废弃液晶面板偏光膜中磷系阻燃剂的微波萃取及气相色谱-质谱法测定  

Microwave Extraction of Phosphorus-based Flame Retardant in Polarizing Film from Waste LCD and Determination by GC-MS

作　　者：邓毅 顾卫华[2] 陈梦君[1] DENG Yi;GU Weihua;CHEN Mengjun(Key Laboratory of Solid Waste Treatment and Resource Recycle,Ministry of Education,Southwest University of Science and Technology,Mianyang 621010,Sichuan,China;School of Resources and Environmental Engineering,Shanghai Polytechnic University,Shanghai 201209,China)

机构地区：[1]西南科技大学固体废物处理与资源化教育部重点实验室,四川绵阳621010 [2]上海第二工业大学资源与环境工程学院,上海201209

出　　处：《有色金属（冶炼部分）》2024年第9期109-113,共5页Nonferrous Metals（Extractive Metallurgy)

基　　金：国家自然科学基金资助项目(51974262);四川省科技厅重点研发计划项目(2019YFS0450)。

摘　　要：废弃液晶面板(LCD)中所含的磷酸三苯酯(TPP)属典型的磷系无卤阻燃剂,具有稳定性高、挥发少、分解时低烟、低毒等优点。利用微波萃取技术提取废弃LCD偏光膜中的TPP,考察了料液比、萃取温度和时间、萃取剂种类对萃取效果的影响,并基于气相色谱-质谱(GC-MS)技术建立TPP的标准检测和分析方法。GC-MS分析结果表明:TPP在0.5~10 mg/L,线性相关系数可达0.9996,线性关系良好,测定下限为0.51 mg/L,方法平均回收率为97.33%~101.00%,相对标准偏差为2.06%~2.70%,可满足废弃LCD中TPP提取过程的检测要求。微波萃取结果表明,在优化条件(萃取剂为丙酮、料液比1∶50、萃取温度55℃、萃取时间20 min、功率250 W)下,TPP提取率为95.20%~96.32%。研究结果为绿色、高效回收废弃LCD提供理论基础和实践经验。Triphenyl phosphate(TPP)contained in waste liquid crystal displays(LCDs)is a typical phosphorus-based non-halogenated flame retardant with the advantages of high stability,low volatility,low smoke and low toxicity during decomposition.The microwave extraction technique was used to extract TPP from waste LCD polarizing film,and the effects of material-liquid ratio,extraction temperature,extraction time and extractant type on extraction effect were investigated.A standard detection and analysis method for TPP based on gas chromatography-mass spectrometry(GC-MS)was established.The results of GC-MS analysis show that the linear correlation coefficients of TPP reach up to 0.9996 in the range of 0.5—10 mg/L with good linearity,and the lower limit of detection is 0.51 mg/L.The average recoveries of the method ranges from 97.33%to 101.00%with the relative standard deviations(RSDs)ranging from 2.06%to 2.70%,which can satisfy the requirements of the detection of TPP extraction process in waste LCDs.The microwave extraction results show that TPP extraction rate is 95.20%—96.32%under the optimum conditions including acetone as the extractant,material-liquid ratio of 1∶50,extraction temperature of 55℃,extraction time of 20 min,and power of 250 W.This study provides theoretical basis and practical experience for environmentally friendly and efficient recycling of waste LCD.

关 键 词：偏光膜 磷系阻燃剂 微波萃取 气相色谱-质谱法(GC-MS) 

分 类 号：TF804.2[冶金工程—有色金属冶金]