H_(2)O_(2)+KOH氧解云南褐煤提取黄腐酸实验研究  

Experimental study on extraction of fulvic acid from Yunnan lignite with H_(2)O_(2)+KOH

作　　者：袁申富 原照然 尚睿航 邓晋 杨太 丁锐 马航 王国栋 YUAN Shenfu;YUAN Zhaoran;SHANG Ruihang;DENG Jin;YANG Tai;DING Rui;MA Hang;WANG Guodong(School of Chemical Science and Technology,Yunnan University,Key Laboratory of Medicinal Chemistry for Natural Resource-Ministry of Education,National Demonstration Center for Experimental Chemistry and Chemical Engineering Education(Yunnan University),Kunming 650091,Yunnan,China;Yunnan Yuntianhua Co.,Ltd,Kunming 650100,Yunnan,China)

机构地区：[1]云南大学化学科学与工程学院,自然资源药物化学教育部重点实验室,化学化工国家级实验教学示范中心(云南大学),云南昆明650091 [2]云南云天化股份有限公司,云南昆明650100

出　　处：《云南大学学报（自然科学版）》2024年第4期735-742,共8页Journal of Yunnan University(Natural Sciences Edition)

基　　金：国家自然科学基金(21968037);云南省基础研究项目(202301bf070001-010);国家级大学生创新训练项目(202310673093).

摘　　要：研究采用H_(2)O_(2)与碱液混合氧化法从褐煤中提取黄腐酸(FA),在H_(2)O_(2)的氧解活化作用下探究不同碱液(NaOH、KOH)对FA提取的影响.选用KOH+H_(2)O_(2)对FA进行混合氧化提取,通过滴加消泡剂控制反应速率,同时对提取条件进行优化,在最优条件下(50℃下反应2.5 h)FA产率达40.00%.利用UV、IR、TG对不同条件下提取的FA进行结构分析,对比发现KOH+H_(2)O_(2)氧解法提取的FA具有官能团丰富、相对分子质量小、不饱和度低等特点,对K^(+)和H_(2)O_(2)在提取过程中发挥的作用进行合理推测.利用Py-GC/MS对FA进行裂解,通过裂解产物对FA的结构组成进行分析,认为FA可能由醋酸、3-糠醛等结构构成,还含有直接提取得到的小分子丝氨酸.根据表征结果提出桥键、含氧官能团、不饱和键的氧化反应过程,为褐煤的资源化利用和混合氧解提高FA产率提供借鉴意义.In this study,FA was extracted from lignite of Xianfeng coal mine by mixed oxidation with H_(2)O_(2) and alkali,and the effects of different alkalis(NaOH and KOH)on FA extraction were investigated under the oxygenation activation of H_(2)O_(2).KOH+H_(2)O_(2) was selected for the mixed oxidation and extraction of FA,and the reaction rate was controlled by the addition of antifoam agent dropwise,and the conditions of extraction were optimized,and the FA yield was up to 40.00%under the optimal conditions(2.5 h at 50℃).The structures of FA extracted under different conditions were analysed by UV,IR and TG,and it was found that the FA extracted by KOH+H_(2)O_(2) oxygenation method was rich in functional groups,small molecular weight and low unsaturation,and the roles of K^(+) and H_(2)O_(2) in the extraction process were reasonably speculated.FA was cleaved using Py-GC/MS,and the structural composition of FA was analysed by the cleavage products,which suggested that FA might be composed of structures such as acetic acid and 3 furfural,and also had a small molecule of serine that was directly extracted.Based on the characterisation results,the oxidation reaction process of bridge bonds,oxygen-containing functional groups,and unsaturated bonds was proposed to provide implications for the resourceful utilisation of lignite and the mixed-oxygen cleavage to improve the FA yield.

关 键 词：褐煤 黄腐酸提取 分子结构 提取剂 氧解机理 

分 类 号：TD849.2[矿业工程—煤矿开采]