稻秸秆硝解制备黄腐酸和腐植酸研究  

Preparation of Fulvic Acid and Humic Acid by Nitric Acid Oxidized Rice Straw

作　　者：李斌斌 吴诗勇[1] 吴幼青[1] 黄胜[1] 高晋生[1] LI Binbin;WU Shiyong;WU Youqing;HUANG Sheng;GAO Jinsheng(Department of Chemical Engineering for Energy Resources,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学能源化工系,上海200237

出　　处：《华东理工大学学报（自然科学版）》2021年第2期189-194,共6页Journal of East China University of Science and Technology

基　　金：国家自然科学基金(21878096,2197080732);中央高校基本科研业务费专项资金资助(222201718003);国家重点研发计划(2018YFB0604602)。

摘　　要：研究了稻秸秆硝解制备黄腐酸(FA)和腐植酸(HA)的工艺条件,结果表明增加HNO3质量分数、升高反应温度或延长反应时间均可以提高FA收率,改变液固比(溶液体积与原料质量之比,mL/g)对FA收率影响较小。正交试验得到制备FA的较优条件为:HNO3质量分数5%、温度90℃、液固比13 mL/g,在该条件下反应1 h,FA平均收率为32.63%,HA平均收率为12.77%,n_(C)/n_(O)分别为0.87(FA)和1.93(HA),n_(C)/n_(H)分别为0.78(FA)和0.73(HA),465 nm和665 nm处的吸光度比分别为13.87(FA)和8.47(HA),表明产物具有较高的活性和芳香特征,红外光谱结果也表明产物具有明显的酸性基团和芳香特征。Preparation of fulvic acid(FA)and humic acid(HA)from nitric acid-oxidized rice straw was studied through single factor analysis and orthogonal experiment.The effects of concentration of nitric acid,temperature,time and liquid-solid ratio on the yields of FA and HA were investigated,and optimal process conditions for FA were revealed.The results of single analysis showed that the increases of concentration of HNO_(3)within a certain range,reaction temperature or reaction time could all increase the yield of fulvic acid,the effects of liquid-solid ratio on the yields of FA and HA were not significant.The same conclusion was obtained by the range analysis of the FA yield in the orthogonal experiment.The optimal conditions obtained by the orthogonal experiment were:HNO3 mass fraction 5%,reaction temperature 90℃,liquid-solid ratio 13 mL/g.The average yield of FA of the reaction for 1 h was 32.63%,and the average yield of HA was 12.77%under the optimal condition.Elemental analysis showed that n_(C)/n_(O)of the FA and HA was 0.87 and 1.93,respectively,and n_(C)/n_(H)of the FA and HA was 0.78 and 0.73,respectively,indicating the high biological activity and obvious aroma characteristics of the product.Infrared spectroscopy showed that FA contained obvious aromatic characteristics,acidic groups and nitro groups,suggesting that the oxidation and nitrification of HNO3,and the nitro group of HA was not obvious.The UV-visible spectrum analysis showed that the E465/E665 of the FA and HA was 13.87 and 8.47,respectively,higher than those of FA and HA that were prepared from low rank coal,which further indicated its higher activity.

关 键 词：稻秸秆 硝酸 黄腐酸 腐植酸 

分 类 号：TK6[动力工程及工程热物理—生物能]