稻草酸性水解的实验研究
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摘要
采用生物纤维制备燃料乙醇,是今后能源发展的方向。稻草作为一种植物纤维,是重要的可再生资源,特别是其来源丰富,利用意义重大。人们在制备燃料乙醇时,一般采用的步骤是:预处理、水解和发酵。而实验研究的是制备燃料乙醇的前两个步骤:预处理和水解。木质纤维素类原料的水解,是其生物质转化为燃料乙醇的首要步骤。
以稻草秸杆为原料,对稻草进行两步酸水解实验。实验中,采用的无机酸是硫酸,利用单因素实验和正交实验相结合的实验方法确定出了最佳的水解工艺条件。
稻草的两步酸水解实验中,探讨了浓硫酸低温水解中的硫酸浓度(50%,60%,70%,75%,80%)、料液比(1∶4,1∶6,1∶8,1∶10,1∶12)、反应温度(25℃,30℃,35℃,40℃,45℃)、反应时间(1.0h,1.5h,2.0h,2.5h,3.0h);稀硫酸高温水解中的硫酸浓度(3%,4%,5%……21%)和反应时间(0.5h,1.0h,1.5h……5.0h)对水解实验(即还原糖得率)的影响。
在单因素实验的基础上,又采用六因素三水平L_(18)(3~6)的正交实验来优化水解条件,以还原糖得率为考察指标,对实验结果进行方差分析,得出:影响稻草两步酸水解的主要因素是浓硫酸水解的硫酸浓度、稀硫酸水解的硫酸浓度和料液比,而稀硫酸水解的反应时间对还原糖得率影响较小。
最后得出两步酸水解的最佳工艺条件是:浓硫酸水解的料液比1∶4,浓硫酸水解的硫酸浓度70%,浓硫酸水解的反应温度30℃,浓硫酸水解的时间2.0h,稀硫酸水解的硫酸浓度9%,稀硫酸水解的时间2.5h,还原糖得率达50%,还原糖浓度达5.18g/L。
采用热分析法和红外光谱法对水解产物进行初步成分分析。
Using biological fiber to produce biofuel is the direction of energy development in the future.As a plant fiber,rice straw is an abundant renewable resource,and has special significance of utilization.The steps of the production of fuel ethanol in general are pretreatment,hydrolysis and fermentation.This experiment studied on the first two steps of the production of fuel ethanol:pretreatment and hydrolysis.The hydrolysis of lignocellulose is the primary step for the bio-transformation fuel ethanol of it.
In this research,rice straw is the raw material,and two stages of acidic hydrolysis craft were carried on.The acid using in the experiment was sulfuric acid.The method of single factor experiments and orthogonal experiments were utilized to study the optimal hydrolysis conditons.
The two stages of acidic hydrolysis craft were studied.The influence factors to the yield of reducing sugar include the concentration of concentrated sulfuric acid (50%,60%,70%,75%,80%),the ratio of material and liquid(1:4,1:6,1:8,1:10, 1:12),hydrolysis temperature(25℃,30℃,35℃,40℃,45℃) and hydrolysis time (1.0 h,1.5 h,2.0 h,2.5 h,3.0 h) in concentrated sulfuric acid hydrolysis at low temperature;the concentration of dilute sulfuric acid(3%,4%,5%……21%) and hydrolysis time(0.5 h,1.0 h,1.5 h……5.0 h) in the dilute sulfuric acid hydrolysis at high temperature.
Utilizing the results of the single factor experiment,six factors and three levels orthogonal experiment L_(18)(3~6) was designed to optimize the hydrolysis conditions. The yield of reducing sugar is the target,and the variance of the experimental results are analysed.Known from the experimental results,the concentration of sulfuric acid, the ratio of material and liquid were the main factors among them.However, hydrolysis time in the dilute acid hydrolysis is the least factor.
The optimized hydrolysis conditions are that the ratio of material and liquid is 1:4,the concentration of sulfuric acid is 70%,hydrolysis temperature is 30℃and hydrolysis time is 2.0 h in the concentrated acid hydrolysis;The concentration of sulfuric acid is 9%,and hydrolysis time is 2.5 h in the dilute acid hydrolysis.The yield of reducing sugar is about 50%under this condition,and the concentration of reducing sugar is 5.18 g/L.
Thermal analysis(TA) and Infrared spectrum(IR spectrum) were used to analyse the preliminary components of the hydrolyzate in this experiment.
以稻草秸杆为原料,对稻草进行两步酸水解实验。实验中,采用的无机酸是硫酸,利用单因素实验和正交实验相结合的实验方法确定出了最佳的水解工艺条件。
稻草的两步酸水解实验中,探讨了浓硫酸低温水解中的硫酸浓度(50%,60%,70%,75%,80%)、料液比(1∶4,1∶6,1∶8,1∶10,1∶12)、反应温度(25℃,30℃,35℃,40℃,45℃)、反应时间(1.0h,1.5h,2.0h,2.5h,3.0h);稀硫酸高温水解中的硫酸浓度(3%,4%,5%……21%)和反应时间(0.5h,1.0h,1.5h……5.0h)对水解实验(即还原糖得率)的影响。
在单因素实验的基础上,又采用六因素三水平L_(18)(3~6)的正交实验来优化水解条件,以还原糖得率为考察指标,对实验结果进行方差分析,得出:影响稻草两步酸水解的主要因素是浓硫酸水解的硫酸浓度、稀硫酸水解的硫酸浓度和料液比,而稀硫酸水解的反应时间对还原糖得率影响较小。
最后得出两步酸水解的最佳工艺条件是:浓硫酸水解的料液比1∶4,浓硫酸水解的硫酸浓度70%,浓硫酸水解的反应温度30℃,浓硫酸水解的时间2.0h,稀硫酸水解的硫酸浓度9%,稀硫酸水解的时间2.5h,还原糖得率达50%,还原糖浓度达5.18g/L。
采用热分析法和红外光谱法对水解产物进行初步成分分析。
Using biological fiber to produce biofuel is the direction of energy development in the future.As a plant fiber,rice straw is an abundant renewable resource,and has special significance of utilization.The steps of the production of fuel ethanol in general are pretreatment,hydrolysis and fermentation.This experiment studied on the first two steps of the production of fuel ethanol:pretreatment and hydrolysis.The hydrolysis of lignocellulose is the primary step for the bio-transformation fuel ethanol of it.
In this research,rice straw is the raw material,and two stages of acidic hydrolysis craft were carried on.The acid using in the experiment was sulfuric acid.The method of single factor experiments and orthogonal experiments were utilized to study the optimal hydrolysis conditons.
The two stages of acidic hydrolysis craft were studied.The influence factors to the yield of reducing sugar include the concentration of concentrated sulfuric acid (50%,60%,70%,75%,80%),the ratio of material and liquid(1:4,1:6,1:8,1:10, 1:12),hydrolysis temperature(25℃,30℃,35℃,40℃,45℃) and hydrolysis time (1.0 h,1.5 h,2.0 h,2.5 h,3.0 h) in concentrated sulfuric acid hydrolysis at low temperature;the concentration of dilute sulfuric acid(3%,4%,5%……21%) and hydrolysis time(0.5 h,1.0 h,1.5 h……5.0 h) in the dilute sulfuric acid hydrolysis at high temperature.
Utilizing the results of the single factor experiment,six factors and three levels orthogonal experiment L_(18)(3~6) was designed to optimize the hydrolysis conditions. The yield of reducing sugar is the target,and the variance of the experimental results are analysed.Known from the experimental results,the concentration of sulfuric acid, the ratio of material and liquid were the main factors among them.However, hydrolysis time in the dilute acid hydrolysis is the least factor.
The optimized hydrolysis conditions are that the ratio of material and liquid is 1:4,the concentration of sulfuric acid is 70%,hydrolysis temperature is 30℃and hydrolysis time is 2.0 h in the concentrated acid hydrolysis;The concentration of sulfuric acid is 9%,and hydrolysis time is 2.5 h in the dilute acid hydrolysis.The yield of reducing sugar is about 50%under this condition,and the concentration of reducing sugar is 5.18 g/L.
Thermal analysis(TA) and Infrared spectrum(IR spectrum) were used to analyse the preliminary components of the hydrolyzate in this experiment.
引文
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2.夏黎明.可再生纤维素资源酶法降解的研究进展[J],林产化工通讯,1999,33(1):23-28.
3.陈洪章.纤维素生物技术[M],北京:化学工业出版社,2005,1-2.
4.姜锋,马丁,包信和.酸性离子液中纤维素的水解[J],催化学报,2009,30(4):279-283
5.肖军.生物质利用现状[J],安全与环境工程,2003,10(1):11-14.
6.但卫华.生物质与生物质工程[J],中国皮革,2002,31(11):31-35.
7.孔宪文,李丽萍.发展生物质能可获得多方面的效益[J],节能,2003,(2):45-47.
8.高荫榆,雷占兰,郭磊,等.生物质能转化利用技术及其研究进展[J],江西科学,2006,24(6):529-533.
9.董玉平,王里鹏,邓波,等.国内外生物质能源开发利用技术[J],山东大学学报(工学版),2007,37(3):64-68.
10.张继泉,王瑞明,关凤梅,等.玉米秸秆同时糖化发酵生产燃料酒精的研究[J],纤维素科学与技术,2002,10(3):35-39.
11.张继泉,孙玉英,关凤梅,等.玉米秸秆稀硫酸预处理条件的初步研究[J],纤维素科学与技术,2002,10(2):32-36.
12.杨斌,高孔荣.甘蔗渣的糖化及转化为酒精的研究概况[J],食品与发酵工业,1995,(6):61-65.
13.安宏.纤维素稀酸水解制取燃料酒精的试验研究[D],杭州:浙江大学,2005.
14.Nagel J.Biomass in energy supply,especially in the state of Brandenburg,Germany[J],Ecological Engineering,2000,16(1):103-110.
15.Mckendry P.Energy production from biomass(part 1):overview of biomass[J],Bioresource Technology,2002,83(1):37-46.
16.Maniatis K,Millich E.Energy from biomass and waste:the contribution of utility scale biomass gasification plants[J],Biomass and Bioenergy,1998,15(3):195-200.
17.辛欣.生物质能--未来全球能源的新亮点[J],节能与环保,2005,(10):15-17.
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