热解技术处理废弃印刷线路板的实验研究
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摘要
热解法作为一种较新的线路板处理技术不仅实现线路板中有机组分转化为高品质能源——可燃气、可燃油,同时实现线路板中金属组分与非金属组分的高效分离,最终实现线路板环境友好型资源化回收目的。但是基础数据的缺乏减缓了大型设备研发进程,进而阻碍了热解技术推广应用。针对这一现状,本文选取了两种典型的废弃印刷线路板(FR4板和Teflon板)作为实验对象,开展了如下工作:
利用差热热重分析仪,在N2气氛下考察了两种线路板的热解特性,获得了热解温度、最大热解速率温度、热失重率等重要参数并研究了升温速率对热解参数的影响。着重考察了升温速率、颗粒大小、热解终温对热解残余物性状的影响。研究结果表明:FR4板500℃热解终温,Teflon板700℃热解终温可保证两种线路板中有机组分热解完成,同时实现线路板金属与玻璃纤维很好的分离效果,分离金属片表面干净。而FR4板在320~360℃,Teflon板在560~620℃温度区间达到最大热解速率,在工程设计中可考虑物料在此温区滞留时间。
采用蔡式温度积分近似式,Levenberg-Marqurdt优化非线性回归方法实现了线路板的热解动力学参数的计算,并建立热解模型,所建模型与实验结果拟合良好。可应用该模型预测热解过程中任意温度下原始物样质量随温度变化情况,以指导和优化反应器的设计和运行。
自行设计了固定床热解实验装置,实现了两种线路板热解气体、液体、固体产物的收集,并利用GC-MS(气-质联用)、FTIR(红外光谱)、SEM(扫描电镜)等多种分析测试手段实现了三种产物的定性分析。FR4板中溴元素主要存在于气体产物中,气体产物主要为CO、CO2、丙烯、2-甲基丙烯、溴甲烷以及其他小分子烯烷烃产物,气体产物可通过除溴无害化处理作可燃气回收;液体产物中含有8.333%的水和油质成分。油质成分主要为苯,苯酚,苯和苯酚烷基取代等芳香族化合物,热值可高达30000kJ/kg,可作燃料油回收。Teflon热解气体产物主要为八氟环丁烷以及其他小分子碳氟氢烷烃化合物。两种线路板固体产物主要是由玻璃纤维和金属构成。制作过程中镀金的金属片热解后含有铜、镍、金以及附着在上面未清除干净的碳;而未镀金的金属片仅有铜和附着的碳。
本文还进行了热解技术处理两种线路板的能耗分析。FR4、Teflon型线路板热解反应热分别为19.692MJ/kg和11.374MJ/kg。对于FR4板来说,回收的热解油作为燃料回收,热量仅为反应热的1/4,不足以维持热解反应的持续进行。
Pyrolysis, as a new technique to recycle waste printed circuit boards (PCB), makes the organic fractions of PCB convert to flammable gas and oil which are high-quality energy sources, also leads to the effective seperation of metallic and glassfibre fractions of PCB. Pyrolysis technique achieves the aim of environment- friendly, resource reclamation of PCB. However, the scarce of basic information prevents the large-scale equipment development process; furthermore baffles the application and popularization to recycling PCB with pyrolysis technique. Aiming at these questions, two typical kinds of PCB, called FR4 and Teflon PCB, were chosen as experimental materials and the following studies had been done in the paper:
Pyrolysis characteristics of two kinds of PCB were investigated with the thermo- gravimetric analyser (TGA) with N2and basic parameters such as the pyrolysis initial and final temperature, the temperature at the maximum pyrolysis rate, thermogravi- metric loss were obtained. The influence of heating rate on the pyrolysis characteristic parameters was studied also. The influence of effective factors of heating rate, particle size, and pyrolysis final temperature on the pyrolysis residue morphology was inves- tigated in detail. The results showed that: the pyrolysis temperatures of 500℃for FR4 PCB and of 700℃for Teflon PCB in engineering design not only ensure the complete decomposition of organic component, but also effective seperation of metallic compo- nent and glassfibre component. Also, the temperature at the maximum pyrolysis rate appeared at the range of 320~360℃for FR4 and of 560~620℃for Teflon PCB. Therefore, the longer residence time at the temperature zone of the feedstocks can be considered in engineering design.
The method based on CAI-temperature integral approximation and Levenberg- Marquardt nonlinear regression was carried out to calculate the kinetic parameters of two kinds of PCB respectively and corresponding kinetic models were established. The models were in good agreement with the experimental ones at different heating rate. The effect of the original waste PCB with different pyrolysis time or temperature in process could be estimated based on the models, which could effectively direct and optimize design of pyrolysis reactor.
Pyrolysis gas, liquid, solid products of two kinds of PCB was collected using self-designed fixed-bed pyrolysis experimental device and was analyzed qualitatively with the test methods of GC-MS, FT-IR and SEM. For FR4 PCB, bromide exsited mainly in pyrolysis gas and gas products mainly consisted of CO, CO2, propylene, 2-methacrylate, bromomethane, and a small amount of acetone, C1-C3 halogenation alkyls. The pyrolysis gas could be reclaimed as fules after debromide treatment. Pyrolysis liquid products consisted of 8.333% water and 91.667% oil component.The oil component contained high concentrations of benzene, phenol, alkyl benzene and alkyl phenols, which caloric value was up to 30000kJ/kg and could be reclaimed as fuels.For Teflon PCB, pyrolysis gas contained high concentration of octafluoro- cyclobutane and low concentration of small molecular fluorocarbon-hydrogen compounds. The solid products of two kinds of PCB contained glassfibre and metals. The plated sheet metal after pyrolysis treatment contain copper, nickel, gold and a little carbon; non-plated metal contained copper and carbon attached on the metals.
Energy consumption was analyzed on the treatment of PCB by pyrolysis technology. Pyrolysis reaction heat was 19.692MJ/kg for FR4 PCB and 11.374MJ/kg for Teflon PCB respectively.
For FR4, caloric value of pyrolysis oil was about 1/4 of pyrolysis reaction heat value, which was not enough to support the pyrolysis process of FR4 PCB.
利用差热热重分析仪,在N2气氛下考察了两种线路板的热解特性,获得了热解温度、最大热解速率温度、热失重率等重要参数并研究了升温速率对热解参数的影响。着重考察了升温速率、颗粒大小、热解终温对热解残余物性状的影响。研究结果表明:FR4板500℃热解终温,Teflon板700℃热解终温可保证两种线路板中有机组分热解完成,同时实现线路板金属与玻璃纤维很好的分离效果,分离金属片表面干净。而FR4板在320~360℃,Teflon板在560~620℃温度区间达到最大热解速率,在工程设计中可考虑物料在此温区滞留时间。
采用蔡式温度积分近似式,Levenberg-Marqurdt优化非线性回归方法实现了线路板的热解动力学参数的计算,并建立热解模型,所建模型与实验结果拟合良好。可应用该模型预测热解过程中任意温度下原始物样质量随温度变化情况,以指导和优化反应器的设计和运行。
自行设计了固定床热解实验装置,实现了两种线路板热解气体、液体、固体产物的收集,并利用GC-MS(气-质联用)、FTIR(红外光谱)、SEM(扫描电镜)等多种分析测试手段实现了三种产物的定性分析。FR4板中溴元素主要存在于气体产物中,气体产物主要为CO、CO2、丙烯、2-甲基丙烯、溴甲烷以及其他小分子烯烷烃产物,气体产物可通过除溴无害化处理作可燃气回收;液体产物中含有8.333%的水和油质成分。油质成分主要为苯,苯酚,苯和苯酚烷基取代等芳香族化合物,热值可高达30000kJ/kg,可作燃料油回收。Teflon热解气体产物主要为八氟环丁烷以及其他小分子碳氟氢烷烃化合物。两种线路板固体产物主要是由玻璃纤维和金属构成。制作过程中镀金的金属片热解后含有铜、镍、金以及附着在上面未清除干净的碳;而未镀金的金属片仅有铜和附着的碳。
本文还进行了热解技术处理两种线路板的能耗分析。FR4、Teflon型线路板热解反应热分别为19.692MJ/kg和11.374MJ/kg。对于FR4板来说,回收的热解油作为燃料回收,热量仅为反应热的1/4,不足以维持热解反应的持续进行。
Pyrolysis, as a new technique to recycle waste printed circuit boards (PCB), makes the organic fractions of PCB convert to flammable gas and oil which are high-quality energy sources, also leads to the effective seperation of metallic and glassfibre fractions of PCB. Pyrolysis technique achieves the aim of environment- friendly, resource reclamation of PCB. However, the scarce of basic information prevents the large-scale equipment development process; furthermore baffles the application and popularization to recycling PCB with pyrolysis technique. Aiming at these questions, two typical kinds of PCB, called FR4 and Teflon PCB, were chosen as experimental materials and the following studies had been done in the paper:
Pyrolysis characteristics of two kinds of PCB were investigated with the thermo- gravimetric analyser (TGA) with N2and basic parameters such as the pyrolysis initial and final temperature, the temperature at the maximum pyrolysis rate, thermogravi- metric loss were obtained. The influence of heating rate on the pyrolysis characteristic parameters was studied also. The influence of effective factors of heating rate, particle size, and pyrolysis final temperature on the pyrolysis residue morphology was inves- tigated in detail. The results showed that: the pyrolysis temperatures of 500℃for FR4 PCB and of 700℃for Teflon PCB in engineering design not only ensure the complete decomposition of organic component, but also effective seperation of metallic compo- nent and glassfibre component. Also, the temperature at the maximum pyrolysis rate appeared at the range of 320~360℃for FR4 and of 560~620℃for Teflon PCB. Therefore, the longer residence time at the temperature zone of the feedstocks can be considered in engineering design.
The method based on CAI-temperature integral approximation and Levenberg- Marquardt nonlinear regression was carried out to calculate the kinetic parameters of two kinds of PCB respectively and corresponding kinetic models were established. The models were in good agreement with the experimental ones at different heating rate. The effect of the original waste PCB with different pyrolysis time or temperature in process could be estimated based on the models, which could effectively direct and optimize design of pyrolysis reactor.
Pyrolysis gas, liquid, solid products of two kinds of PCB was collected using self-designed fixed-bed pyrolysis experimental device and was analyzed qualitatively with the test methods of GC-MS, FT-IR and SEM. For FR4 PCB, bromide exsited mainly in pyrolysis gas and gas products mainly consisted of CO, CO2, propylene, 2-methacrylate, bromomethane, and a small amount of acetone, C1-C3 halogenation alkyls. The pyrolysis gas could be reclaimed as fules after debromide treatment. Pyrolysis liquid products consisted of 8.333% water and 91.667% oil component.The oil component contained high concentrations of benzene, phenol, alkyl benzene and alkyl phenols, which caloric value was up to 30000kJ/kg and could be reclaimed as fuels.For Teflon PCB, pyrolysis gas contained high concentration of octafluoro- cyclobutane and low concentration of small molecular fluorocarbon-hydrogen compounds. The solid products of two kinds of PCB contained glassfibre and metals. The plated sheet metal after pyrolysis treatment contain copper, nickel, gold and a little carbon; non-plated metal contained copper and carbon attached on the metals.
Energy consumption was analyzed on the treatment of PCB by pyrolysis technology. Pyrolysis reaction heat was 19.692MJ/kg for FR4 PCB and 11.374MJ/kg for Teflon PCB respectively.
For FR4, caloric value of pyrolysis oil was about 1/4 of pyrolysis reaction heat value, which was not enough to support the pyrolysis process of FR4 PCB.
引文
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