生物质发酵制氢过程基础研究
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摘要
在化石能源日益枯竭和环境污染日趋严重的背景下,开发可再生新能源,解决人类面临的能源和环境危机,成为当今世界共同关注和亟待解决的问题。生物质发酵制氢技术因具有能源和环保双重功效,得到了广泛重视,并取得了大量研究成果。但是,该技术尚处于实验研究阶段,菌种稳定性差、底物利用率低、过程机理尚不明晰等成为其向产业化发展的瓶颈。基于此,本文在现有基础上,对牛粪堆肥为菌种的生物质发酵制氢过程进行了关键工艺条件优化、机理探讨、过程动力学和相关流体相平衡研究及废液资源化利用,具有重要的学术理论意义和工程应用价值。
运用响应面法进行生物质发酵制氢菌种富集实验设计和实验,建立以比产氢量为优化目标的响应面模型,预测出生物质发酵制氢菌种的最优富集条件。5批验证实验的蔗糖比产氢量重复性好,均值为270.26mL/(g·sucrose),与模型预测值一致。
提出玉米秸秆稀酸辅助蒸汽爆破再Fe2+催化水解预处理技术。进行了该技术的响应面优化设计和实验,建立了以糖化率为目标的响应面模型。在模型预测的优化工艺条件下,玉米秸秆的糖化率达到35.5%,比产氢量为151.50mLH2/(g·corn stalk)。
研究表明,对生物质发酵制氢菌种有毒害作用的是生物质预处理过程中生成的糠醛、5-羟甲基糠醛、乙酸等副产物。提出对玉米秸秆水解液进行活性炭吸附脱毒。在所得吸附脱毒较优条件下,糠醛、5-羟甲基糠醛、乙酸等的脱除率分别为91.5%、87.86%、20.52%,总还原糖损失率7.09%。对活性炭吸附糠醛、5.羟甲基糠醛、乙酸及还原糖过程的吸附动力学研究表明,活性炭对各物质的吸附过程均符合拟二级动力学模型。经脱毒后,玉米秸秆比产氢量提高至(?)169.74mL H2/(g·corn stalk)。
在30L反应器中实验测得蔗糖、葡萄糖、木糖、玉米秸秆等4种底物发酵制H2过程动力学数据,建立4种底物发酵制H2过程中微生物生长、H2生成、底物消耗3类动力学模型。对比4种底物3类动力学模型参数表明,葡萄糖最有利于生物质发酵制氢。添加3.0g/L葡萄糖时玉米秸秆发酵制H2过程的比产氢量达213.4mL H2/(g·corn stalk),秸秆利用率达60.85%,反应稳定期气相产物中H2浓度大于50%。探讨了生物质发酵制氢过程的机理,以牛粪堆肥富集菌种进行的玉米秸秆发酵制氢过程,是以丁酸型发酵为主的发酵过程。
采用激光动态法测定了生物质发酵制氢过程关键中间体木糖和葡萄糖在脂肪酸、混合脂肪酸、脂肪酸+水混合溶剂中的溶解度,运用Apelblat模型进行了关联,确定方程参数。由溶解度数据计算出木糖、葡萄糖在脂肪酸、混合脂肪酸、脂肪酸+水混合溶剂中的标准溶解焓△solH°、标准溶解熵△solS°和标准溶解吉布斯自由能变△solG°。△solH°＞0,表明木糖、葡萄糖分子与溶剂分子之间的交互作用弱于分子间的缔合作用,木糖、葡萄糖溶于溶剂的过程中缔合键的断裂占主导地位,为吸热过程。△solH°＞0,表明木糖、葡萄糖分子溶解进入溶剂中时扰乱了溶剂分子的排列,使体系的有序度降低,混乱度增大,熵增加。△solH°、△solHS°均为正值,说明木糖、葡萄糖在溶剂中的溶解为熵驱动过程。
以磷酸三丁酯一正辛醇为络合剂,对玉米秸秆发酵制氢废液中主要副产物混合酸进行络合萃取回收。在优化所得萃取、反萃取条件下,三级错流萃取混合酸的萃取率达98.76%,二级反萃取混合酸的反萃取率达99.10%,经10次萃取.反萃取的络合剂,对废液中混合酸的萃取效果基本不变。
研究结果既将加快生物质发酵制氢技术进步,也将在一定程度上促进相关学科发展。
Under the background of increasing depletion of fossil energy and environmental pollution worsening, development of renewable energy to deal with current energy and environmental crisis has become problems common concerned and to be solved in the world today. Bio-hydrogen production from biomass has been attracting extensive attention as an environmentally friendly process that does not consume fossil fuels. And a lot of research results have been made. However, this technology remains in an early stage of experimentation and investigation. Strains of poor stability, low utilization rate of substrate, and process mechanism of fuzzy become the bottlenecks which hinder its industrial development. Based on this and existing research, optimization of critical process conditions, discussion on mechanism, study on kinetics and relevant fluid phase equilibria, and resource utilization of fermentation liquid waste were conducted on process of bio-hydrogen production from biomass with dairy manure compost as strains. The results will have a great significance in science theory and engineering applications.
Experimental design and experiments of strains enrichment process for bio-hydrogen production were carried out by response surface method. Response surface model with yield of hydrogen production as the optimization goal was built. Optimum conditions of strains enrichment of bio-hydrogen production from biomass was forecasted. The yield of hydrogen production of sucrose of5batch verifying experiments had excellent repetition. The average value was270.26mL/(g·sucrose) which was consistent with the model prediction.
Two-stage pretreatment of corn stalk by dilute sulfuric acid assisted steam explosion and enhancement of dilute acid hydrolysis with Fe2+was proposed. Experimental design and experiments of this technology were carried out. Response surface model with saccharification rate of corn stalk as the optimization goal was built. Under the optimal conditions of model prediction, saccharification rate of corn stalk reached35.5%, and the yield of hydrogen production was151.50mL H2/(g·corn stalk).
The study showed that byproducts of biomass pretreatment process such as furfural,5-hydroxymethylfurfural, acetic acid were toxic to strains of bio-hydrogen production from biomass. Activated carbon adsorption detoxification of corn stalk hydrolysate was proposed. Under the optimal conditions of detoxification, removal rate of furfural,5-hydroxymethylfurfural, acetic acid were91.5%,87.86%, and20.52%, respectively. And the loss ratio of total reducing sugar was7.09%. The results of kinetics studies of activated carbon adsorption of furfural,5-hydroxymethylfurfural, acetic acid, and total reducing sugar indicated that activated carbon adsorption process of each substance followed the pseudo-second-order kinetics. And the yield of hydrogen production of corn stalk increased to169.74mL H2/(g·corn stalk) after detoxification.
Kinetics data of bio-hydrogen production of sucrose, glucose, xylose, and corn stalk in30L reactor were obtained. The kinetic models of microbial growth, hydrogen generation, and substrate consumption of the four substrates were built. The comparison of three kinds of kinetic model parameters of four substrates showed that glucose was best for the bio-hydrogen production. The yield of hydrogen production of bio-hydrogen production from corn stalk by adding glucose of3.0g/L reached213.4mL H2/(g·corn stalk). The utilization rate of corn stalk reached60.85%, and H2concentration in gas products at the reaction stationary phase was more than50%. The discussion of process mechanism of bio-hydrogen production showed that the hydrogen was mainly produced by the butyric acid type fermentation in the process of bio-hydrogen production from corn stalk with dairy manure compost as strains.
Using the laser monitoring observation technique, the solubilities of xylose and glucose which are the key intermediates of bio-hydrogen production process in fatty acid, mixed fatty acids, and mixed solvents of fatty acids+water were determined. The experimental data were correlated with Apelblat model, and the equation parameters were obtained completely. The standard enthalpy, standard entropy and standard Gibbs free energy change of xylose and glucose in fatty acid, mixed fatty acids, and mixed solvents of fatty acids+water were calculated.△solH>0reveals that the interactions between the xylose, or glucose and solvent molecules are weaker than those between the solvent molecules. The dissolved process is endothermic and the break of association bond is principal.△solS>0shows that when xylose, or glucose dissolved into solvents, the array of solvents molecular was disturbed, the degree of order decrease, randomness increases and entropy increases. The positive△solH and AsolS reveal that the dissolution process of xylose, or glucose in the studied systems were entropy-driven processes.
The complexation extraction with tributyl phosphate-octanol as complexing agent was used to recover the mixed carboxylic acid in the fermentation liquid waste of bio-hydrogen production from corn stalk. Under the optimized extraction and back extraction conditions, the extraction rate of mixed carboxylic acid reached98.76%, and the back-extraction rate reached99.10%. The extraction effect of complexing agent was essentially unchanged after ten times of extraction and back-extraction.
The results not only will be expedite technological progress of bio-hydrogen production from biomass, but also will be sure to promote the development of relevant subjects.
运用响应面法进行生物质发酵制氢菌种富集实验设计和实验,建立以比产氢量为优化目标的响应面模型,预测出生物质发酵制氢菌种的最优富集条件。5批验证实验的蔗糖比产氢量重复性好,均值为270.26mL/(g·sucrose),与模型预测值一致。
提出玉米秸秆稀酸辅助蒸汽爆破再Fe2+催化水解预处理技术。进行了该技术的响应面优化设计和实验,建立了以糖化率为目标的响应面模型。在模型预测的优化工艺条件下,玉米秸秆的糖化率达到35.5%,比产氢量为151.50mLH2/(g·corn stalk)。
研究表明,对生物质发酵制氢菌种有毒害作用的是生物质预处理过程中生成的糠醛、5-羟甲基糠醛、乙酸等副产物。提出对玉米秸秆水解液进行活性炭吸附脱毒。在所得吸附脱毒较优条件下,糠醛、5-羟甲基糠醛、乙酸等的脱除率分别为91.5%、87.86%、20.52%,总还原糖损失率7.09%。对活性炭吸附糠醛、5.羟甲基糠醛、乙酸及还原糖过程的吸附动力学研究表明,活性炭对各物质的吸附过程均符合拟二级动力学模型。经脱毒后,玉米秸秆比产氢量提高至(?)169.74mL H2/(g·corn stalk)。
在30L反应器中实验测得蔗糖、葡萄糖、木糖、玉米秸秆等4种底物发酵制H2过程动力学数据,建立4种底物发酵制H2过程中微生物生长、H2生成、底物消耗3类动力学模型。对比4种底物3类动力学模型参数表明,葡萄糖最有利于生物质发酵制氢。添加3.0g/L葡萄糖时玉米秸秆发酵制H2过程的比产氢量达213.4mL H2/(g·corn stalk),秸秆利用率达60.85%,反应稳定期气相产物中H2浓度大于50%。探讨了生物质发酵制氢过程的机理,以牛粪堆肥富集菌种进行的玉米秸秆发酵制氢过程,是以丁酸型发酵为主的发酵过程。
采用激光动态法测定了生物质发酵制氢过程关键中间体木糖和葡萄糖在脂肪酸、混合脂肪酸、脂肪酸+水混合溶剂中的溶解度,运用Apelblat模型进行了关联,确定方程参数。由溶解度数据计算出木糖、葡萄糖在脂肪酸、混合脂肪酸、脂肪酸+水混合溶剂中的标准溶解焓△solH°、标准溶解熵△solS°和标准溶解吉布斯自由能变△solG°。△solH°＞0,表明木糖、葡萄糖分子与溶剂分子之间的交互作用弱于分子间的缔合作用,木糖、葡萄糖溶于溶剂的过程中缔合键的断裂占主导地位,为吸热过程。△solH°＞0,表明木糖、葡萄糖分子溶解进入溶剂中时扰乱了溶剂分子的排列,使体系的有序度降低,混乱度增大,熵增加。△solH°、△solHS°均为正值,说明木糖、葡萄糖在溶剂中的溶解为熵驱动过程。
以磷酸三丁酯一正辛醇为络合剂,对玉米秸秆发酵制氢废液中主要副产物混合酸进行络合萃取回收。在优化所得萃取、反萃取条件下,三级错流萃取混合酸的萃取率达98.76%,二级反萃取混合酸的反萃取率达99.10%,经10次萃取.反萃取的络合剂,对废液中混合酸的萃取效果基本不变。
研究结果既将加快生物质发酵制氢技术进步,也将在一定程度上促进相关学科发展。
Under the background of increasing depletion of fossil energy and environmental pollution worsening, development of renewable energy to deal with current energy and environmental crisis has become problems common concerned and to be solved in the world today. Bio-hydrogen production from biomass has been attracting extensive attention as an environmentally friendly process that does not consume fossil fuels. And a lot of research results have been made. However, this technology remains in an early stage of experimentation and investigation. Strains of poor stability, low utilization rate of substrate, and process mechanism of fuzzy become the bottlenecks which hinder its industrial development. Based on this and existing research, optimization of critical process conditions, discussion on mechanism, study on kinetics and relevant fluid phase equilibria, and resource utilization of fermentation liquid waste were conducted on process of bio-hydrogen production from biomass with dairy manure compost as strains. The results will have a great significance in science theory and engineering applications.
Experimental design and experiments of strains enrichment process for bio-hydrogen production were carried out by response surface method. Response surface model with yield of hydrogen production as the optimization goal was built. Optimum conditions of strains enrichment of bio-hydrogen production from biomass was forecasted. The yield of hydrogen production of sucrose of5batch verifying experiments had excellent repetition. The average value was270.26mL/(g·sucrose) which was consistent with the model prediction.
Two-stage pretreatment of corn stalk by dilute sulfuric acid assisted steam explosion and enhancement of dilute acid hydrolysis with Fe2+was proposed. Experimental design and experiments of this technology were carried out. Response surface model with saccharification rate of corn stalk as the optimization goal was built. Under the optimal conditions of model prediction, saccharification rate of corn stalk reached35.5%, and the yield of hydrogen production was151.50mL H2/(g·corn stalk).
The study showed that byproducts of biomass pretreatment process such as furfural,5-hydroxymethylfurfural, acetic acid were toxic to strains of bio-hydrogen production from biomass. Activated carbon adsorption detoxification of corn stalk hydrolysate was proposed. Under the optimal conditions of detoxification, removal rate of furfural,5-hydroxymethylfurfural, acetic acid were91.5%,87.86%, and20.52%, respectively. And the loss ratio of total reducing sugar was7.09%. The results of kinetics studies of activated carbon adsorption of furfural,5-hydroxymethylfurfural, acetic acid, and total reducing sugar indicated that activated carbon adsorption process of each substance followed the pseudo-second-order kinetics. And the yield of hydrogen production of corn stalk increased to169.74mL H2/(g·corn stalk) after detoxification.
Kinetics data of bio-hydrogen production of sucrose, glucose, xylose, and corn stalk in30L reactor were obtained. The kinetic models of microbial growth, hydrogen generation, and substrate consumption of the four substrates were built. The comparison of three kinds of kinetic model parameters of four substrates showed that glucose was best for the bio-hydrogen production. The yield of hydrogen production of bio-hydrogen production from corn stalk by adding glucose of3.0g/L reached213.4mL H2/(g·corn stalk). The utilization rate of corn stalk reached60.85%, and H2concentration in gas products at the reaction stationary phase was more than50%. The discussion of process mechanism of bio-hydrogen production showed that the hydrogen was mainly produced by the butyric acid type fermentation in the process of bio-hydrogen production from corn stalk with dairy manure compost as strains.
Using the laser monitoring observation technique, the solubilities of xylose and glucose which are the key intermediates of bio-hydrogen production process in fatty acid, mixed fatty acids, and mixed solvents of fatty acids+water were determined. The experimental data were correlated with Apelblat model, and the equation parameters were obtained completely. The standard enthalpy, standard entropy and standard Gibbs free energy change of xylose and glucose in fatty acid, mixed fatty acids, and mixed solvents of fatty acids+water were calculated.△solH>0reveals that the interactions between the xylose, or glucose and solvent molecules are weaker than those between the solvent molecules. The dissolved process is endothermic and the break of association bond is principal.△solS>0shows that when xylose, or glucose dissolved into solvents, the array of solvents molecular was disturbed, the degree of order decrease, randomness increases and entropy increases. The positive△solH and AsolS reveal that the dissolution process of xylose, or glucose in the studied systems were entropy-driven processes.
The complexation extraction with tributyl phosphate-octanol as complexing agent was used to recover the mixed carboxylic acid in the fermentation liquid waste of bio-hydrogen production from corn stalk. Under the optimized extraction and back extraction conditions, the extraction rate of mixed carboxylic acid reached98.76%, and the back-extraction rate reached99.10%. The extraction effect of complexing agent was essentially unchanged after ten times of extraction and back-extraction.
The results not only will be expedite technological progress of bio-hydrogen production from biomass, but also will be sure to promote the development of relevant subjects.
引文
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