电弧炉飞灰和垃圾焚烧灰及剩余活性污泥的部分资源化处理方法研究

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英文题名：Several Treatment Methods on the Recycling of Electric Arc Furnace Fly Ash, MSWI Ash and Sewage Sludge 作者：林奕明 论文级别：博士 学科专业名称：环境科学与工程 中文关键词：电弧炉飞灰 ; 垃圾焚烧灰 ; 活性污泥 ; PCDD/Fs ; PBDEs ; 重金属 ; 水泥 ; 粒度 ; 处理 ; 资源化 英文关键词：EAF fly ash ; MSWI ash ; sewage sludge ; PCDD/Fs ; PBDEs ; heavy metal ; cement ; particle size ; treatment ; recycling 学位年度：2013 导师：周少奇 学科代码：0830 学位授予单位：华南理工大学 论文提交日期：2013-04-10 答辩委员会主席：张仁铎

摘要

本文主要对电弧炉飞灰，垃圾焚烧灰及污水厂剩余活性污泥开展部分资源化技术方法的研究，以期为进一步实现对这三种固体废物的资源化处理提供一定的研究基础。
     首先，开展了电弧炉飞灰的资源化研究。本研究阶段主要利用电炉熔炼电弧炉飞灰和玻璃粉末回收金属材料并降解其含有的高浓度二恶英（PCDD/Fs）和多溴联苯醚（PBDEs）。从整个装置系统出发，研究了PCDD/Fs和PBDEs在电弧炉飞灰、玻璃材料、熔渣、金属铸块、冷却系统，过滤装置和聚氨酯泡沫塑料套筒系统中的含量。同时分析了PCDD/Fs和PBDEs各种同类物的特性，并基于物质平衡研究了PCDD/Fs的生成，降解和最终归宿。实验结果表明，电弧炉飞灰中PCDD/Fs的国际毒性当量为1414ngI-TEQ/kg，超出了现有的相关土地的排放标准。电炉飞灰经1450℃高温熔炼处理后能回收其所含的金属材料，且PCDD/Fs在所有固体产物中和经过安装尾气处理系统后尾气中的浓度均低于相关的排放标准值。另外，电弧炉飞灰中PBDEs含量为50128ng/kg，经1450℃热处理后，固体产物中PBDEs的含量低于相关背景土壤中的含量，而最终尾气所排放的浓度也都低于其它冶金行业烟囱所排放的浓度。同时实验得出PCDD/Fs和PBDEs都能在实验冷凝系统的管壁中通过de novo主导方式重新合成。通过Pearson相关系数分析结果表明，logPBDEs/(logPCDD/Fs)比值能够用来评价烟囱中同时排放PBDEs和PCDD/Fs两种污染物相互之间的变化关系。因此，实验所设计的利用电炉熔炼电弧炉飞灰和玻璃粉的研究方法，不但能够很好的降解含氯/溴量高的PCDD/Fs和PBDEs同类物，同时也能够降解PCDD/Fs和PBDEs的碳环结构并回收了电弧飞灰中的金属材料。
     其次，开展了垃圾焚烧灰主要特性的研究。结果表明，华南地区垃圾焚烧飞灰主要质量分布的粒径范围小于0.28mm中，而底灰的主要质量分布在当其粒径大于0.28mm中。通过XRF和XRD分析不同粒径范围下的飞灰和底灰的化合物组成成分和晶体特征，得出飞灰中含有的主要物质同其它地区产生的飞灰和底灰基本相同。经检测得出不同粒径飞灰和底灰中重金属元素Cd, Cr, Cu, Pb和Zn超出了土壤标准GB15618-1995中三类土壤中所规定的值。同时得出其十六种PAHs同类物的总量在不同粒径底灰的含量范围为43.42～247.14ng/g，该含量与欧洲一些国家焚烧底灰中的含量基本相同，但低于中国一些地区焚烧底灰中的含量。通过对不同粒径范围的飞灰和底灰的毒性浸出实验，得出当用蒸馏水作为浸提剂时，Pb元素超过了标准GB5085.3-2007中所规定的值，而当用2#溶液作为浸提剂时，Cd元素则超过了该标准中所规定的值，而所有粒径范围的底灰的重金属浓度都低于该标准所规定的值。因此，建议可将焚烧底灰适当进行资源化利用，但需要进一步进行环境评估和监测。
     另外，利用城市垃圾焚烧飞灰对染料的吸附实验结果表明，粒径小于0.076mm的飞灰对亚甲基蓝的最大吸附量为0.692mg/g，比发电厂所产生的粉煤灰的吸附能力要低。当用0.5mol/L乙酸溶液以液固比值分别为4,6和8处理飞灰后，得出的飞灰样品比原灰对染料的吸附能力得到很大的提升。同时，该样品在对亚甲基蓝染料吸附后混合液中重金属元素Pb, Cr和Cd浓度都低于毒性浸出标准GB5085.3-2007。飞灰对亚甲基蓝染料的吸附符合Langmuir和Freundlich等温吸附模型，动力学模型则符合假二级动力学吸附模型。此外，分别对用蒸馏水和酸溶液处理后的飞灰样品的BET比表面积，XRD，SEM及相应EDS，FT-IR图谱分析研究证明，经乙酸处理后飞灰的微孔数增多，且飞灰中大部分可溶性碱性物质都被溶解于溶液中，从而提高了其对亚甲基蓝染料的去除效率。
     通过对两座垃圾焚烧厂不同粒径的焚烧底灰中PBDEs的含量及其毒性浸出的研究，发现含有工业上常用的PBDEs同类物的垃圾在焚烧过程中有部分PBDEs化合物未被完全降解而直接存留在底灰中。PBDEs主要分布在底灰中的粒径范围为0.25～1.0mm，且趋向于分布在粒径较大的底灰里面。此外，底灰中PBDEs的毒性浸出浓度范围为0.684～18.1ng/l，其百分浸出率是电视机外壳生产过程中所用的原料和加入PBDEs同类物后的成品的5倍以上，因而在利用垃圾焚烧厂焚烧底灰作为资源化材料时必须慎重考虑可能会导致PBDEs的渗出而造成相应的环境问题，建议将底灰进行粒径分类后资源化利用。
     最后，开展了市政活性污泥的资源化利用研究，实验将干污泥以不同百分含量的方式掺入到水泥生产过程的生料中，从而利用水泥窑煅烧熟料的过程来达到完全处理剩余活性污泥的目的。通过对水泥熟料，水泥凝结时间，水泥抗压抗折强度，水泥XRD，SEM的表征测定及毒性浸出实验得出：XRD图谱显示所有熟料中的主要物质是C3S, C_2S,C3A和C4AF，熟料中还发现了存在物质形式为Ca54MgAl2Si16O90的晶体相。同时，熟料中C_2S (α-C_2S或β-C_2S)晶相随着干污泥掺入量的增加而增加。通过SEM测定得出，当干污泥的掺入量达到15%时，熟料中的微观结构上出现了一定量的微孔特征，说明干污泥的掺入导致了熟料的微相结构发生了变化。另外，干污泥的掺入导致了所得水泥产品的的初凝和终凝时间的增加，并降低水泥砂胶的早期抗折强度且随着干污泥掺入量的增加而逐渐降低，但对水泥抗压强度的影响不大。这是由于经煅烧后所得熟料中C_2S(α-C_2S或β-C_2S)晶相含量的增加，从而降低了水泥的水化速度。并且C_2S的含量随着干污泥掺入量的增加而增加，从而水化速度降低程度也就越大，初期强度降低也就越大。熟料中金属元素Ti, Ba, Zn, Cr, Cu, Ni和Pb的含量随着干污泥掺入量的增加而增加，而Al, Fe和Mn则略显降低。而这些元素含量的变化可能与水泥的水化速度和熟料煅烧过程中晶体的形成变化有关。通过毒性浸出实验得出所有熟料中重金属的浸出浓度都低于国家标准GB5085.3-2007中所规定的值。
In this study, several treatment methods on the recycling of electric arc furnace (EAF) flyash，municipal solid waste incineration（MSWI）ash and sewage sludge were carried out basedon the disposal and reuse of those waste solids.
     Firstly, thermal treatment equipment was employed to treat the EAF fly ash. ThePCDD/F and PBDEs contents/concentrations in the EAF fly ash, cullet, slag, ingot, coolingunit, filter and PUF cartridge were all determined. The congener profiles were then derivedand analyzed, while the fate of the PCCD/Fs and PBDEs was discussed based on massbalance calculations. The results showed that the total PCDD/F I-TEQ in the EAF fly ash was1414ng I-TEQ/kg, revealing that it exceeded the soil pollution standard (1000ng I-TEQ/kg).After treatment of EAF fly ash at1450°C, the total contents of PCDD/Fs and I-TEQ in theEAF fly ash can be effectively reduced and the metal contents were sucessful to be recoveredas the ingot. The PCDD/Fs I-TEQ in the emission was lower than the value of relativeemission standards after the emission was treated with the air pollution control devices(APCDs). Moreover, the total PBDE content in EAF fly ash was50128ng/kg. After thethermal treatment at1450°C, the amount of PBDEs in EAF fly could significantly reduce andthe PBDEs existed in the slag and ingot also were less than in the natural ground soil. Thetotal PBDE concentration in the flue gas was much lower than the content in all the otherplants when it was installed the APCDs. In addition, the reformation of PCDD/F and PBDEcongeners was found in the cooling unit through de novo synthesis and precursorcondensation. The results of the mass ratio and Pearson correlation analyses suggested thatthe ratio of log PBDEs/(log PCDD/Fs) could be used to evaluate the emissions from one tothe other (PCDD/Fs and PBDEs) from the emission sources. Therefore, the thermal treatmentmethod presented in this work not only enhanced the dechlorination/debromination of thehigh-chlorinated/brominated congeners, but also decomposed the aromatic rings of PCDD/Fsand PBDEs. But most of all, it recovered the metal from the EAF fly ash.
     In addition, the characteristics of the MSWI fly ash and bottom ash which had beenproduced from the incinerator located in South China were investigated. The results showedthat the size distributions of the highest particle mass content in the fly ash was located at theparticle size below0.28mm, while that in the bottom ash was located at the particle sizelarger than0.28mm. The main components and its characteriation of the MSWI fly ash andbottom ash were detected by XRD and XRF. The results showed that main components andcrystal phases of them were similar to those of other areas of China and abroad. The contents of Cd, Cr, Cu, Pb and Zn in the MSWI fly ash and bottom ash exceeded the regulatorythreshold value of the Ⅲ kind soil in accordance with GB15618-1995. The total contents ofPAHs in different particle sizes of bottom ash had a range of43.42-247.14ng/g, revealing thatit was similar to those in the European regional. However, it was lower than some areas ofChina. The leaching concentrations of Pb was exceeded the regulatory threshold value inChina which was listed in accordance with GB5085.3-2007when it used distilled water asleaching agent, while the leaching concentrations of Cd was exceeded the regulatory thresholdvalue when it used2#solution as leaching agent. Moreover, the leaching concentrations of allthe heavy metals in the bottom ash were lower than the regulatory threshold criteria values inChina (GB5085.3-2007) when it used distilled water and2#solution as leaching agents.Therefore, we recommend that the bottom ash can be reutilization as construction material,but its the environmental safety and influences need to be further evaluated.
     Moreover, the evaluation and test of adsorption dye from aqueous solutions by theoriginal and modified MSWI fly ash were investigated. The fly ash was used to remove theMethylene Blue from aqueous solutions. The maximum amount of MB on to the original flyash was0.692mg/g when their the particle size of the was below0.076mm, which showedthat it lower than those of using coal fly ash as adsorbent for the removal of MB. Moreover, itcould be found that the Pb content in the fly ash could be completely removed and itsadsorption capacity could be obvious improved when the fky ash was treated with a0.5mol/Lacetic acid solution at the L/S ratios of4,6and8. The concentrations of Pb, Cr and Cd in theMB solutions after adsorption processes were below the regulatory threshold values in Chinawhich were listed in accordance with GB5085.3-2007. In addition, the adsorption isothermdata were well fitted by both Langmuir and Freundlich models, and the seconded-orderkinetic model perfectly fitted for the MSWI fly ash systems. According to the results of BET,XRD, SEM-EDS and FT-IR, it revealed that the BET surface area of acetic acid solutiontreatment fly ash was four times than that of original fly ash. This was due to the impurities insurface of original fly ash could be removed by acetic acid solutions and formed the smallerpores, leading to the increasing of BET surface and increase the dye removal percentage.
     The leaching characteristics and particle size distributions of polybrominated diphenylethers (PBDEs) in the bottom ash of two municipal solid waste incinerators (MSWIs A and B)were measured and discussed. The results showed that industrial waste in the municipal wastecontained commercial PBDE mixtures and they were not completely destroyed during theincineration process. The size distribution of the PBDE content in the bottom ash of bothMSWIs was mainly in the range of0.25to1.0mm, with the larger particles predominating. Moreover, the PBDE concentrations in the leachate for MSWI A and B ranged from0.684to1.23ng/l. The mean normalized leaching ratios of the individual PBDE congeners in thebottom ash in MSWIs A and B were5times more than the levels found in the leaching test forone raw plastic material (ND-HIPS) and three different TV housing samples. Therefore, thepotential leaching of PBDEs to the around during reutilization of bottom ash from MSWIsmust be carefully considered. We suggest that the bottom ash may be reutilization asconstruction material with different particle sizes.
     Finally, the effects of using dried sewage sludge as additive on cement property in theprocess of clinker burning were investigated in this part. The results indicated that the majorcomponents in the eco-cement clinkers were similar to those in ordinary Portland cement. Theflexural and compressive strength and setting time of eco-cement pastes, scanning electronmicroscope (SEM) micrographs, XRD characterization analysis, heavy metal leachability andchanges of element content of eco-cement clinkers are also investigated. The X-ray diffractionpatterns of all the clinkers showed that the major components present in the eco-cementclinkers were C3S, C2S, C3A, C4AF and that the phase formation of Ca54MgAl2Si16O90wasidentified in all the clinkers. The C2S (α-C2S or β-C2S) phase formation and peaks increasedwith increases in sewage sludge. Investigations by SEM gave evidence of the C2S (α-C2S orβ-C2S) phase formation increasing with increases in sewage sludge content while the C3Sstructures decreased. Particularly, the microstructure of the mixture in the clinker containing15.0%sewage sludge was significantly different in that it displayed a larger amount of poredistribution. Moreover, all the eco-cement pastes had both delayed initial setting times andfinal setting times. The early flexural strengths of all the eco-cement pastes were lower thanthat of the plain paste, whereas their compressive strengths only were a little lower than theplain paste. The more sewage sludge that was added to the raw meals, the lower the flexuralstrengths of the eco-cement pastes. However, there was no significant effect on all thestrengths at later curing ages. This might be primarily attributed to the increased amounts ofC2S in the eco-clinkers and the minor elements carried from the sewage sludge. In addition,the concentrations of Ti, Ba, Zn, Cr, Cu, Ni and Pb in the clinkers increased with the sewagesludge addition into the raw meals, while Mg, Sr obviously decreased, and Al, Fe, Mn slightlydecreased. Finally, the leaching concentrations of all types of eco-cement clinkers met thestandard of current Chinese regulatory thresholds.

引文

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