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板栗壳基5-羟甲基糠醛的快速测定及工艺参数优化

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生物质基5-羟甲基糠醛(5-HMF)作为一种重要平台化学品而受到重点关注。生物质转化体系中检测5-HMF方法主要有高效色谱法、紫外分光光度法等,但色谱法所需样品前处理复杂、设备仪器昂贵,已有文献报道的紫外分光度法需使用冰醋酸等作为稀释溶剂,大大提高了5-HMF的工业检测成本。本文以农业废弃板栗壳为原料来制备5-HMF,建立了一种快捷检测板栗壳提取液中5-HMF的紫外三波长分光光度法,该方法用水替换冰醋酸作为样品稀释溶剂,极大地降低了检测成本。另外,五组加标实验的5-HMF回收率范围为94。4%~105。5%,这表明建立的实验方法具有较好的检测精度。本文还对反应温度、反应时间和固液比等影响板栗壳基5-HMF产率的关键工艺参数进行了优化,实验结果表明最佳反应温度、最佳反应时间和最佳固液比分别为190℃、4 h和1∶20。本文研究结果可为检测板栗壳基5-HMF提供一种廉价快速准确方法,并在一定程度上为农业废弃板栗壳的高值转化制备5-HMF提供指导借鉴。
Rapid Determination and Process Parameter Optimization of 5-hydroxymethylfurfural from Chestnut Shell Biomass
Biomass-based 5-hydroxymethylfurfural(5-HMF)is highlighted as an important platform chemical.The detection of 5-HMF in biomass conversion system mainly includes HPLC,UV spectrophotometry,etc.,but the sample pre-processing required by HPLC is complex,and the equipment is expensive.The UV spectrophotometric method reported in literature requires glacial acetic acid as the dilution solvent,which greatly increases the industrial detection cost of 5-HMF.This work adopts agricultural discarded chestnut shells as raw materials to prepare biomass-based 5-HMF,and establishes a UV three-wavelength spectrophotometric method to quickly detect 5-HMF in extraction solution.This method uses deionized water instead of glacial acetic acid as the sample dilution solvent,greatly reducing the detection cost.In addition,the 5-HMF recovery rates of the five sets of recycling experiments ranged from 94.4%to 105.5%,indicating that the established experimental method has good detection accuracy.The key process parameters such as reaction temperature,reaction time and solid-liquid ratio affect the 5-HMF yield,and the experimental results show that the optimal reaction temperature,optimal reaction time and optimal solid-liquid ratio are 190℃,4 h and 1∶20,respectively.The results of this paper can provide a cheap,fast,and accurate method for the detection of 5-HMF,and provide guidance to some extent for the preparation of 5-HMF by high-value transformation of agricultural discarded chestnut shells.

5-hydroxymethylfurfuraluv spectrumthree-wavelength methodwaterchestnut shell

石桥、罗怡帆、徐乾坤、胡敬民、张钰涵、余子恒、曾裕晨、高宁宁、龚升高

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湖南工学院,湖南 衡阳 421002

5-羟甲基糠醛 紫外光谱 三波长法 板栗壳

2024

广东化工
广东省石油化工研究院

广东化工

影响因子:0.288
ISSN:1007-1865
年,卷(期):2024.51(24)