitrogen and lead to the formation of HCN.
(7) The high-frequency furnace not only could make the fuel particles obtain high heating rates, but also could make the biomass and coal particles contact well. Under this condition, obvious synergies were observed during co-pyrolysis of biomass and coal to decrease the yields of char and increase the yields of gas. Packing densities of the biomass and the skeleton collapse characteristics during pyrolysis were important impact factors on the synergies during co-pyrolysis of biomass and coal. Synergies could be observed during co-gasification of biomass char and coal char. But scarcely synergies were found during gasification of the co-pyrolysis char, and inherences between biomass and coal during co-pyrolysis and pore block during char crush might be the reasons. These two aspects also increased the structure homogeneity of the co-pyrolysis char, resulted in a gentle variation of the gasification rates.
(8) Nitrogen evolution during rapid pyrolysis of biomass/coal blends was also studied. By affecting the heating rate, nitrogen evolution was also affected significantly by the packing densities and carbon skeleton collapse characteristics of biomass. Co-pyrolysis of biomass and coal could decrease the char-N yields, increase the volatile-N yields, but (NH3+HCN)-N in volatile-N was also decreased. NH3-N was decreased in all the conditions. HCN-N was decreased in the high-temperature range, but under the temperature of 600～700℃, HCN-N yields were increased during co-pyrolysis.
本文将高频感应加热方法用于热解实验,设计了一种独特的高频炉快速热解装置,利用该装置对煤和生物质的单独快速热解以及煤/生物质共快速热解(600～1200℃)时气固相产物的分布、焦的结构和气化特性进行了研究。同时考察了煤、生物质单独快速热解和共快速热解过程中氮元素的迁移特性,应用量子化学方法和模型化合物快速热解实验相结合的方法对煤和生物质快速热解时氮的逸出机理进行了分析。主要内容如下：
(1)对内蒙南露天褐煤、神府烟煤和遵义无烟煤快速热解时产物的分布进行了考察。结果表明,煤快速热解相比慢速热解能析出更多的挥发分。热解温度的升高能显著提高热解气产率,降低焦产率。煤阶的升高使焦产率上升,热解气产率降低。热解气主要成分为H2和CO,其次为CH4和CO2,还有少量气态烃(C2～C3)。热解温度的升高使H2和CO产率升高,CO2产率下降,CH4等气态烃大多呈先上升后下降的趋势。热解气低位热值均随热解温度的升高逐步下降。
(2)分析了热解条件对煤快速热解焦理化结构及最终气化特性的影响。结果表明,褐煤焦具有粗糙的表面和丰富的孔隙结构；烟煤焦在热解时发生了严重的熔融,形成了光滑的表面,但焦的内部孔隙结构发达；无烟煤焦仅在表面可见少量裂缝。因此,随煤阶的升高,孔隙率和比表面积降低,而煤焦有序化程度则逐步升高,导致气化反应活性下降。褐煤和烟煤的气化反应速率在气化时先升高后迅速下降,导致随机孔模型的拟合效果较差,而变换后的修正随机孔模型能得到较好的拟合效果。
(3)对煤快速热解时氮的迁移进行了考察。结果表明,大部分氮保留在焦中,N2是主要的气相含氮产物,NH3是主要的含氮污染物,HCN的产率较低。HCN和NH3均可以在热解的初始阶段直接生成。利用量子化学方法和模型化合物快速热解实验对煤中氮的逸出机理进行分析时发现,N-6在快速热解时会倾向于以-CN基的形式逸出并产生较多的HCN, N-5在快速热解时会倾向于以-NH基的形式逸出并主要转化为NH3, N-Q在快速热解的剧烈热冲击条件下可能会以N自由基的形式逸出并转化为NH3。HCN受二次反应程度的影响最为明显。
(4)对稻草、树叶和木屑快速热解产物分布进行了考察。生物质有机质转化率顺序为松木屑>稻草>梧桐树叶。快速热解焦的产率较低,因此灰分的含量在一定程度影响了焦的产率。生物质有机质向热解气的转化率可达到80%以上。热解气主要成分为CO和H2,二者的产率均随着热解温度的升高而升高；CH4等烃类的产率则先升高后下降；高温条件下CO2的产率很低。随热解温度的升高,热解气的低位热值先升高后下降。
(5)对三种生物质快速热解焦的结构及气化特性进行了考察。结果表明,热解温度的升高使生物质焦的有序化程度升高,并导致气化活性的下降。稻草和梧桐树叶快速热解焦基本保持了原始结构,而松木屑发生软化和熔缩,导致孔隙结构的破坏,进而导致其气化反应活性的显著下降。随机孔模型在多数情况下能较好地描述生物质焦的气化反应动力学。但当气化反应速率在高转化率范围内仍较高或者急剧下降时,修正随机孔模型的的拟合效果更好。
(6)对生物质快速热解时氮的迁移进行了考察。生物质快速热解时残留在焦中的氮很少,氮主要转化为了N2,热解温度的提高会降低含氮污染物的生成,促使更多的氮转化为N2。蛋白质、氨基酸和含氮碱基快速热解时,含氮污染物以NH3为主。而三种农林生物质快速热解时HCN的产率远高于NH3,且HCN的产率随生物质木质素含量的升高而升高。木质素构成的微腔结构可能会在热解初期导致蛋白质、氨基酸等含氮物质与生物质有机组分发生缩聚反应而生成含氮杂环,并导致HCN的大量生成。
(7)高频炉在煤/生物质共热解过程中既能保证样品较好的接触,又能使其达到高的升温速率,在这种条件下共热解能发生明显的协同作用,导致焦产率的降低,热解气产率的升高。生物质的堆积密度及其在热解过程中碳骨架的变化是影响协同作用的重要因素。生物质焦与煤焦共气化时气化活性有所升高,而生物质与煤共热解所得焦的活性并未明显提高,生物质与煤共热解时发生的相互粘附及研磨时孔隙结构的阻塞是导致上述现象的原因。这两个因素又导致共热解焦具有较高的均一性,使其气化反应速率随转化率的变化较为平缓。
(8)对生物质与煤共快速热解时氮的迁移进行了研究。生物质与煤混合样品的堆积密度以及生物质碳骨架在热解过程中的坍塌特性,是影响混合样品升温速率及其最终含氮产物分布的重要条件。生物质与烟煤共热解能明显降低焦-N产率,提高挥发分-N的产率,降低(NH3+HCN)-N的产率。NH3-N的产率的实验值在所有条件下均低于叠加值。HCN-N产率的实验值在高温条件下均低于叠加值,但在600～700℃条件下,HCN-N的产率却明显提高。
Pyrolysis is not only one of the thermal conversion method, but also an important process in combustion and gasification. In the entrained-flow gasifier, rapid pyrolysis happens immediately when the fuels are injected into the gasifier. As reaction temperature in entrained-flow gasifier is very high and average residence time of reactants is very short, product distribution of the rapid pyrolysis and gasification characteristics of the pyrolysis char are important factors of the subsequent gasification reactions. Especially for the nitrogen containing compounds whose conversion rates are relatively low, thus nitrogen evolution during rapid pyrolysis greatly affects the yields of the final nitrogen pollutants. Therefore, investigation on product distribution and nitrogen evolution during rapid pyrolysis of coal and biomass and gasification characteristics of the derived char has important significances for clean and efficient utilization of coal and biomass.
In this study, high-frequency inductive heating method was employed to the pyrolysis experiments, and a high-frequency furnace which has innovation significance was designed. Yields of gaseous and solid products during rapid pyrolysis (600～1200℃) of coal, biomass, and their blends, structure and gasification characteristics of the residual char were investigated. Nitrogen evolution during individual pyrolysis and co-pyrolysis of biomass and coal was also studied. Nitrogen release mechanisms during rapid pyrolysis were analyzed by integrating the results of quantum chemical calculation and nitrogen containing model compound pyrolysis. Main contents and results are summarized as the follows:
(1) Product distributions during rapid pyrolysis of the Inner Mongolia Nanlutian lignite, Shenfu bituminous, and Zunyi anthracite were investigated. Results show that, more volatiles released under rapid pyrolysis than slow pyrolysis. The increasing temperature increased the yields of gas but decreased the char yields. The increasing coal rank decreased the gas yields and increased the char yields. H2 and CO were the main components of the pyrolysis gas, followed by CH4 and CO2, some gaseous hydrocarbons (C2～C3) were also formed. As the temperature increased, yields of H2 and CO increased, yields of CO2 decreased, and yields of CH4 and the other gaseous hydrocarbons mainly increased first and deceased then. Low heating values of all the pyrolysis gas decreased with the increasing temperature.
(2) Effects of pyrolysis conditions on morphologic and instinct chemical structures and further on gasification characteristics of the char derived from coal pyrolysis were studied. Lignite char presents a very coarse surface and rich porosity. Serious melting happened to the bituminous char which resulted in smooth surfaces but rich internal porosity. Just some gaps formed on the anthracite char. Thus as the coal rank increased, specific areas of the char decrease, graphitization degrees of the char also increased with the coal rank. Therefore, gasification reactivity decreased with the increasing coal rank. During gasification of lignite char and bituminous char, reaction rates increased first and decreased sharply then, which resulted in unsatisfied fitting results of random pore model (RPM). But the shifted modified random pore model (S-M-RPM) could obtain very good fitting results.
(3) Nitrogen evolution during rapid pyrolysis of the three coals was investigated. Most of the fuel-N was retained in char after pyrolysis, N2 was the main gaseous nitrogen product, and NH3 was the main nitrogen pollutant. Both HCN and NH3 could be formed in the primary stage of rapid pyrolysis. With the results of quantum chemical calculations and pyrolysis of nitrogen-containing model compound, it was found that N-6 tended to release as -CN radicals and formed HCN mainly, N-5 tended to release as -NH radicals and formed NH3 mainly, and N-Q tended to release as N radicals under the drastic heat impact and formed NH3 mainly. HCN has the highest sensitivity to the secondary reactions.
(4) Product distributions under rapid pyrolysis of rice straw, chinar leaves, and pine sawdust were investigated. During pyrolysis order the organic matter conversions are pine sawdust>rice straw>chinar leaves. Conversion of the organic matters to gas could reach as high as 80%. Char yields were very low after rapid pyrolysis of biomass at high temperature, therefore ash contents had important affected on the char yields. CO and H2 were the main components of the pyrolysis gas, which increased with the increasing temperature. As the temperature increased, yields of CH4 increased first and decreased then, those of CO2 decreased gradually to a very low value in the high temperature. Low heating values of the pyrolysis gas increased first and decreased then.
(5) Morphologic and instinct chemical structures of the biomass char and their effect on the gasification characteristics were studied. Graphitization degrees of the char increased with the increasing pyrolysis temperature and led to the decrease of gasification reactivity. Char derived from rapid pyrolysis of rice straw and chinar leaves almost remained the original structures. Serious melting happened to the pine sawdust, and resulted in the destruction of the pore structures and low reactivity. RPM performed well under most of the conditions to describe the gasification rates. But under the condition that high gasification rates were remained or drastic decrease of the gasification rates happened in the high conversion range, the S-M-RPM performed better.
(6) Nitrogen evolution during rapid pyrolysis of biomass was investigated. Little nitrogen retained in char after pyrolysis of biomass, and most of the nitrogen converted to N2. The increasing temperature could decrease the yields of nitrogen pollutants and promote nitrogen conversion to N2. NH3 was the main nitrogen pollutant during rapid pyrolysis of protein, amino acids, and nucleobases. While yields of HCN were much higher than those of NH3 during rapid pyrolysis of the 3 agriculture and forestry biomass, and the yields of HCN increased with the lignin contents of biomass. The reason might be that "Microcells" composed by the lignin could result in the polymerization reactions between protein, amino acids, etc. and the organic compositions (cellulose, hemicellulose, and lignin) to form heterocyclic nitrogen and lead to the formation of HCN.
(7) The high-frequency furnace not only could make the fuel particles obtain high heating rates, but also could make the biomass and coal particles contact well. Under this condition, obvious synergies were observed during co-pyrolysis of biomass and coal to decrease the yields of char and increase the yields of gas. Packing densities of the biomass and the skeleton collapse characteristics during pyrolysis were important impact factors on the synergies during co-pyrolysis of biomass and coal. Synergies could be observed during co-gasification of biomass char and coal char. But scarcely synergies were found during gasification of the co-pyrolysis char, and inherences between biomass and coal during co-pyrolysis and pore block during char crush might be the reasons. These two aspects also increased the structure homogeneity of the co-pyrolysis char, resulted in a gentle variation of the gasification rates.
(8) Nitrogen evolution during rapid pyrolysis of biomass/coal blends was also studied. By affecting the heating rate, nitrogen evolution was also affected significantly by the packing densities and carbon skeleton collapse characteristics of biomass. Co-pyrolysis of biomass and coal could decrease the char-N yields, increase the volatile-N yields, but (NH3+HCN)-N in volatile-N was also decreased. NH3-N was decreased in all the conditions. HCN-N was decreased in the high-temperature range, but under the temperature of 600～700℃, HCN-N yields were increased during co-pyrolysis.
引文
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