微波辅助下木质纤维素降解与溶解过程的研究
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摘要
木质纤维素主要是由纤维素、半纤维素和木质素构成的，作为人类可利用的最丰富的天然可再生资源，木质纤维素中的半纤维素、纤维素经水解后，分别可以获得以木糖为主的五碳糖及以葡萄糖为主的六碳糖。玉米秸秆中纤维素含量约为30%，半纤维素含量约为17%，木质素含量约为17%，经过降解可以将生物质转化为还原糖，利用水解生成的糖进一步发酵可以制取酒精、糠醛等高附加值的化工原料。本文重点讨论了不同降解方法对纯纤维素和玉米秸秆降解、溶解过程的影响，得出如下结论：
首先，探讨了盐酸/H2O2催化下，常规加热与微波加热条件下纯纤维素降解过程的规律。通过单因素实验，确定了微波-盐酸/H2O2耦合条件下，催化降解纯纤维素最佳工艺条件为：催化剂体积分数为5.0％，纯纤维素质量与水溶液体积比为300mg：100ml水溶液，搅拌速度200r/min，反应温度100℃，反应时间2.0h，还原糖得量为2.15mg/ml。利用IR、SEM对纯纤维素降解后的固体剩余物进行了分析，IR分析结果表明，微波加热与常规加热下固体降解剩余物的结构相似；而SEM分析表明：微波加热较常规加热更大程度地促进纤维素中的糖苷键断裂，因而提高了还原糖的产量。
其次，探讨了微波加热下，磷钨杂多酸为催化剂，玉米秸秆的降解过程。通过单因素实验，确定了最适宜的反应条件为：玉米秸秆质量：杂多酸质量：水溶液体积为5.0g:1.0g:200ml，反应温度90℃，反应时间50min，此条件下，玉米秸秆的降解率为46.5%。
第三，研究了常规加热下，离子液体（1-丁基-3甲基咪唑氯盐）在酸性（盐酸）条件下，玉米秸秆的降解过程。通过单因素实验、正交试验及SAS软件对数据进行优化和回归，确定了该体系下玉米秸秆降解的适宜工艺条件为：玉米秸秆质量与离子溶液体积比5.0g:100ml，催化剂体积分数为7.4%，反应温度为85℃，反应时间2.5h,玉米秸秆的降解率为65.8%，比水溶液体系下的玉米秸秆降解率提高了48.7%。
最后，探讨了玉米秸秆在两种碱性体系下的溶解过程及规律：（1）微波加热条件下，6%NaOH/4%Urea/90%水体系下，玉米秸秆溶解的最适宜参数：液固比25ml：1.0g，溶解时间1.0h，溶解温度60℃，玉米秸秆溶解率为48.6%。在常规加热条件下，玉米秸秆溶解最适宜参数：液固比25ml：1.0g，溶解时间6.0h，溶解温度60℃，溶解率为46.7%，并且通过对玉米秸秆溶解后的固体剩余物进行IR和SEM分析，发现微波体系和常规加热体系下，固体降解剩余物的结构相似，玉米秸秆在微波加热体系下的溶解情况优于常规加热体系下的溶解情况。
（2）确定了常规加热条件下，6%NaOH/5%Thiourea/89%水体系下，玉米秸秆溶解的最适宜参数：液固比35ml：1.0g，溶解时间9.0h，溶解温度50℃，玉米秸秆的溶解率为54.4%。微波加热下，液固比35ml：1.0g，溶解时间1.0h，溶解温度50℃时，得到玉米秸秆的溶解率为48.0%。通过玉米秸秆溶解后的固体剩余物的IR和SEM分析表明，玉米秸秆在微波加热下的溶解性比常规加热下的溶解性好。
Ligno cellulose contains cellulose, hemi-cellulose,and lignin.Cellulose is the most abundant and renewable biomass in the biosphere. There is about30%cellulose, about17%hemi-cellulose, and about17%lignin in maize straw. Cellulose can be converted to glucose,and hemi-cellulose can be converted to glucose xylose.By degradation these reducing sugars further can be converted ethanol and other more valuable chemical materials.
This article has firstly discussed the influence of the conventional heating and the microwave heating on the degradation of pure cellulose under catalysis HC1/H2O2. By single-factor experiments, the optimal degradation condition were received as follows: HCl/H2O2concentration5.0%, the ratio of solid to solvent300mg:100ml, stirring speed200r/min, reaction temperature100℃and reaction time2.Oh, The yield of reducing sugars is2.15mg/ml. IR and SEM analysis of the solid remains after pure cellulose degradation displays that there is not seriously destruction of the molecular structure of cellulose under microwave heating. SEM indicates microwave heating can help to enhance the scission of the chain of cellulose.therefore,more reducing sugars is obtained.
Secondly,the lignocellulose degradation with H3PW12O40as catalyst under conventional heating and microwave heating have been conducted. By single-factor experiments, the optimal conditions has been found as following:mass of Maize straw:mass of heteroploly-acid:volume of aqueous solution is5.0g:1.0g:200ml,reaction temperature90℃and reaction time50min.The degradation yield is46.5%.
Third, maize straw degradation by conventional heating in ionic liquid have been conducted. By single-factor experiment and orthogonal experimental design,the optimal conditions were obtained as follows:the ratio of solid to solvent5.Og:100ml, catalyst concentration7.4%, solvent pH of4.8, reaction temperature85℃and reaction time2.5h, The degradation yield is68.5%.
Last, maize straw dissolution in two alkaline liquid systems have been conducted. Maize straw dissolution in NaOH-urea solution system was studied by conventional heating and microwave heating. A series of experiments on maize straw dissolution by microwave heating were finished and the following were the optimal conditions:the ratio of solid to solvent1.0g:25ml, dissolution temperature60℃and dissolution time1.0h.The dissolution yield of maize straw is48.6%. Under conventional heating, the optimal conditions were obtained as follows:the ratio of solid to solvent1.0g:25ml, dissolution temperature60℃and dissolution time6.Oh.The dissolution yield of maize straw is46.7%. IR and SEM analysis of the solid remains after dissolution displays that crystalline region of cellulose in maize straw by microwave heating is less than that by conventional heating, Therefore,the dissolution effect by microwave heating is better than that by conventional heating.
Maize straw dissolution in NaOH-Thiourea solution system was also studied by conventional heating. the following were the optimal conditions:the ratio of solid to solvent1.0g:35ml, dissolution temperature50℃and dissolution time9.Oh.The dissolution yield is54.4%.
Under microwave heating, the optimal conditions were obtained, dissolution time1.0h.The dissolution yield of maize straw is48.0%. The solid remains of maize straw dissolution in these two systems have been identified by IR and SEM analysis.The dissolution effect by conventional heating is better than that by microwave heating.
首先，探讨了盐酸/H2O2催化下，常规加热与微波加热条件下纯纤维素降解过程的规律。通过单因素实验，确定了微波-盐酸/H2O2耦合条件下，催化降解纯纤维素最佳工艺条件为：催化剂体积分数为5.0％，纯纤维素质量与水溶液体积比为300mg：100ml水溶液，搅拌速度200r/min，反应温度100℃，反应时间2.0h，还原糖得量为2.15mg/ml。利用IR、SEM对纯纤维素降解后的固体剩余物进行了分析，IR分析结果表明，微波加热与常规加热下固体降解剩余物的结构相似；而SEM分析表明：微波加热较常规加热更大程度地促进纤维素中的糖苷键断裂，因而提高了还原糖的产量。
其次，探讨了微波加热下，磷钨杂多酸为催化剂，玉米秸秆的降解过程。通过单因素实验，确定了最适宜的反应条件为：玉米秸秆质量：杂多酸质量：水溶液体积为5.0g:1.0g:200ml，反应温度90℃，反应时间50min，此条件下，玉米秸秆的降解率为46.5%。
第三，研究了常规加热下，离子液体（1-丁基-3甲基咪唑氯盐）在酸性（盐酸）条件下，玉米秸秆的降解过程。通过单因素实验、正交试验及SAS软件对数据进行优化和回归，确定了该体系下玉米秸秆降解的适宜工艺条件为：玉米秸秆质量与离子溶液体积比5.0g:100ml，催化剂体积分数为7.4%，反应温度为85℃，反应时间2.5h,玉米秸秆的降解率为65.8%，比水溶液体系下的玉米秸秆降解率提高了48.7%。
最后，探讨了玉米秸秆在两种碱性体系下的溶解过程及规律：（1）微波加热条件下，6%NaOH/4%Urea/90%水体系下，玉米秸秆溶解的最适宜参数：液固比25ml：1.0g，溶解时间1.0h，溶解温度60℃，玉米秸秆溶解率为48.6%。在常规加热条件下，玉米秸秆溶解最适宜参数：液固比25ml：1.0g，溶解时间6.0h，溶解温度60℃，溶解率为46.7%，并且通过对玉米秸秆溶解后的固体剩余物进行IR和SEM分析，发现微波体系和常规加热体系下，固体降解剩余物的结构相似，玉米秸秆在微波加热体系下的溶解情况优于常规加热体系下的溶解情况。
（2）确定了常规加热条件下，6%NaOH/5%Thiourea/89%水体系下，玉米秸秆溶解的最适宜参数：液固比35ml：1.0g，溶解时间9.0h，溶解温度50℃，玉米秸秆的溶解率为54.4%。微波加热下，液固比35ml：1.0g，溶解时间1.0h，溶解温度50℃时，得到玉米秸秆的溶解率为48.0%。通过玉米秸秆溶解后的固体剩余物的IR和SEM分析表明，玉米秸秆在微波加热下的溶解性比常规加热下的溶解性好。
Ligno cellulose contains cellulose, hemi-cellulose,and lignin.Cellulose is the most abundant and renewable biomass in the biosphere. There is about30%cellulose, about17%hemi-cellulose, and about17%lignin in maize straw. Cellulose can be converted to glucose,and hemi-cellulose can be converted to glucose xylose.By degradation these reducing sugars further can be converted ethanol and other more valuable chemical materials.
This article has firstly discussed the influence of the conventional heating and the microwave heating on the degradation of pure cellulose under catalysis HC1/H2O2. By single-factor experiments, the optimal degradation condition were received as follows: HCl/H2O2concentration5.0%, the ratio of solid to solvent300mg:100ml, stirring speed200r/min, reaction temperature100℃and reaction time2.Oh, The yield of reducing sugars is2.15mg/ml. IR and SEM analysis of the solid remains after pure cellulose degradation displays that there is not seriously destruction of the molecular structure of cellulose under microwave heating. SEM indicates microwave heating can help to enhance the scission of the chain of cellulose.therefore,more reducing sugars is obtained.
Secondly,the lignocellulose degradation with H3PW12O40as catalyst under conventional heating and microwave heating have been conducted. By single-factor experiments, the optimal conditions has been found as following:mass of Maize straw:mass of heteroploly-acid:volume of aqueous solution is5.0g:1.0g:200ml,reaction temperature90℃and reaction time50min.The degradation yield is46.5%.
Third, maize straw degradation by conventional heating in ionic liquid have been conducted. By single-factor experiment and orthogonal experimental design,the optimal conditions were obtained as follows:the ratio of solid to solvent5.Og:100ml, catalyst concentration7.4%, solvent pH of4.8, reaction temperature85℃and reaction time2.5h, The degradation yield is68.5%.
Last, maize straw dissolution in two alkaline liquid systems have been conducted. Maize straw dissolution in NaOH-urea solution system was studied by conventional heating and microwave heating. A series of experiments on maize straw dissolution by microwave heating were finished and the following were the optimal conditions:the ratio of solid to solvent1.0g:25ml, dissolution temperature60℃and dissolution time1.0h.The dissolution yield of maize straw is48.6%. Under conventional heating, the optimal conditions were obtained as follows:the ratio of solid to solvent1.0g:25ml, dissolution temperature60℃and dissolution time6.Oh.The dissolution yield of maize straw is46.7%. IR and SEM analysis of the solid remains after dissolution displays that crystalline region of cellulose in maize straw by microwave heating is less than that by conventional heating, Therefore,the dissolution effect by microwave heating is better than that by conventional heating.
Maize straw dissolution in NaOH-Thiourea solution system was also studied by conventional heating. the following were the optimal conditions:the ratio of solid to solvent1.0g:35ml, dissolution temperature50℃and dissolution time9.Oh.The dissolution yield is54.4%.
Under microwave heating, the optimal conditions were obtained, dissolution time1.0h.The dissolution yield of maize straw is48.0%. The solid remains of maize straw dissolution in these two systems have been identified by IR and SEM analysis.The dissolution effect by conventional heating is better than that by microwave heating.
引文
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