基于Fe-SiO_2的POPs废物机械化学处置工艺及机理研究
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摘要
持久性有机物（POPs）具有致癌、致畸、致突变的“三致”特性，对人类健康和环境构成严重危害。2001年通过的《斯德哥尔摩公约》要求对POPs废物进行环境无害化管理和处置，我国作为缔约方之一目前尚存有数量可观的多种POPs废物，如：滴滴涕、六六六、氯丹、灭蚁灵等禁用农药。传统的高温焚烧技术易生成毒性更大的二噁英类，因此近年来非焚烧处置技术的开发应用在国际上成为热点。本论文针对机械化学法常用的氧化钙（CaO）脱卤剂存在反应慢、脱氯率不高等问题，旨在开发基于更为高效稳定的脱卤试剂的新工艺，优化反应关键工况参数，考察对典型POPs的降解动力学和反应机理，并探索对处置后的无害化产物加以综合利用。
通过在同等条件下的对比试验发现，以铁粉和石英砂为脱卤剂的Fe-SiO_2机械化学工艺对四种目标污染物（六氯苯、灭蚁灵、得克隆和五氯硝基苯）处置效率最高、速率最快（比传统氧化钙工艺节省25%以上的时间）。以灭蚁灵为例，对Fe-SiO_2机械化学工艺进行工况参数影响分析，发现速率常数对球料比、转速的二阶导数以及速率常数对转速、球料比的二阶导数都为常数0.00038，这个值是速率常数、转速和球料比三者之间的内在联系。由此获得了速率常数和球料比、转速的响应面方程，经检验能够对不同工况下的降解情况做出合理预测。
通过气相色谱/质谱仪、离子色谱等化学分析方法，结合红外光谱、拉曼光谱、顺磁共振等固体表征手段，发现反应的最终产物为石墨碳、无定形碳和无机氯化合物。提出了Fe-SiO_2机械化学处置五氯硝基苯的脱氯-缩合-碳化反应路径。发现石英砂在高能球磨下可以引发固体废物中氯代有机物的脱氯反应，石英砂粉碎过程中生成的自由基是导致这一反应的主要因素。铁粉有利于机械球磨反应中形成摩擦等离子体区域，而石英砂有利于反应中自由基的生成，这二者是互相促进，互补的关系。
利用铁碳微电解原理，将Fe-SiO_2机械化学处置五氯硝基苯后的无害化固体残渣用于水相中4-氯酚的还原脱氯。当投加量100g/L时，初始浓度为100mg/L的4-氯酚在4h可以达到46%以上的脱氯率，机械化学处置中生成的无机碳对脱氯具有促进作用。
Persistent organic Pollutants (POPs) have three kinds of characteristics which willlead to cancer, teratogenic and the mutation. They will damage human lives andenvironment. The Stockholm convention requests non-hazardous administration anddisposal of POPs wastes since2001. China now has plenty of POPs wastes to be treated,such as DDT, benzex, chlordane and mirex. The traditional high temperatureincineration will generate the much more toxic compounds such as dioxins and furans,so the non-combustion technologies became more and more attractive internationally.According to the problems of slower reaction and lower dechlorination in the CaOreagents applied in mechanochemical destruction, our thesis will try to develop a moreeffective dechlorniation reagent, and to investigate the kinetics and mechanisms of theprocess, the possibility of reutilization of non-hazardous products.
The mechanochmeical degradations of four model pollutants (HCB, Mirex, DPand PCNB) under different reagents proved that Fe-SiO_2(containg iron powder andquartz sand) is the highest and best reagents. To analyze the technological parametersof mirex destruction by using Fe-SiO_2process, the second derivatives of reaction rateconstants to charge ratio and rotation speed were the same numerical value,~0.00038.This value was the internal relations between rotation speed, charge ratio and reactionrate constants. The response-area-equation was deduced and its feasibility waspredicted.
After solid powder’s characterization by degradation, dechlorination,intermediates from GC/MS, FTIR spectrum, Raman spectrum and ESR spectrum, thefinal products contains graphite, amorphous carbon and inorganic chlorine. Thedechlorination-polymerization-carbonization pathways in MCD process wereconcluded respectively by Fe and by SiO2. The SiO2has the dechlorination reactionwith chlorinated organic compounds in the mechanochemical system. The mechanicradicals produced by smash of quartz sand were the main factor for this dechlorinationreaction. It is concluded that the iron powder was in favor of triboplasma areaproduction and SiO2was in favor of formation of mechanic-radicals. They bothpromoted and complemented each other. Based on the principle of micro-electrolysis by Fe/C, it is found that the non-hazardousproducts of MCD PCNB by Fe-SiO_2can reduce and dechlorinate4-Chlorophenol(4-CP). The carbon materials formed after MCD treatment fercilitated thedechlorination of4-CP.
通过在同等条件下的对比试验发现，以铁粉和石英砂为脱卤剂的Fe-SiO_2机械化学工艺对四种目标污染物（六氯苯、灭蚁灵、得克隆和五氯硝基苯）处置效率最高、速率最快（比传统氧化钙工艺节省25%以上的时间）。以灭蚁灵为例，对Fe-SiO_2机械化学工艺进行工况参数影响分析，发现速率常数对球料比、转速的二阶导数以及速率常数对转速、球料比的二阶导数都为常数0.00038，这个值是速率常数、转速和球料比三者之间的内在联系。由此获得了速率常数和球料比、转速的响应面方程，经检验能够对不同工况下的降解情况做出合理预测。
通过气相色谱/质谱仪、离子色谱等化学分析方法，结合红外光谱、拉曼光谱、顺磁共振等固体表征手段，发现反应的最终产物为石墨碳、无定形碳和无机氯化合物。提出了Fe-SiO_2机械化学处置五氯硝基苯的脱氯-缩合-碳化反应路径。发现石英砂在高能球磨下可以引发固体废物中氯代有机物的脱氯反应，石英砂粉碎过程中生成的自由基是导致这一反应的主要因素。铁粉有利于机械球磨反应中形成摩擦等离子体区域，而石英砂有利于反应中自由基的生成，这二者是互相促进，互补的关系。
利用铁碳微电解原理，将Fe-SiO_2机械化学处置五氯硝基苯后的无害化固体残渣用于水相中4-氯酚的还原脱氯。当投加量100g/L时，初始浓度为100mg/L的4-氯酚在4h可以达到46%以上的脱氯率，机械化学处置中生成的无机碳对脱氯具有促进作用。
Persistent organic Pollutants (POPs) have three kinds of characteristics which willlead to cancer, teratogenic and the mutation. They will damage human lives andenvironment. The Stockholm convention requests non-hazardous administration anddisposal of POPs wastes since2001. China now has plenty of POPs wastes to be treated,such as DDT, benzex, chlordane and mirex. The traditional high temperatureincineration will generate the much more toxic compounds such as dioxins and furans,so the non-combustion technologies became more and more attractive internationally.According to the problems of slower reaction and lower dechlorination in the CaOreagents applied in mechanochemical destruction, our thesis will try to develop a moreeffective dechlorniation reagent, and to investigate the kinetics and mechanisms of theprocess, the possibility of reutilization of non-hazardous products.
The mechanochmeical degradations of four model pollutants (HCB, Mirex, DPand PCNB) under different reagents proved that Fe-SiO_2(containg iron powder andquartz sand) is the highest and best reagents. To analyze the technological parametersof mirex destruction by using Fe-SiO_2process, the second derivatives of reaction rateconstants to charge ratio and rotation speed were the same numerical value,~0.00038.This value was the internal relations between rotation speed, charge ratio and reactionrate constants. The response-area-equation was deduced and its feasibility waspredicted.
After solid powder’s characterization by degradation, dechlorination,intermediates from GC/MS, FTIR spectrum, Raman spectrum and ESR spectrum, thefinal products contains graphite, amorphous carbon and inorganic chlorine. Thedechlorination-polymerization-carbonization pathways in MCD process wereconcluded respectively by Fe and by SiO2. The SiO2has the dechlorination reactionwith chlorinated organic compounds in the mechanochemical system. The mechanicradicals produced by smash of quartz sand were the main factor for this dechlorinationreaction. It is concluded that the iron powder was in favor of triboplasma areaproduction and SiO2was in favor of formation of mechanic-radicals. They bothpromoted and complemented each other. Based on the principle of micro-electrolysis by Fe/C, it is found that the non-hazardousproducts of MCD PCNB by Fe-SiO_2can reduce and dechlorinate4-Chlorophenol(4-CP). The carbon materials formed after MCD treatment fercilitated thedechlorination of4-CP.
引文
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