生物质选择性热裂解机理研究
摘要
生物质快速热裂解技术是当今生物质能开发应用领域的前沿技术,能够将生物质转化为易储存、易运输的液体燃料,但因其复杂的成分和不稳定的化学性质限制了其作为高品位液体燃料的应用,究其原因是缺乏对相关机理的深入了解。本文结合相关国家项目的支持,对生物质和生物油及馏分的热裂解机理进行了较为系统的研究。
生物质主要由纤维素、半纤维素和木质素组成,纤维素结构简单且随物料种类的变化较小,半纤维素则种类繁多由多种糖类构成,而木质素结构极其复杂,目前还不十分清楚。本文在热裂解-色谱质谱联用(PY-GC/MS)分析仪上开展了纤维素快速热裂解机理研究,发现纤维素的主要热裂解产物包括以左旋葡聚糖和左旋葡聚糖酮为代表的吡喃类物质,以糠醛和5-羟甲基糠醛为代表的呋喃类物质,以乙醛和1-羟基-2-丙酮等为代表的小分子直链物质。其中小分子直链产物主要由纤维素直接分解形成,而不是由一次产物的二次分解获得。纤维素在热裂解过程中,首先发生解聚反应形成聚合度较低的活性纤维素,进而通过脱水反应、开环反应和环化反应等形成多种热裂解产物。基于纤维素热裂解过程分析,开展了以D-吡喃型葡萄糖单体为反应物的密度泛函理论模拟计算,确定左旋葡聚糖的形成较为容易,其同分异构体3,4-脱水阿卓糖的形成则较为困难。5-羟甲基糠醛可通过D-吡喃型葡萄糖单体分解产生,而它的转化率要高于左旋葡聚糖,另外,5-羟甲基糠醛通过进一步的脱羟甲基作用会生成糠醛和小分子产物,该反应可自发进行。热裂解产物的组成与组分的结构密切相关,木聚糖快速热裂解的产物主要含有乙酸、糠醛和环戊烯酮类等物质,木质素的产物则主要包括烷基酚类、愈创木基型酚类和紫丁香基型酚类物质,还有少量的苯、甲苯等芳香烃类物质。
本文还开展了生物质选择性热裂解行为研究。在热重-红外联用(TG-FTIR)分析仪上研究了沸石分子筛催化剂HZSM-5、H-β和USY对生物质及其组分选择性热裂解过程的影响规律,研究发现三种催化剂都促进了热裂解初期脱水反应的发生,造成了初期阶段失重的增加,同时对热裂解后期焦炭形成的影响也较大。USY的添加对初始阶段的脱水效果最明显,而HZSM-5和H-β的添加则抑制了焦炭的生成。催化剂的添加并没有改变热裂解产物的种类,只是引起产物析出强度的变化。三种催化剂的添加均降低了含氧化合物的产量,增加了小分子产物CO、CO2、甲烷等烃类产物的产量。USY的作用使得热裂解产物中含氧化合物主要向水和CO2等转化,而HZSM-5和H-β则通过促进焦炭的二次分解反应形成CO、CO2和甲烷等小分子直链产物。
同时,基于生物油分级分离改性的后续研究需要,本文针对分子蒸馏仪获得的生物油馏分在热重-红外联用分析仪上开展了生物油及其馏分的热裂解动力学研究。轻质馏分富含水分和酸性化合物,在较低温度下就会通过挥发的形式开始失重,并生成CO2、CO、乙酸、醇类等小分子化合物,最后在200℃左右完成全部失重。重质馏分含有较多的酚类和糖类等高沸点物质,几乎没有水分,因此热值较高,稳定性较好,在热裂解过程中具有较宽的失重区间,焦炭产量高达30wt%左右。在这其中,失重低温段以化合物自身的挥发为主,较容易发生,高温段则以物质的分解为主,形成小分子气体和稳定的中间物质。中质馏分的热裂解行为介于轻质馏分和重质馏分之间,具有较多的物质种类析出,但因其蒸馏分离产量不高,可在实际应用过程视反应工况选择性地划归为轻质馏分或重质馏分。
Fast pyrolysis is one of the promising technologies, which can convert biomass into liquid fuel "bio-oil". However, the high-quality utilization of bio-oil, substituted for transportation fuels, is quite limited by its complex chemical composition. It is attributed to the lack of sufficient understanding of reaction mechanisms in biomass pyrolysis. Supported by the related national projects, a systematic research on pyrolysis mechanism of biomass and bio-oil fractions is presented in this thesis.
Biomass is mainly consisted of cellulose, hemicellulose and lignin. Among the three components. the structure of cellulose is simple and nearly changeless with the feedstock, the structure of hemicellulose is complex due to the existence of various polysaccharides, and lignin is extremely complex with unclear understanding till now. Mechanism research on fast pyrolysis of cellulose was first investigated by using an analytical pyrolyzer coupled with Gas Chromatography and Mass Spectrometer (Py-GC/MS). The results showed that the main products were composed of pyrans such as levoglucosan and levoglucosenone, furans like furfural and5-hydroxymethyl-furfural. and small molecular chemicals with linear chain like acetaldehyde and1-hydroxy-2-propanone. Small molecular compounds were obtained from the direct decomposition of cellulose, not the secondary cracking of the initial products. Based on the depolymerization of cellulose to form active cellulose, pyrans and furans were produced by dehydration reaction, ring opening reaction and cyclization reaction etc. Moreover. the simulation began with D-glucopyranose monomer, based on the density functional methods, were carried out combined with the previous experimental results on cellulose pyrolysis. It was identified that the formation of levoglucosan was easier than its isomeride of3.4-altrosan. The formation of5-hydroxymethyl-furfural was attributed to the degradation of D-glucopyranose, which had a higher conversion than levoglucosan. In addition, furfural was produced by the cleavage of hydroxymethyl group in5-hydroxymethyl-furfural spontaneously. The composition of products was closely related to the structure of samples. The products from fast pyrolysis of xylan mainly included acetic acid, furfural, and cyclopentenone etc.. and the products of lignin were predominantly composed of phenols, such as alkylphenols. guaiacols and syringols, as well as some aromatic hydrocarbons like benzene and toluene.
The selective pyrolysis of biomass and its components was also studied by using the thermogravimetric analyzer coupled with a Fourier transform infrared (TG-FTIR) spectrometry. All the three zeolite catalysts HZSM-5, H-β and USY had significant influence on the dehydration reaction, resulting in an increase of weight loss in the initial stage, and meanwhile affected the char formation process during the final stage. The addition of USY had the most obvious effect on the dehydration reaction, and the effect of HZSM-5and H-β focused on the inhibition of the char formation. Though the pyrolysis products were nearly the same, their release intensities changed after the addition of catalysts. It was observed that the yield of oxygenated compounds reduced compared with pure samples pyrolysis, but the yield of light gases increased such as CO, CO2and methane. The presence of USY enhanced the conversion of oxygenated compounds mainly to water and CO2, while the addition of HZSM-5and H-β promoted the secondary cracking of residual chars to form light gases CO. CO2and methane.
In view of the sequent researches on classification and upgrading of bio-oil for high-quality applications, pyrolysis behaviors of bio-oil fractions were studied on the TG-FTIR analyzer. combined with the first separation of bio-oil into fractions by using the molecular distillation technique. The obtained light fractions were constituted of water and acidic chemical, which began to loss weight at very low temperature by evaporation or was decomposed into small molecular compounds (CO2. CO. acetic acid, alcohols etc.) before200℃. Heavy fractions contained more compounds of phenols and sugars with high boiling point temperature and no water, so its heating value was highest and the stability was best among the three fractions. The weight loss range of heavy fraction was wide and the yield of char was high up to30wt%. During pyrolysis, self-evaporation was dominant at lower temperature, and decomposition was leading at higher temperature to produce more stable chemicals. The pyrolysis behavior of middle fraction was between light fraction and heavy fraction with the most kinds of products. Its yield was lowest, so it was regarded as light fraction or heavy fraction selectively based on the experimental conditions.
生物质主要由纤维素、半纤维素和木质素组成,纤维素结构简单且随物料种类的变化较小,半纤维素则种类繁多由多种糖类构成,而木质素结构极其复杂,目前还不十分清楚。本文在热裂解-色谱质谱联用(PY-GC/MS)分析仪上开展了纤维素快速热裂解机理研究,发现纤维素的主要热裂解产物包括以左旋葡聚糖和左旋葡聚糖酮为代表的吡喃类物质,以糠醛和5-羟甲基糠醛为代表的呋喃类物质,以乙醛和1-羟基-2-丙酮等为代表的小分子直链物质。其中小分子直链产物主要由纤维素直接分解形成,而不是由一次产物的二次分解获得。纤维素在热裂解过程中,首先发生解聚反应形成聚合度较低的活性纤维素,进而通过脱水反应、开环反应和环化反应等形成多种热裂解产物。基于纤维素热裂解过程分析,开展了以D-吡喃型葡萄糖单体为反应物的密度泛函理论模拟计算,确定左旋葡聚糖的形成较为容易,其同分异构体3,4-脱水阿卓糖的形成则较为困难。5-羟甲基糠醛可通过D-吡喃型葡萄糖单体分解产生,而它的转化率要高于左旋葡聚糖,另外,5-羟甲基糠醛通过进一步的脱羟甲基作用会生成糠醛和小分子产物,该反应可自发进行。热裂解产物的组成与组分的结构密切相关,木聚糖快速热裂解的产物主要含有乙酸、糠醛和环戊烯酮类等物质,木质素的产物则主要包括烷基酚类、愈创木基型酚类和紫丁香基型酚类物质,还有少量的苯、甲苯等芳香烃类物质。
本文还开展了生物质选择性热裂解行为研究。在热重-红外联用(TG-FTIR)分析仪上研究了沸石分子筛催化剂HZSM-5、H-β和USY对生物质及其组分选择性热裂解过程的影响规律,研究发现三种催化剂都促进了热裂解初期脱水反应的发生,造成了初期阶段失重的增加,同时对热裂解后期焦炭形成的影响也较大。USY的添加对初始阶段的脱水效果最明显,而HZSM-5和H-β的添加则抑制了焦炭的生成。催化剂的添加并没有改变热裂解产物的种类,只是引起产物析出强度的变化。三种催化剂的添加均降低了含氧化合物的产量,增加了小分子产物CO、CO2、甲烷等烃类产物的产量。USY的作用使得热裂解产物中含氧化合物主要向水和CO2等转化,而HZSM-5和H-β则通过促进焦炭的二次分解反应形成CO、CO2和甲烷等小分子直链产物。
同时,基于生物油分级分离改性的后续研究需要,本文针对分子蒸馏仪获得的生物油馏分在热重-红外联用分析仪上开展了生物油及其馏分的热裂解动力学研究。轻质馏分富含水分和酸性化合物,在较低温度下就会通过挥发的形式开始失重,并生成CO2、CO、乙酸、醇类等小分子化合物,最后在200℃左右完成全部失重。重质馏分含有较多的酚类和糖类等高沸点物质,几乎没有水分,因此热值较高,稳定性较好,在热裂解过程中具有较宽的失重区间,焦炭产量高达30wt%左右。在这其中,失重低温段以化合物自身的挥发为主,较容易发生,高温段则以物质的分解为主,形成小分子气体和稳定的中间物质。中质馏分的热裂解行为介于轻质馏分和重质馏分之间,具有较多的物质种类析出,但因其蒸馏分离产量不高,可在实际应用过程视反应工况选择性地划归为轻质馏分或重质馏分。
Fast pyrolysis is one of the promising technologies, which can convert biomass into liquid fuel "bio-oil". However, the high-quality utilization of bio-oil, substituted for transportation fuels, is quite limited by its complex chemical composition. It is attributed to the lack of sufficient understanding of reaction mechanisms in biomass pyrolysis. Supported by the related national projects, a systematic research on pyrolysis mechanism of biomass and bio-oil fractions is presented in this thesis.
Biomass is mainly consisted of cellulose, hemicellulose and lignin. Among the three components. the structure of cellulose is simple and nearly changeless with the feedstock, the structure of hemicellulose is complex due to the existence of various polysaccharides, and lignin is extremely complex with unclear understanding till now. Mechanism research on fast pyrolysis of cellulose was first investigated by using an analytical pyrolyzer coupled with Gas Chromatography and Mass Spectrometer (Py-GC/MS). The results showed that the main products were composed of pyrans such as levoglucosan and levoglucosenone, furans like furfural and5-hydroxymethyl-furfural. and small molecular chemicals with linear chain like acetaldehyde and1-hydroxy-2-propanone. Small molecular compounds were obtained from the direct decomposition of cellulose, not the secondary cracking of the initial products. Based on the depolymerization of cellulose to form active cellulose, pyrans and furans were produced by dehydration reaction, ring opening reaction and cyclization reaction etc. Moreover. the simulation began with D-glucopyranose monomer, based on the density functional methods, were carried out combined with the previous experimental results on cellulose pyrolysis. It was identified that the formation of levoglucosan was easier than its isomeride of3.4-altrosan. The formation of5-hydroxymethyl-furfural was attributed to the degradation of D-glucopyranose, which had a higher conversion than levoglucosan. In addition, furfural was produced by the cleavage of hydroxymethyl group in5-hydroxymethyl-furfural spontaneously. The composition of products was closely related to the structure of samples. The products from fast pyrolysis of xylan mainly included acetic acid, furfural, and cyclopentenone etc.. and the products of lignin were predominantly composed of phenols, such as alkylphenols. guaiacols and syringols, as well as some aromatic hydrocarbons like benzene and toluene.
The selective pyrolysis of biomass and its components was also studied by using the thermogravimetric analyzer coupled with a Fourier transform infrared (TG-FTIR) spectrometry. All the three zeolite catalysts HZSM-5, H-β and USY had significant influence on the dehydration reaction, resulting in an increase of weight loss in the initial stage, and meanwhile affected the char formation process during the final stage. The addition of USY had the most obvious effect on the dehydration reaction, and the effect of HZSM-5and H-β focused on the inhibition of the char formation. Though the pyrolysis products were nearly the same, their release intensities changed after the addition of catalysts. It was observed that the yield of oxygenated compounds reduced compared with pure samples pyrolysis, but the yield of light gases increased such as CO, CO2and methane. The presence of USY enhanced the conversion of oxygenated compounds mainly to water and CO2, while the addition of HZSM-5and H-β promoted the secondary cracking of residual chars to form light gases CO. CO2and methane.
In view of the sequent researches on classification and upgrading of bio-oil for high-quality applications, pyrolysis behaviors of bio-oil fractions were studied on the TG-FTIR analyzer. combined with the first separation of bio-oil into fractions by using the molecular distillation technique. The obtained light fractions were constituted of water and acidic chemical, which began to loss weight at very low temperature by evaporation or was decomposed into small molecular compounds (CO2. CO. acetic acid, alcohols etc.) before200℃. Heavy fractions contained more compounds of phenols and sugars with high boiling point temperature and no water, so its heating value was highest and the stability was best among the three fractions. The weight loss range of heavy fraction was wide and the yield of char was high up to30wt%. During pyrolysis, self-evaporation was dominant at lower temperature, and decomposition was leading at higher temperature to produce more stable chemicals. The pyrolysis behavior of middle fraction was between light fraction and heavy fraction with the most kinds of products. Its yield was lowest, so it was regarded as light fraction or heavy fraction selectively based on the experimental conditions.
引文
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