玉米秆活性氧蒸煮过程中半纤维素的结构变化及其机理的研究
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摘要
我国是一个农业大国，每年会产生大量的农业秸秆，但是大部分都被直接回填到田中或者在田间烧掉，只有少部分被用做饲料喂养牲畜和作为造纸原料。而随着化石能源储量的逐步减少以及人们对化石能源燃烧后产生的有害气体对环境造成的危害的认识，同时为了找到一种替代化石能源的清洁、可再生的能源，很多的研究将注意力集中到了可再生的生物质上。木质纤维素生物质的利用可以分为直接转化和间接转化。在直接转化的过程中木质纤维生物质不经过分离、全组分转化为工业产品，比如通过热解，气化、液化将生物质转化为燃料，生物油等。如果想从生物质中得到高附加值的化学品就有必要在转化之前对其进行预处理，将其分离成为纤维素、半纤维素和木素。预处理使得生物质的利用率大大提高，而且更利于后期的分离和纯化。因此生物质的高效、清洁预处理成为生物质炼制的第一个要解决的难题。对此我们提出了一个新型的生物质预处理工艺——活性氧蒸煮工艺。本文用玉米秆作为原料，用活性氧(氧气和过氧化氢)作为化学品对玉米秆进行处理，探讨了这个过程中半纤维素结构的变化和活性氧在蒸煮过程中作用的机理。
首先在最优的蒸煮条件下(温度：165°C；氧气压力：1.0MPa；过氧化氢用量：3%（基于绝干原料）；液比：1:6；MgO用量：15%(基于绝干原料))对玉米秆进行蒸煮，通过分离原料、浆和黄液中的半纤维素，用各种分析手段表征了半纤维素的结构变化，发现玉米秆的半纤维素结构是聚阿拉伯糖木糖，此外还有一些乙酰基和葡萄糖醛酸。半纤维素的糖苷键在蒸煮过程中被严重破坏，乙酰基也在蒸煮过程中发生了水解。
为了更好了理解半纤维素在蒸煮黄液中的分布情况，用1，2，3，5和7体积的乙醇分级沉淀了黄液中的半纤维素。通过分析发现用1体积乙醇沉淀出的占总量5.3%的半纤维素分子量是24824g/mol，两体积乙醇沉淀出来的占总量15.63%半纤维素的分子量仅为4574g/mol，剩下的半纤维素的分子量都在2500g/mol左右。而且随着乙醇浓度的增加，分离出来的半纤维素组分所含的杂质越来越多。在最终的残液中还有29.61%的固形物，主要是一些木素的降解产物。
在研究活性氧蒸煮工艺中各个主要的化学品对于蒸煮过程中的影响中，我们设计了不同的活性氧蒸煮工艺。通过比较发现足量的MgO能够防止碳水化合物的降解，此外Mg(OH)_2能够起到与MgO相同的作用，可以取代MgO，而用NaOH替代MgO，虽然能取得比较好的蒸煮效果，但是纤维素发生了严重降解。从蒸煮效果上来看，在活性氧蒸煮过程中，氧气是主要脱木素和半纤维素的试剂，过氧化氢对于木素的脱除能起到一定的作用，但是过氧化氢与氧气同时添加时，过氧化氢的脱木素效果可以被忽略。在蒸煮过程中将支链比较多的半纤维素溶出，而将支链比较少的半纤维素留在浆中。
在研究半纤维素在不同保温时间下的脱除效果中发现蒸煮过程中半纤维素和木素的溶出主要在蒸煮的升温阶段和蒸煮保温半小时的这个时间段中，其溶出率分别达到67.87%和75.6%，而在剩下的保温时间中，半纤维素和木素的脱除很少，这个过程主要是纤维发生纤维化的过程。半纤维的分子量随着蒸煮时间的延长从保温时的19643g/mol下降到了蒸煮结束时的5471g/mol，半纤维素被溶解在黄液中之后糖苷键被严重破坏。此外蒸煮过程中也会有己烯糖醛酸的产生。
通过前面的分析对活性氧蒸煮过程中半纤维素的溶出和结构的变化提出一些可能的机理。MgO在蒸煮液中的碱性和Mg~(2+)的保护作用是分子氧能够用作蒸煮的首要条件。蒸煮过程中热水抽提和MgO的碱性对半纤维素的水解是半纤维素溶出的主要途径，氧气对木素的溶出也能加速半纤维素的溶出，此外半纤维素的主链还会发生碱性降解使半纤维素的分子量降低而且还会生成一些低分子物质。
China is an agricultural country and lots of agricultural straws are produced per year.Most of them are backfilled to the field and burnt in the field, while small part is used for thefeed and raw material of pulp. With the decrease of fossil energy reserve and enhancement ofenvironmental protection consciousness, many research focus on the renewable biomass tofind an alternative energy resources for the fossil energy. Generally speaking, there are twoways to utilize the lignocellulosic biomass: direct conversion and indirect conversion. Thelignocellulosic biomass can be converted into fuels, bio-oil by pyrolysis, gasification, andliquidation in the direct conversion process. If want to get the high-value-added chemicalsfrom the biomass, it is necessary to pretreat the biomass into hemicelluloses, cellulose, andlignin before carry through the conversion. Pretreatment can increase the percent conversionof reactant, and is in favor of the isolation and purification of products. Therefore, it is a keyquestion to find an efficient and clean pretreatment process for the biorefinery. And our groupdeveloped a novel biomass pretreatment process, active oxygen cooking process. In thepresent study, corn stalk is treated by the active oxygen, and the structural changes and themechanism of corn stalk hemicelluloses during the active oxygen cooking process are studied.
The active oxygen cooking process of corn stalk was performed on the optimumconditions, temperature165°C, initial oxygen pressure1.0MPa, peroxide dosage3%(basedon the oven dry raw material), ratio of solid to liquid1:6, MgO dosage15%(based on theoven dry raw material). Isolation and characterization the hemicelluloses from the rawmaterial, pulp, and yellow liquor showed that the structure of corn hemicelluloses wereL-arabino-D-xylan, and the4-O-methyl-glucuronic acids and acetyl groups also attached tothe backbone of hemicellulose and the glycosidic bonds were broken during cooking process,and the acetyl groups were also hydrolyzed.
For further understand the hemicelluloses in the yellow liquor, the hemicelluloses weresequentially precipitated with one, two, three, five, and seven volume of ethanol. The resultsshowed that the weight-average molecular weight (MW) of hemicelluloses precipitated by onevolume of ethanol was24824g/mol, but it accounted for5.31%of total hemicelluloses. Andthe MWof hemicelluloses precipitated with two volume ethanol was only4574g/mol, the rest of hemicelluloses fractions presented low-molecular-weight (c.a.2500g/mol). With increaseof the volume of ethanol, the impurities in the hemicelluloses fractions increased. In the finalresidue, there was29.61%solid content, which mainly composed of degradation products oflignin.
To study the effects of chemicals added in the cooking process, several cookingprocesses were designed. After cooking, it found that enough dosage MgO can preventcarbonizing of raw material during the active oxygen cooking process, and Mg(OH)_2showedthe some protective effect to the raw material and can replace MgO. However, the cellulosewas seriously degraded when MgO was replaced by NaOH in the active oxygen cookingprocess, even show good cooking effect. In this study, we also found that the oxygen played aleading role in the cooking process to remove the lignin and hemicelluloses, the effect ofperoxide can be ignored when both oxygen and peroxide were added. The structure ofhemicelluloses obtained from cooking liquor indicated that the hemicelluloses removedduring the cooking process possessed more side chains than that in the pulp.
In the study of effect of incubation time on the cooking effect, it found that67.86%hemicelluloses and75.60%lignin were removed from the raw material after get the desiredtemperature half an hour. In the rest of incubation time, the removal ratio of lignin andhemicelluloses was very low. The MWof hemicelluloses decreased from19643g/mol to5471g/mol due to the break of glycosidic bonds during the cooking process. And the HexA alsowas detected in pulp.
Based on the analysis of structural changes of hemicelluloses, some mechanisms abouthemicellulosic remove and structural changes were presented. The alkalinity of MgO in thecooking liquor and protective function of Mg~(2+)were first condition of active oxygen appliedin the cooking process. Hot-water extraction and basic hydrolysis were the primarily route ofremoving hemicelluloses, and the remove of lignin also can accelerated the remove ofhemicelluloses. Moreover, alkaline degradation of hemicelluloses backbone also caused theglycosidic bounds break and produced some low molecular substances.
首先在最优的蒸煮条件下(温度：165°C；氧气压力：1.0MPa；过氧化氢用量：3%（基于绝干原料）；液比：1:6；MgO用量：15%(基于绝干原料))对玉米秆进行蒸煮，通过分离原料、浆和黄液中的半纤维素，用各种分析手段表征了半纤维素的结构变化，发现玉米秆的半纤维素结构是聚阿拉伯糖木糖，此外还有一些乙酰基和葡萄糖醛酸。半纤维素的糖苷键在蒸煮过程中被严重破坏，乙酰基也在蒸煮过程中发生了水解。
为了更好了理解半纤维素在蒸煮黄液中的分布情况，用1，2，3，5和7体积的乙醇分级沉淀了黄液中的半纤维素。通过分析发现用1体积乙醇沉淀出的占总量5.3%的半纤维素分子量是24824g/mol，两体积乙醇沉淀出来的占总量15.63%半纤维素的分子量仅为4574g/mol，剩下的半纤维素的分子量都在2500g/mol左右。而且随着乙醇浓度的增加，分离出来的半纤维素组分所含的杂质越来越多。在最终的残液中还有29.61%的固形物，主要是一些木素的降解产物。
在研究活性氧蒸煮工艺中各个主要的化学品对于蒸煮过程中的影响中，我们设计了不同的活性氧蒸煮工艺。通过比较发现足量的MgO能够防止碳水化合物的降解，此外Mg(OH)_2能够起到与MgO相同的作用，可以取代MgO，而用NaOH替代MgO，虽然能取得比较好的蒸煮效果，但是纤维素发生了严重降解。从蒸煮效果上来看，在活性氧蒸煮过程中，氧气是主要脱木素和半纤维素的试剂，过氧化氢对于木素的脱除能起到一定的作用，但是过氧化氢与氧气同时添加时，过氧化氢的脱木素效果可以被忽略。在蒸煮过程中将支链比较多的半纤维素溶出，而将支链比较少的半纤维素留在浆中。
在研究半纤维素在不同保温时间下的脱除效果中发现蒸煮过程中半纤维素和木素的溶出主要在蒸煮的升温阶段和蒸煮保温半小时的这个时间段中，其溶出率分别达到67.87%和75.6%，而在剩下的保温时间中，半纤维素和木素的脱除很少，这个过程主要是纤维发生纤维化的过程。半纤维的分子量随着蒸煮时间的延长从保温时的19643g/mol下降到了蒸煮结束时的5471g/mol，半纤维素被溶解在黄液中之后糖苷键被严重破坏。此外蒸煮过程中也会有己烯糖醛酸的产生。
通过前面的分析对活性氧蒸煮过程中半纤维素的溶出和结构的变化提出一些可能的机理。MgO在蒸煮液中的碱性和Mg~(2+)的保护作用是分子氧能够用作蒸煮的首要条件。蒸煮过程中热水抽提和MgO的碱性对半纤维素的水解是半纤维素溶出的主要途径，氧气对木素的溶出也能加速半纤维素的溶出，此外半纤维素的主链还会发生碱性降解使半纤维素的分子量降低而且还会生成一些低分子物质。
China is an agricultural country and lots of agricultural straws are produced per year.Most of them are backfilled to the field and burnt in the field, while small part is used for thefeed and raw material of pulp. With the decrease of fossil energy reserve and enhancement ofenvironmental protection consciousness, many research focus on the renewable biomass tofind an alternative energy resources for the fossil energy. Generally speaking, there are twoways to utilize the lignocellulosic biomass: direct conversion and indirect conversion. Thelignocellulosic biomass can be converted into fuels, bio-oil by pyrolysis, gasification, andliquidation in the direct conversion process. If want to get the high-value-added chemicalsfrom the biomass, it is necessary to pretreat the biomass into hemicelluloses, cellulose, andlignin before carry through the conversion. Pretreatment can increase the percent conversionof reactant, and is in favor of the isolation and purification of products. Therefore, it is a keyquestion to find an efficient and clean pretreatment process for the biorefinery. And our groupdeveloped a novel biomass pretreatment process, active oxygen cooking process. In thepresent study, corn stalk is treated by the active oxygen, and the structural changes and themechanism of corn stalk hemicelluloses during the active oxygen cooking process are studied.
The active oxygen cooking process of corn stalk was performed on the optimumconditions, temperature165°C, initial oxygen pressure1.0MPa, peroxide dosage3%(basedon the oven dry raw material), ratio of solid to liquid1:6, MgO dosage15%(based on theoven dry raw material). Isolation and characterization the hemicelluloses from the rawmaterial, pulp, and yellow liquor showed that the structure of corn hemicelluloses wereL-arabino-D-xylan, and the4-O-methyl-glucuronic acids and acetyl groups also attached tothe backbone of hemicellulose and the glycosidic bonds were broken during cooking process,and the acetyl groups were also hydrolyzed.
For further understand the hemicelluloses in the yellow liquor, the hemicelluloses weresequentially precipitated with one, two, three, five, and seven volume of ethanol. The resultsshowed that the weight-average molecular weight (MW) of hemicelluloses precipitated by onevolume of ethanol was24824g/mol, but it accounted for5.31%of total hemicelluloses. Andthe MWof hemicelluloses precipitated with two volume ethanol was only4574g/mol, the rest of hemicelluloses fractions presented low-molecular-weight (c.a.2500g/mol). With increaseof the volume of ethanol, the impurities in the hemicelluloses fractions increased. In the finalresidue, there was29.61%solid content, which mainly composed of degradation products oflignin.
To study the effects of chemicals added in the cooking process, several cookingprocesses were designed. After cooking, it found that enough dosage MgO can preventcarbonizing of raw material during the active oxygen cooking process, and Mg(OH)_2showedthe some protective effect to the raw material and can replace MgO. However, the cellulosewas seriously degraded when MgO was replaced by NaOH in the active oxygen cookingprocess, even show good cooking effect. In this study, we also found that the oxygen played aleading role in the cooking process to remove the lignin and hemicelluloses, the effect ofperoxide can be ignored when both oxygen and peroxide were added. The structure ofhemicelluloses obtained from cooking liquor indicated that the hemicelluloses removedduring the cooking process possessed more side chains than that in the pulp.
In the study of effect of incubation time on the cooking effect, it found that67.86%hemicelluloses and75.60%lignin were removed from the raw material after get the desiredtemperature half an hour. In the rest of incubation time, the removal ratio of lignin andhemicelluloses was very low. The MWof hemicelluloses decreased from19643g/mol to5471g/mol due to the break of glycosidic bonds during the cooking process. And the HexA alsowas detected in pulp.
Based on the analysis of structural changes of hemicelluloses, some mechanisms abouthemicellulosic remove and structural changes were presented. The alkalinity of MgO in thecooking liquor and protective function of Mg~(2+)were first condition of active oxygen appliedin the cooking process. Hot-water extraction and basic hydrolysis were the primarily route ofremoving hemicelluloses, and the remove of lignin also can accelerated the remove ofhemicelluloses. Moreover, alkaline degradation of hemicelluloses backbone also caused theglycosidic bounds break and produced some low molecular substances.
引文
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