强化木质纤维素干消化产气机理研究
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摘要
稻草和互花米草都属于木质纤维素。稻草的废弃与焚烧,以及互花米草的疯长,带来严重的环境污染与生态问题和重大的经济损失。合理利用稻草和互花米草成了一个亟待解决的新问题。稻草和互花米草的干消化生产清洁的沼气,不仅解决其污染和危害,而且给当地居民带来经济的收益和生态环境的良性循环；从而激发当地居民的积极性,积极参与禁止稻草焚烧和控制互花米草疯长的活动。
本论文考察石灰预处理和干消化稻草过程中组分和结构的变化,揭示复杂的木质纤维素结构是限制微生物利用、降低稻草产气率的根本原因；试图通过高温、同时石灰处理与干消化工艺和两相工艺来强化木质纤维素结构的破坏、提高木质纤维素的水解效率,增加干消化互花米草的产气,以期为提高干消化木质纤维素的产气效率提供理论基础和技术指导。主要结果如下：
1.中温、干消化稻草的结构变化及产气特性。木质纤维素复杂结构导致了干消化的低水解速率,造成了低的生物转化效率和低的产气效率。60天干消化稻草的累积产气量达到278.1mL/g VS,产气转化率仅为39.9%;纤维素和半纤维相对含量分别降低22.4%和13.1%,而木质素相对含量增加了59%。石灰预处理导致乙酰基链断裂,致使木质素和多糖的去除；预处理过程中结晶区氢键的重组导致结晶指数的增加；发酵阶段主要通过p-1,4糖苷键断裂实现脱聚、结晶区氢键改变实现晶体结构破坏,最终实现多糖的降解。预处理和干消化显著影响稻草的热解特性。一级热解动力学很好的模拟了原稻草、预处理与干消化后稻草热解的主失重阶段,活化能在42.27-47.82KJ/mol之间变化。
2.高温强化互花米草的产气效率。高温强化干消化的产气速率和木质素纤维素降解,产气率从181.2mL/g VS(中温)增加到283.9mL/g VS(高温),生物转化率从32.2%(中温)提高到50.4%(高温),VS去除率从57.3%(中温)提高到69%(高温)。
3.同时石灰处理与干消化工艺强化干消化互花米草的产气效率。同时石灰处理与干消化工艺厌氧发酵木质纤维素在技术上是可行的,有最高的初始产气速率(k=0.023d-1)和最大的VS去除率(71.9%),厌氧发酵的前40天的产气率达到192.7mL/g VS,但干消化过程存在着抑制。Na+、K+和Ca2+阳离子并不是导致同时石灰处理与干消化工艺产气抑制的根本原因。
4.高温强化互花米草结构破坏机理。高温强化了木质纤维素结构的破坏,同时石灰处理与干消化工艺实现了最大的结构破坏和组分去除。木质素去除主要出现在预处理阶段,主要通过乙酰基链断裂、羧基碳、芳碳和酚碳的脱除来实现。干消化去除多糖,主要通过p,1-4糖苷键断裂、多糖碳和乙缩醛碳的脱除。石灰预处理对木质纤维素素结构破坏有限,需要强化预处理,提高木质纤维素的生物降解性。预处理和干消化显著影响互花米草的热解特性。一级热解动力学很好的模拟了原、预处理与干消化后互花米草的主失重阶段,预处理增加活化能而干消化降低活化能。
5.两相工艺强化木质纤维素的水解效率,增加干消化互花米草的产气效率。补加尿素调节碳氮比,创造更适宜生存环境、试图增加水解效率,但导致气相甲烷菌的氨抑制;FA抑制产甲烷反应,其值高于55mg/L就会对高温产甲烷菌产生严重的抑制。两相干消化互花米草的产气量为98.6mL/g VS,转化率仅为17.5%。木质纤维素复杂结构导致了低的水解效率,需要大幅度地强化预处理效果,增加木质纤维素结构的破坏,才能明显提高干消化木质纤维素的产气量。
Rice straw is one of main agricultural residues in country and smooth cordgrass is main salt-mash plant at the coast of China Sea. Rice straw and smooth cordgrass all belong to lignocelluloses. Recently open-field burning of rice straw and excessive spread of smooth cordgrass has lead to seriously environmental pollution, economical loss and ecological problem. Effective utilization of rice straw and smooth cordgrass has become a new problem. Dry digestion of rice straw or smooth cordgrass for biogas production may not only solve the pollution question, but also may bring economical and environmental benefits to local inhabitants. This helps to further control and lessen their negative impacts on environment.
In this work, an investigation on changes of lignocellulosic composition and structure was performed during lime pretreatment and dry digestion of rice straw; changes of complex lignocelluloses structure was discussed by X-ray, FTIR and TG analysis. Result showed that lignocellulosic structure was main limited factor of low biogas yield. Enhancing measures for biogas production, including thermophilic conditions, simultaneous lime treatment and dry digestion process, and two-phase process was carried out. Main contents and results are as follows:
In chapter2, structure changes and biogas production characteristics of rice straw were investigated during lime pretreatment and dry digestion. Low hydrolysis rate limits utilization of lignocelluloses for microorganism. Cumulative biogas yield reached278.1mL/g VS at60days dry digestion of rice straw, and the relative content of cellulose and hemicellulose decreased23.4%and13.1%, respectively; and whereas lignin content relative increased59%. Lime pretreatment resulted in the lignin and polysaccharides removal by the cleavage of ester linkage and rearrangement of hydrogen bonding in the crystalline region. The decomposition of polysaccharides was carried out by the cleavage of β,1-4glycosidic bonds linkages during dry digestion. Biogas conversation rate was only39.9%and measures need be adopted for the improvement of biogas production for dry digestion of lignocelluloses. Pretreatment and dry digestion had obvious influence on pyrolysis characteristics of rice straw. The part of main weight loss for pyrolysis rice straw very fit first-order kinetic model, and the value of activate energy ranged from42.27to47.82KJ/mol.
In chapter3, enhancing biogas production was discussed by thermophilic conditions. Thermophilic conditions enhanced biogas production and lignocellulosic bioconversion. During60days dry digestion, biogas yield reached283.9mL/g VS and181.2mL/g VS at55℃and35℃, respectively. Compared with32.2%biogas conversion rate and57.3%VS reduction at mesophilic condition (35℃), thermophilic condition (55℃) obtained50.4%biogas conversion rate and69%VS reduction.
In chapter3, enhancing biogas production was also discussed by simultaneous lime treatment and dry digestion (SLTTD) process. SLTTD process was achieved in one reactor with highest initial biogas production constant (k=0.023d-1) and VS removal rate (71.9%). Biogas yield with192.7mL/g VS was obtained at the beginning of40days during60days dry digestion, but inhibition of anaerobic microorganisms occurred at SLTTD process during dry digestion. Sodium, potassium and calcium ions were not the cause of inhibition for SLTTD process.
In chapter4, the breakage of lignocellusic structure was investigated at mesophilic and thermophilic conditions. Thermophilic conditions brought a greater rupture of lignocellulosic structure. Highest breakage of lignocelluloses and higher composition remove was carried out in SLTTD experiment. Lignin removal occurred at lime pretreatment phase by the cleavage of ester linkage and the reducing carboxyl, aryl and phenolic C functional group. Polysaccharides decomposition happened at dry digestion by the cleavage of β,1-4glycosidic bonds linkages, and the reduction of carbohydrate and Di-O-alkl C functional group. The part of main weight loss very fit a first-order kinetic model for smooth cordgrass pyrolysis. The increase in activate energy appeared at pretreatment phase, and whereas the decrease occurred at dry digestion phase.
In chapter5, Two-phase digestion of smooth cordgrass was investigated for improving hydrolysis rate of lignocelluloses. Free ammonia (FA) inhibition occurred at two-phase process, when the C/N rate of digester was adjusted by adding urea. Adding chemical for adjusting C/N rate should be very cautious and co-digestion with organic wastes containing high nitrogen would be better choice for adjusting C/N rate. When FA concentration was over55mg/L, biogas production rate obviously decreased or stopped. Biogas yield was only98.6mL/g VS with17.5%bioconversion rate during53days two-phase digestion of smooth cordgrass. Hydrolysis of smooth cordgrass was a limited step during anaerobic digestion and lignocellulose pretreatment need be a great scale improved for higher biogas production.
本论文考察石灰预处理和干消化稻草过程中组分和结构的变化,揭示复杂的木质纤维素结构是限制微生物利用、降低稻草产气率的根本原因；试图通过高温、同时石灰处理与干消化工艺和两相工艺来强化木质纤维素结构的破坏、提高木质纤维素的水解效率,增加干消化互花米草的产气,以期为提高干消化木质纤维素的产气效率提供理论基础和技术指导。主要结果如下：
1.中温、干消化稻草的结构变化及产气特性。木质纤维素复杂结构导致了干消化的低水解速率,造成了低的生物转化效率和低的产气效率。60天干消化稻草的累积产气量达到278.1mL/g VS,产气转化率仅为39.9%;纤维素和半纤维相对含量分别降低22.4%和13.1%,而木质素相对含量增加了59%。石灰预处理导致乙酰基链断裂,致使木质素和多糖的去除；预处理过程中结晶区氢键的重组导致结晶指数的增加；发酵阶段主要通过p-1,4糖苷键断裂实现脱聚、结晶区氢键改变实现晶体结构破坏,最终实现多糖的降解。预处理和干消化显著影响稻草的热解特性。一级热解动力学很好的模拟了原稻草、预处理与干消化后稻草热解的主失重阶段,活化能在42.27-47.82KJ/mol之间变化。
2.高温强化互花米草的产气效率。高温强化干消化的产气速率和木质素纤维素降解,产气率从181.2mL/g VS(中温)增加到283.9mL/g VS(高温),生物转化率从32.2%(中温)提高到50.4%(高温),VS去除率从57.3%(中温)提高到69%(高温)。
3.同时石灰处理与干消化工艺强化干消化互花米草的产气效率。同时石灰处理与干消化工艺厌氧发酵木质纤维素在技术上是可行的,有最高的初始产气速率(k=0.023d-1)和最大的VS去除率(71.9%),厌氧发酵的前40天的产气率达到192.7mL/g VS,但干消化过程存在着抑制。Na+、K+和Ca2+阳离子并不是导致同时石灰处理与干消化工艺产气抑制的根本原因。
4.高温强化互花米草结构破坏机理。高温强化了木质纤维素结构的破坏,同时石灰处理与干消化工艺实现了最大的结构破坏和组分去除。木质素去除主要出现在预处理阶段,主要通过乙酰基链断裂、羧基碳、芳碳和酚碳的脱除来实现。干消化去除多糖,主要通过p,1-4糖苷键断裂、多糖碳和乙缩醛碳的脱除。石灰预处理对木质纤维素素结构破坏有限,需要强化预处理,提高木质纤维素的生物降解性。预处理和干消化显著影响互花米草的热解特性。一级热解动力学很好的模拟了原、预处理与干消化后互花米草的主失重阶段,预处理增加活化能而干消化降低活化能。
5.两相工艺强化木质纤维素的水解效率,增加干消化互花米草的产气效率。补加尿素调节碳氮比,创造更适宜生存环境、试图增加水解效率,但导致气相甲烷菌的氨抑制;FA抑制产甲烷反应,其值高于55mg/L就会对高温产甲烷菌产生严重的抑制。两相干消化互花米草的产气量为98.6mL/g VS,转化率仅为17.5%。木质纤维素复杂结构导致了低的水解效率,需要大幅度地强化预处理效果,增加木质纤维素结构的破坏,才能明显提高干消化木质纤维素的产气量。
Rice straw is one of main agricultural residues in country and smooth cordgrass is main salt-mash plant at the coast of China Sea. Rice straw and smooth cordgrass all belong to lignocelluloses. Recently open-field burning of rice straw and excessive spread of smooth cordgrass has lead to seriously environmental pollution, economical loss and ecological problem. Effective utilization of rice straw and smooth cordgrass has become a new problem. Dry digestion of rice straw or smooth cordgrass for biogas production may not only solve the pollution question, but also may bring economical and environmental benefits to local inhabitants. This helps to further control and lessen their negative impacts on environment.
In this work, an investigation on changes of lignocellulosic composition and structure was performed during lime pretreatment and dry digestion of rice straw; changes of complex lignocelluloses structure was discussed by X-ray, FTIR and TG analysis. Result showed that lignocellulosic structure was main limited factor of low biogas yield. Enhancing measures for biogas production, including thermophilic conditions, simultaneous lime treatment and dry digestion process, and two-phase process was carried out. Main contents and results are as follows:
In chapter2, structure changes and biogas production characteristics of rice straw were investigated during lime pretreatment and dry digestion. Low hydrolysis rate limits utilization of lignocelluloses for microorganism. Cumulative biogas yield reached278.1mL/g VS at60days dry digestion of rice straw, and the relative content of cellulose and hemicellulose decreased23.4%and13.1%, respectively; and whereas lignin content relative increased59%. Lime pretreatment resulted in the lignin and polysaccharides removal by the cleavage of ester linkage and rearrangement of hydrogen bonding in the crystalline region. The decomposition of polysaccharides was carried out by the cleavage of β,1-4glycosidic bonds linkages during dry digestion. Biogas conversation rate was only39.9%and measures need be adopted for the improvement of biogas production for dry digestion of lignocelluloses. Pretreatment and dry digestion had obvious influence on pyrolysis characteristics of rice straw. The part of main weight loss for pyrolysis rice straw very fit first-order kinetic model, and the value of activate energy ranged from42.27to47.82KJ/mol.
In chapter3, enhancing biogas production was discussed by thermophilic conditions. Thermophilic conditions enhanced biogas production and lignocellulosic bioconversion. During60days dry digestion, biogas yield reached283.9mL/g VS and181.2mL/g VS at55℃and35℃, respectively. Compared with32.2%biogas conversion rate and57.3%VS reduction at mesophilic condition (35℃), thermophilic condition (55℃) obtained50.4%biogas conversion rate and69%VS reduction.
In chapter3, enhancing biogas production was also discussed by simultaneous lime treatment and dry digestion (SLTTD) process. SLTTD process was achieved in one reactor with highest initial biogas production constant (k=0.023d-1) and VS removal rate (71.9%). Biogas yield with192.7mL/g VS was obtained at the beginning of40days during60days dry digestion, but inhibition of anaerobic microorganisms occurred at SLTTD process during dry digestion. Sodium, potassium and calcium ions were not the cause of inhibition for SLTTD process.
In chapter4, the breakage of lignocellusic structure was investigated at mesophilic and thermophilic conditions. Thermophilic conditions brought a greater rupture of lignocellulosic structure. Highest breakage of lignocelluloses and higher composition remove was carried out in SLTTD experiment. Lignin removal occurred at lime pretreatment phase by the cleavage of ester linkage and the reducing carboxyl, aryl and phenolic C functional group. Polysaccharides decomposition happened at dry digestion by the cleavage of β,1-4glycosidic bonds linkages, and the reduction of carbohydrate and Di-O-alkl C functional group. The part of main weight loss very fit a first-order kinetic model for smooth cordgrass pyrolysis. The increase in activate energy appeared at pretreatment phase, and whereas the decrease occurred at dry digestion phase.
In chapter5, Two-phase digestion of smooth cordgrass was investigated for improving hydrolysis rate of lignocelluloses. Free ammonia (FA) inhibition occurred at two-phase process, when the C/N rate of digester was adjusted by adding urea. Adding chemical for adjusting C/N rate should be very cautious and co-digestion with organic wastes containing high nitrogen would be better choice for adjusting C/N rate. When FA concentration was over55mg/L, biogas production rate obviously decreased or stopped. Biogas yield was only98.6mL/g VS with17.5%bioconversion rate during53days two-phase digestion of smooth cordgrass. Hydrolysis of smooth cordgrass was a limited step during anaerobic digestion and lignocellulose pretreatment need be a great scale improved for higher biogas production.
引文
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