脂塑产品生产过程中有毒物质的分析与应用

发布时间：2018-04-02 16:13

本文选题：废旧线路板　切入点：脂塑　出处：《江苏理工学院》2017年硕士论文

【摘要】：废线路板回收再利用形成脂塑产品可以应用于各种场所大大提高了废线路板的利用率。然而,在脂塑产品生产及回收利用过程中产生的有毒有害物质造成的二次污染亟须关注。本文介绍了一种以废线路板为原料的脂塑产品—仿石板砖的生产工艺,并根据其样品基质的特点建立了仿石板砖生产过程中有毒物质二VA英、重金属铅、多溴联苯以及多溴联苯醚的分析方法,并应用于仿石板砖生产过程中这四类有毒物质的含量监测。采用甲苯索氏提取固体样品中的二VA英,经多层硅胶柱和活性炭柱净化、旋蒸浓缩,以60 m超长毛细管色谱柱进行分离和MID模式进行检测,以保留时间和同位素特征离子丰度比进行定性,用~(13)C标记同位素稀释内标法进行定量,建立了针对废线路板及脂塑基质特点的ID-HRGC/HRMS测定二VA英的方法。该方法所得15种~(13)C-2,3,7,8-PCDD/Fs提取内标的平均回收率范围为62.24%~86.29%,满足国标(17%~181%)要求。建立了甲苯索氏提取固体样品中的PBBs以及PBDEs,并经自填多层硅胶柱净化,旋蒸浓缩后采用GC-MS/MS定性定量分析废线路板及脂塑产品中PBBs以及PBDEs的检测方法。该方法检出限为3.26μg/mL~9.25μg/m L,平均加标回收率范围为71.44%~94.39%和67.32%~75.71%,相对标准偏差为1.09%~3.05%。此外,采用灰化法和酸消解法对废线路板及脂塑产品进行前处理,ICP-AES及外标法定量分析金属铅的含量。结果表明,此方法标准曲线的线性相关性良好,线性相关系数大于0.9999。对仿石板砖样品中四类有毒物质的含量监测结果可知,仿石板二VA英的总量为5.0860 ng TEQ/Kg,PBBs和PBDEs的含量为6.8869μg/g和2.5570μg/g,铅含量为0.0622 mg/g,均低于国家标准-危险废物鉴别标准/毒性物质含量鉴别标准(GB5085.6-2007)中的规定限值。这四类有毒物质均来源于仿石板砖生产原料。生产过程中有毒物质的含量变化不大。废水中检出少量的有毒物质。
[Abstract]:The recovery and reuse of waste circuit board can be used in various places to improve the utilization rate of waste circuit board.However, the secondary pollution caused by toxic and harmful substances in the process of production and recycling of lipoplastic products should be paid close attention to.In this paper, the production process of imitating stone slabs, which is made of waste circuit board as raw material, is introduced. According to the characteristics of sample matrix, the toxic substances diVA and heavy metal lead in the production process of imitating stone slabs are established.The analytical methods of polybrominated biphenyls and polybrominated diphenyl ethers were used to monitor the contents of these four toxic substances in the production of stone imitation slabs.DiVA was extracted from solid sample by toluene Soxhlet, purified by multilayer silica gel column and activated carbon column, then concentrated by spin steam, separated by 60 m long capillary column and detected by MID model.Based on retention time and isotopic characteristic ion abundance ratio, a ID-HRGC/HRMS method for the determination of diVA in waste circuit boards and lipopolysaccharide substrates was established by using 13C labeled isotope dilution method.The average recovery range of the internal standard extracted by this method is 62.24 ~ 86.29, which meets the requirements of the national standard 17 ~ (181).A method was established for the determination of PBBs and PBDEs in waste circuit board and lipoplastic products by GC-MS/MS after extraction by toluene Soxhlet and purified by self-filled multilayer silica gel column.The detection limit of this method is 3.26 渭 g/mL~9.25 渭 g / mL, and the average recoveries are 71.44% and 67.32 渭 g / mL, respectively. The relative standard deviation is 1.09% and 3.05%.In addition, ICP-AES and external standard method were used to determine the content of lead in waste circuit board and lipoplastic products by means of ashing method and acid digestion method.The results show that the linear correlation of the standard curve is good, and the linear correlation coefficient is greater than 0.9999.The results of monitoring the contents of four kinds of toxic substances in the samples of imitated slabs show that,The contents of PBDEs and PBDEs were 6.8869 渭 g / g and 2.5570 渭 g / g, respectively, and the content of lead was 0.0622 mg / g, which was lower than the prescribed limit of GB5085.6-2007in the national standard, the identification standard for hazardous wastes and the identification standard for toxic substances content (GB5085.6-2007).The four kinds of toxic substances all come from the raw materials of stone-imitating brick production.The content of toxic substances does not change much during production.A small amount of toxic substances were detected in the waste water.
【学位授予单位】：江苏理工学院
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X799.1;TU522.09

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