木质纤维素水热预处理及连续效膜蒸馏的过程研究
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摘要
在木质纤维素生化转化为乙醇的过程中，预处理单元作为该过程的核心反应单元，对后续酶解发酵步骤的效率起着决定性作用。浓缩单元作为过程的分离单元，可用于预水解液、酶解液和过程废水等含不挥发性溶质水溶液的浓缩，其性能指标也对整个过程能量的高效利用和公用工程中纯水的循环使用起到决定性作用。本文围绕预处理和浓缩这两个关键单元操作，旨在建立从木质纤维素到乙醇的高效转化路线和平台，研究内容主要分为两部分：1）研究植物细胞壁化学组成和超微结构在预处理过程中的变化规律以及这些变化如何对后续生化转化过程产生影响；2）研究相关高效浓缩过程的开发以达到整个流程较高的热量利用率和浓缩效率。
水热预处理过程作用于生物质本身，会造成葡聚糖、木聚糖和木质素三者之间的分离和改变。针对不对称反应温度曲线，建立修改过的处理强度因子，统一表征不同条件的反应进程。借助于物料衡算和多维表征手段，研究过程输入参数包括处理强度、固液比和pH，对各组分水热反应化学行为的关联及其对后续酶解发酵的影响，研究结果发现对于热水/蒸汽处理后酶解整个糖化过程，葡萄糖和木糖得率存在权衡取舍问题，但通过引入第三个独立参数pH，可以同时达到较高的葡萄糖（>90%）和木糖得率（>85%）。木聚糖所涉及到的水解、降解和沉积反应和木质素的水解反应同pH密切相关。预水解液中的可溶性寡糖和某些降解产物会在酶解时表现出不同的抑制作用，而呋喃类物质和一些芳香醛/酮/酸则被认为是酿酒酵母发酵的主要抑制剂。控制水热过程的pH在中性范围，其过程总体指标要优于未控制过程。综合定量和定性实验数据，清晰且系统的水热过程作用机制被呈现出来。
连续效膜蒸馏过程通过将严格平行的气隙式膜蒸馏中空纤维组件同内换热功能耦连一起，使得过程造水比在实验研究的范围内最高达到了13.8。应用面心式中心复合实验设计方法，研究过程操作参数，包括冷的进管温度、热的进膜温度和流量对过程性能指标（通量、造水比和蒸发效率）的影响规律。通过借助一系列控制传递方程组用于解释并预测过程性能，发现所建立的数学模型可以很好的描述实验数据。因此获得了可借助于模型进一步提高造水比的方法。成功采用连续效膜蒸馏技术高效浓缩稀糖溶液12倍至最终浓度20%wt，最终造水比为8.2，实现了连续效膜蒸馏过程的较高能量利用率。
In biochemical conversion process from lignocellulose to ethanol, thepretreatment step, as the core reaction unit in the whole process, plays a decisive rolein the efficiency of subsequent enzymatic hydrolysis and fermentation steps. Theseparation unit for concentrating prehydrolyzate, enzymatic hydrolyzate and processwastewater containing non-volatile solutes generated in the whole process, whoseperformance also plays a vital role in the efficiency of energy utilization and recycleof utility water. Focusing on the above two key unit operations, in this dissertation,how the chemical composition and ultrastructure of plant cell wall change withdifferent pretreatment conditions, and how these changes impact the subsequentbiochemical conversion were studied. Research related to development ofenergy-efficient concentration process in order to achieve high performance ratio wasalso conducted. The objective of this dissertation was aimed at establishing a highlyefficient route and platform that could convert lignocellulose to ethanol.
Hydrothermal processing of corn stover, as a pretreatment step, caused a varietyof effects including fractionation of glucan, xylan and lignin from whole biomassmatrix and modification of physicochemical properties in both solid and liquidfractions. A modified severity factor for non-isothermal pretreatment with asymmetrictemperature curve was successfully applied as a reaction ordinate to evaluate differentpretreatment conditions. In light of material balance and multiple characterizationmethods, the influence of process parameters including severity facor, solid loadingand pH on the kinetic behaviors of major components in lignocellulose duringhydrothermal pretreatment and these influences on the subsequent bioconversion werestudied. It was found that a trade-off between glucose and xylose yield existed aftereither aqueous/steam pretreatment followed by enzymatic hydrolysis, but this couldbe eliminated by introduction of the third parameter, pH. High yields in glucose(>90%) and xylose (>85%) were simultaneously obtained. Hydrolysis, degradationand condensation reaction involved in xylan chemistry and hydrolysis of lignin werestrongly pH-dependent. Soluble xylo-oligmers in the prehydrolyzate and somedegradation products were verified as the inhibitory compounds to enzymatichydrolysis but behaved in a different way. Furan derivatives and some aromatic aldehydes/ketones/acids were assumed to be key potential fermentation inhibitors.Aqueous pretreatment controlling its pH at a near neutral value showed advantagesover that without pH control. Based upon the quantitative and qualitative informationon destruction of plant cell wall, a clear and systematic picture of mechanisims ofhydrothermal pretreatment was finally provided.
A continuous-effect membrane distillation (CEMD) process was developed byequipping air gap membrane distillation (AGMD)-based and strictly-parallel hollowfiber module with internal heat recovery. Within the studied experimental range, themaximum PR of13.8was obtained. A face-centered central composite experimentaldesign was conducted to investigate the influences of operating variables includingcold-feed temperature, hot-feed temperature, and feed-in flow rate on the performancewhich was indicated by flux, performance ratio and evaporation efficiency. Atheoretical model based on governing transport equations was established to predictthe process performance and the model described the experimental data fairly well. Inlight of model, possible ways to further increase PR were predicted. The diluteaqueous sugar solution was successfully concentrated12-fold to a final concentrationof about20%wt by using CEMD process with a final PR of8.2, and the goal toestablish the high energy-efficiency concentration process was achieved.
水热预处理过程作用于生物质本身，会造成葡聚糖、木聚糖和木质素三者之间的分离和改变。针对不对称反应温度曲线，建立修改过的处理强度因子，统一表征不同条件的反应进程。借助于物料衡算和多维表征手段，研究过程输入参数包括处理强度、固液比和pH，对各组分水热反应化学行为的关联及其对后续酶解发酵的影响，研究结果发现对于热水/蒸汽处理后酶解整个糖化过程，葡萄糖和木糖得率存在权衡取舍问题，但通过引入第三个独立参数pH，可以同时达到较高的葡萄糖（>90%）和木糖得率（>85%）。木聚糖所涉及到的水解、降解和沉积反应和木质素的水解反应同pH密切相关。预水解液中的可溶性寡糖和某些降解产物会在酶解时表现出不同的抑制作用，而呋喃类物质和一些芳香醛/酮/酸则被认为是酿酒酵母发酵的主要抑制剂。控制水热过程的pH在中性范围，其过程总体指标要优于未控制过程。综合定量和定性实验数据，清晰且系统的水热过程作用机制被呈现出来。
连续效膜蒸馏过程通过将严格平行的气隙式膜蒸馏中空纤维组件同内换热功能耦连一起，使得过程造水比在实验研究的范围内最高达到了13.8。应用面心式中心复合实验设计方法，研究过程操作参数，包括冷的进管温度、热的进膜温度和流量对过程性能指标（通量、造水比和蒸发效率）的影响规律。通过借助一系列控制传递方程组用于解释并预测过程性能，发现所建立的数学模型可以很好的描述实验数据。因此获得了可借助于模型进一步提高造水比的方法。成功采用连续效膜蒸馏技术高效浓缩稀糖溶液12倍至最终浓度20%wt，最终造水比为8.2，实现了连续效膜蒸馏过程的较高能量利用率。
In biochemical conversion process from lignocellulose to ethanol, thepretreatment step, as the core reaction unit in the whole process, plays a decisive rolein the efficiency of subsequent enzymatic hydrolysis and fermentation steps. Theseparation unit for concentrating prehydrolyzate, enzymatic hydrolyzate and processwastewater containing non-volatile solutes generated in the whole process, whoseperformance also plays a vital role in the efficiency of energy utilization and recycleof utility water. Focusing on the above two key unit operations, in this dissertation,how the chemical composition and ultrastructure of plant cell wall change withdifferent pretreatment conditions, and how these changes impact the subsequentbiochemical conversion were studied. Research related to development ofenergy-efficient concentration process in order to achieve high performance ratio wasalso conducted. The objective of this dissertation was aimed at establishing a highlyefficient route and platform that could convert lignocellulose to ethanol.
Hydrothermal processing of corn stover, as a pretreatment step, caused a varietyof effects including fractionation of glucan, xylan and lignin from whole biomassmatrix and modification of physicochemical properties in both solid and liquidfractions. A modified severity factor for non-isothermal pretreatment with asymmetrictemperature curve was successfully applied as a reaction ordinate to evaluate differentpretreatment conditions. In light of material balance and multiple characterizationmethods, the influence of process parameters including severity facor, solid loadingand pH on the kinetic behaviors of major components in lignocellulose duringhydrothermal pretreatment and these influences on the subsequent bioconversion werestudied. It was found that a trade-off between glucose and xylose yield existed aftereither aqueous/steam pretreatment followed by enzymatic hydrolysis, but this couldbe eliminated by introduction of the third parameter, pH. High yields in glucose(>90%) and xylose (>85%) were simultaneously obtained. Hydrolysis, degradationand condensation reaction involved in xylan chemistry and hydrolysis of lignin werestrongly pH-dependent. Soluble xylo-oligmers in the prehydrolyzate and somedegradation products were verified as the inhibitory compounds to enzymatichydrolysis but behaved in a different way. Furan derivatives and some aromatic aldehydes/ketones/acids were assumed to be key potential fermentation inhibitors.Aqueous pretreatment controlling its pH at a near neutral value showed advantagesover that without pH control. Based upon the quantitative and qualitative informationon destruction of plant cell wall, a clear and systematic picture of mechanisims ofhydrothermal pretreatment was finally provided.
A continuous-effect membrane distillation (CEMD) process was developed byequipping air gap membrane distillation (AGMD)-based and strictly-parallel hollowfiber module with internal heat recovery. Within the studied experimental range, themaximum PR of13.8was obtained. A face-centered central composite experimentaldesign was conducted to investigate the influences of operating variables includingcold-feed temperature, hot-feed temperature, and feed-in flow rate on the performancewhich was indicated by flux, performance ratio and evaporation efficiency. Atheoretical model based on governing transport equations was established to predictthe process performance and the model described the experimental data fairly well. Inlight of model, possible ways to further increase PR were predicted. The diluteaqueous sugar solution was successfully concentrated12-fold to a final concentrationof about20%wt by using CEMD process with a final PR of8.2, and the goal toestablish the high energy-efficiency concentration process was achieved.
引文
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