废电路板热解特性及其热解油的资源化研究
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摘要
废电路板是电子垃圾中最复杂、最难以处理的重要组成部件。以破碎和分选过程相结合的机械物理方法是其资源化回收处理的主流技术。由于废电路板强度高、硬度大、金属与非金属间结合紧密,机械破碎过程存在二次污染、效率低、能耗高和过粉碎等问题。就如何提高破碎效率和降低过程能耗己成为机械物理技术发展面临的难题。
废电路板是由铜箔、树脂和增强材料层压而成的复合材料。热解作为一种较新的废电路板处理技术,可使废电路板中的树脂粘结层发生分解,削弱金属与非金属层间的结合力,从而实现金属和非金属层的高效解离；此外,热解过程中产生的热解气和热解油可作为燃气或化工原料回用。根据废电路板热解处理的优点,本论文提出废电路板热解后再进行金属和非金属分离回收的“前置热解法”处理废电路板,通过热解对废电路板进行加热改性处理,以提高废电路板中金属与非金属的破碎解离效率,降低过程能耗。本论文开展的主要研究工作和结论如下：
(1)研究了废电路板的机械解离特性。利用两级破碎方式对废电路板进行机械破碎,了解不同粒径下金属和非金属的解离情况,并对其破碎产物的微观形貌、粒径分布等特性进行研究。研究结果表明,废电路板粉碎过程可分为金属解离和粒径调整两个阶段,机械解离的适宜破碎粒度应控制在0.59-0.15mm之间。废电路板粉碎料经筛分后,金属铜在0.25-0.42mm粒径范围内的含量最高,达32.32%。除C,H,O元素外,废电路板中还主要含有Si,Ca,Cu,Br等元素。不同粒径的废电路板热值在8.07-11.69MJ/kg之间,灰分在53.87-80.45%之间。
(2)开展了大物料量热重实验研究。在自行设计的实验室规模的热重分析装置上进行了较大物料量的热重实验,研究了废电路板、键盘和电线三种典型电子垃圾组分的热解行为和特性,并与常规热重分析仪(微热重)上所得的实验结果进行比较,分析了微热重和大物料量热重两种不同模式下电子垃圾的热解机制,得到了相关的热解动力学参数。研究结果表明,大物料量热重相对于微热重存在热滞后效应,具有较低反应活化能值；分布活化能模型分析结果表明,热解过程中活化能随失重率变化,而不是单一数值。在相同热解条件下,实验所用三种物料的热稳定性顺序为：电线<废电路板<键盘,与其活化能值顺序一致。升温速率和颗粒粒径是影响废电路板热解过程的重要参数。随升温速率的增大,废电路板热解的TG和DTG曲线均向高温区移动；物料粒径的增大会抑制颗粒内部热解反应的进行。
(3)借助TG-FTIR和Py-GC/MS联用技术手段,研究了废电路板热解产物的析出过程以及热解产物类型,并探讨了一些代表性产物的形成机理。研究结果表明,废电路板热解过程中气体产物的形成和释放主要集中在270-400℃,和废电路板样品的热失重温度区间一致。废电路板热解时主要经历三个阶段：①第一阶段,<293℃,主要是小分子气体产物H20, CH4, HBr, CO2, CH3COCH3的析出；②第二阶段,293-400℃树脂的主键大规模降解,释放出大量的大分子量有机物质,如酚类、醛类、酮类等；③第三阶段,>400℃,主要发生焦炭的碳化重整。在热解过程中,废电路板环氧树脂中的OH-C, O-CH2, C-C(phenyl), CH2-O-phenyl, C(phenyl)-Br等键发生了断裂,其中O-CH2的断键反应占主导地位。废电路板热解过程中约产生27种有机物,其中苯酚、异丙烯基苯酚和双酚A是主要的降解产物。
(4)在自行设计的管式炉热解实验台上开展了废电路板批量热解实验,考查了热解终温和加热方式对废电路板热解后得到的残渣、热解液和热解气三种状态产物产率和产物性质的影响,利用氧弹热量计,FTIR,1H-NMR, GC-MS等多种测试手段实现了三种产物的定性分析。分析结果表明,当热解终温为600℃时,可得到76.13%的固体产物,14%的液体产物和9.86%的气体产物。当温度在600℃以上时,固体残渣的产率随温度变化不大,升高温度只是改变油气比。快加热方式下的焦油产率要比慢加热方式下的高。废电路板热解后分层效果明显,经加热改性处理后实现了非金属与金属在大粒径范围下的充分解离。解离后的玻璃纤维呈片状,避免了“过粉碎”,使回收获得的玻璃纤维再利用的可行性大增而使得加工容易。此外,热解过程中产生的热解气体中含有H2,CO, CH4等可燃组分,气体热值在11.24-15.21MJ/Nm3,可作为燃气为热解过程提供能量；热解油中含有大量的酚类化合物,如苯酚、异丙基苯酚等,热值在24.5-27.5MJ/kg之间,可作为燃料油回用,也可从中分离提取高附加值化工单体。
(5)开展了废电路板热解油再资源化利用的研究。根据废电路板热解油富含酚类化合物的特点,提出了以热解油代替苯酚制备酚醛树脂的资源化利用方案,接着以制得的酚醛树脂为前躯体,通过与二茂铁进行催化共热解制备了CNTs,利用KOH(?)活化法制备了多孔炭。运用FTIR,1H-NMR, XRD, SEM, TEM, N2-等温吸附等技术手段对所制备产物的性能进行了分析表征。研究结果表明,废电路板热解油与甲醛在氨催化作用下可聚合成热解油酚醛树脂,聚合后,热解油中的芳环质子通过亚甲基键(-CH2-)或醚键(-CH2-O-CH2-)连接。制得的CNTs的产率为56.82%,具有中空结构,外径～338nm,壁厚～86nm,长度达几微米；制得的多孔炭产率为38.05%,表面存在大量的孔隙结构,孔边缘清晰,对氮气的吸附等温线属于典型的I型吸附等温线,以微孔为主,比表面积达1214m2/g,总孔容积为0.64cm3/g。
Printed circuit board (PCB) waste is a major constituent in electronic waste, which is very difficult to treat compared with other components. Mechanical treatment which employs crushing and separation processes for PCB recovery is becoming more popular and widely used in industrial practice. However, the characteristics of PCB with high hardness and tenacity, compact cohesion between metal and non-metal, could lead to secondary pollution, low efficiency, high-energy consumption and over-pulverization during mechanical crushing process.
PCB waste mainly contains organic materials, metals and glass fiber. Pyrolysis is considered as a promising technique to recycle PCB waste. In pyrolysis process, the organic resin in PCB was decomposed into gas and liquid, thus weakening the binding force between the metal and non-metal layer and achieving efficient dissociation of metal and non-metal. Addtionally, the liquid and gas produced during pyrolysis could be reused as chemical feedstock or fuel. Based on the advantages of PCB pyrolysis listed above, a new process for recycling PCB waste defined as'pre-pyrolysis method'was proposed in this study, that is PCB waste was pyrolyzed, and then the metal separation occurred, with the aim to improve the liberation efficiency of metal and non-metal and reduce the energy consumption. The following works are carried out and the main conclusions are as follows in this dissertation:
(1) The mechanical liberation characteristics of PCB waste were studied. A two-step crushing process which combined with a coarse-crushing step and a fine-pulverizing step was adopted. The liberation situation of the crushed products was observed. Properties of the crushed products, such as morphology, particle size distribution were determined. The results indicated that the crushing process of PCB could be divided into two stages, including metal dissociation and particle size adjustment. The suitable particle size for mechanical dissociation of PCB should be controlled in the range of0.59-0.15mm. The major elements in PCB include Si, Ca, Cu, Br except C, H, O. Copper was the most dominating metal in PCB and reached its maximum content in0.42-0.25mm particle size, about32.32%. The calorific values of PCB in different size changed in the range of8.07-11.69MJ/kg. The ash content was between53.87%and80.45%.
(2) Thermogravimetric analysis on a self-designed laboratory scale thermo-balance (called Macro-TG) with more sample loading was carried out. The pyrolysis characteristics of typical components of e-waste, wire, keyboard and PCB waste, were investigated. The results were compared with those obtained in common thermo-gravimetric measurements (called common TG). The kinetic mechanism function of samples both in Macro-TG and common TG was determined. Additionally, the corresponding kinetic parameters of each sample were also obtained. The results indicated that large particles existed a pyrolysis reaction retardarce compared to fine one. And smaller activation energy were found in pyrolysis reaction occurred in Macro-TG. Distributed activation energy model analysis revealed that activation energy did not show a constant value during the pyrolysis process, and it changed with the rate of weight loss. Due to the composition difference, pyrolysis behaviors of wire, keyboard and PCB waste were different. In the same pyrolysis conditions, the sequence of thermal stability for the three studied species is described as:wire (3) A combination of thermogravimetry-fourier transform infrared spectrum (TG-FTIR) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) techniques was employed to investigate the pyrolysis characteristics and gas product properties of PCB waste. The obtained information is used to explain the possible mechanism of PCB pyrolysis. The results indicated that gaseous products from PCB waste pyrolysis mainly evolved at270-400℃, which is in agreement with the observation obtained from the thermoanalysis. PCB waste degradation could be separated into three stages. The main products in the first stage (<293℃) are H2O, CH4, HBr, CO2, CH3COCH3. High-molecular-weight organic species, including phenolic compounds, aldehyde, ketone, etc., mainly evolved in the second stage. In the last stage, at temperatures above400℃, carbonization and char formation occured. The cleavage of OH-C, O-CH2, C-C(phenyl), CH2-O-phenyl and C(phenyl)-Br bonds occurs in the pyrolysis process of PCB, and the cleavage of the O-CH2bonds was a prevailing cracking reaction. About27kinds of organic matters were produced during PCB pyrolysis. Phenol, p-isopropenyl phenol and bisphenol A are the most prominent products.
(4) Batch pyrolysis of PCB waste was conducted on a laboratory scale tubular furnace reactor, the influences of final pyrolysis temperature (FPT) and heating ways on the product yields and product property were investigated. The qualitative analysis of the pyrolysis products were carried out using GC, oxygen bomb calorimeter, FTIR,1H-NMR, and GC-MS. The results indicated that about76.13%solid product,14%pyrolysis liquid and9.86%pyrolysis gas were obtained at600℃. When the FPT above600℃, the char yields reach a constant value. The rise of FPT lead to the change of the ratio of the oil to gas. The yield of pyrolysis liquid obtained at fast pyrolysis was higher than that in slow pyrolysis. The decomposition of the resin binder weaken the binding force between the metal and nonmetal layer, and the metal and nonmetal in PCB achieve100%dissociation at coarse particle size after pyrolysis. The liberated glass fiber was in the form of flaky rather than pulverous. Additionally, the gas products contained combustible components like H2, CO, CH4, heating values of the gases were in the range of11.24-15.21MJ/Nm3. The pyrolysis liquids contained high proportion of phenolic compounds like phenol, isopropylphenol whose heating values were in the range of24.5-27.5MJ/kg.
(5) The reutilization methods of the PCB pyrolysis oil were discussed. As the pyrolysis oil contained high concentration of phenol and phenol derivatives, pyrolysis oil was substituted for phenol as the raw material for preparing pyrolysis oil-based resin, which was then used as a precursor to prepare carbon nanotubes (CNTs) and porous carbon. The CNTs was prepared by catalytic pyrolysis of the oil-based resin with ferrocene at900℃. The porous carbon was prepared from carbonization of KOH-treated resin at700℃. Morphologies and structures of the resulting products were characterized by FTIR,1H-NMR, TG, XRD, SEM, TEM, N2-adsorption isotherm techniques. The results indicated that the oil could be polymerized into pyrolysis oil-based resin with formaldehyde. The aromatic nuclei in the oil were linked by-CH2-O-CH2-or-CH2-after polymerization. The yield of CNTs was56.82%. The products were hollow-centered CNTs with outer diameter of～338nm and wall thickness of-86nm. The length of the prepared tubules reached several micrometers. The prepared resin carbonized to porous carbons at yield of38.05%and its external surface covered cavities. All existing pores were predominance of microporosity. A type I isotherm was observed for the prepared porous carbon. The BET surface area, micropore volume and total pore volume of the porous carbons were1214m2/g,0.41cm3/g and0.64cm3/g, respectively.
废电路板是由铜箔、树脂和增强材料层压而成的复合材料。热解作为一种较新的废电路板处理技术,可使废电路板中的树脂粘结层发生分解,削弱金属与非金属层间的结合力,从而实现金属和非金属层的高效解离；此外,热解过程中产生的热解气和热解油可作为燃气或化工原料回用。根据废电路板热解处理的优点,本论文提出废电路板热解后再进行金属和非金属分离回收的“前置热解法”处理废电路板,通过热解对废电路板进行加热改性处理,以提高废电路板中金属与非金属的破碎解离效率,降低过程能耗。本论文开展的主要研究工作和结论如下：
(1)研究了废电路板的机械解离特性。利用两级破碎方式对废电路板进行机械破碎,了解不同粒径下金属和非金属的解离情况,并对其破碎产物的微观形貌、粒径分布等特性进行研究。研究结果表明,废电路板粉碎过程可分为金属解离和粒径调整两个阶段,机械解离的适宜破碎粒度应控制在0.59-0.15mm之间。废电路板粉碎料经筛分后,金属铜在0.25-0.42mm粒径范围内的含量最高,达32.32%。除C,H,O元素外,废电路板中还主要含有Si,Ca,Cu,Br等元素。不同粒径的废电路板热值在8.07-11.69MJ/kg之间,灰分在53.87-80.45%之间。
(2)开展了大物料量热重实验研究。在自行设计的实验室规模的热重分析装置上进行了较大物料量的热重实验,研究了废电路板、键盘和电线三种典型电子垃圾组分的热解行为和特性,并与常规热重分析仪(微热重)上所得的实验结果进行比较,分析了微热重和大物料量热重两种不同模式下电子垃圾的热解机制,得到了相关的热解动力学参数。研究结果表明,大物料量热重相对于微热重存在热滞后效应,具有较低反应活化能值；分布活化能模型分析结果表明,热解过程中活化能随失重率变化,而不是单一数值。在相同热解条件下,实验所用三种物料的热稳定性顺序为：电线<废电路板<键盘,与其活化能值顺序一致。升温速率和颗粒粒径是影响废电路板热解过程的重要参数。随升温速率的增大,废电路板热解的TG和DTG曲线均向高温区移动；物料粒径的增大会抑制颗粒内部热解反应的进行。
(3)借助TG-FTIR和Py-GC/MS联用技术手段,研究了废电路板热解产物的析出过程以及热解产物类型,并探讨了一些代表性产物的形成机理。研究结果表明,废电路板热解过程中气体产物的形成和释放主要集中在270-400℃,和废电路板样品的热失重温度区间一致。废电路板热解时主要经历三个阶段：①第一阶段,<293℃,主要是小分子气体产物H20, CH4, HBr, CO2, CH3COCH3的析出；②第二阶段,293-400℃树脂的主键大规模降解,释放出大量的大分子量有机物质,如酚类、醛类、酮类等；③第三阶段,>400℃,主要发生焦炭的碳化重整。在热解过程中,废电路板环氧树脂中的OH-C, O-CH2, C-C(phenyl), CH2-O-phenyl, C(phenyl)-Br等键发生了断裂,其中O-CH2的断键反应占主导地位。废电路板热解过程中约产生27种有机物,其中苯酚、异丙烯基苯酚和双酚A是主要的降解产物。
(4)在自行设计的管式炉热解实验台上开展了废电路板批量热解实验,考查了热解终温和加热方式对废电路板热解后得到的残渣、热解液和热解气三种状态产物产率和产物性质的影响,利用氧弹热量计,FTIR,1H-NMR, GC-MS等多种测试手段实现了三种产物的定性分析。分析结果表明,当热解终温为600℃时,可得到76.13%的固体产物,14%的液体产物和9.86%的气体产物。当温度在600℃以上时,固体残渣的产率随温度变化不大,升高温度只是改变油气比。快加热方式下的焦油产率要比慢加热方式下的高。废电路板热解后分层效果明显,经加热改性处理后实现了非金属与金属在大粒径范围下的充分解离。解离后的玻璃纤维呈片状,避免了“过粉碎”,使回收获得的玻璃纤维再利用的可行性大增而使得加工容易。此外,热解过程中产生的热解气体中含有H2,CO, CH4等可燃组分,气体热值在11.24-15.21MJ/Nm3,可作为燃气为热解过程提供能量；热解油中含有大量的酚类化合物,如苯酚、异丙基苯酚等,热值在24.5-27.5MJ/kg之间,可作为燃料油回用,也可从中分离提取高附加值化工单体。
(5)开展了废电路板热解油再资源化利用的研究。根据废电路板热解油富含酚类化合物的特点,提出了以热解油代替苯酚制备酚醛树脂的资源化利用方案,接着以制得的酚醛树脂为前躯体,通过与二茂铁进行催化共热解制备了CNTs,利用KOH(?)活化法制备了多孔炭。运用FTIR,1H-NMR, XRD, SEM, TEM, N2-等温吸附等技术手段对所制备产物的性能进行了分析表征。研究结果表明,废电路板热解油与甲醛在氨催化作用下可聚合成热解油酚醛树脂,聚合后,热解油中的芳环质子通过亚甲基键(-CH2-)或醚键(-CH2-O-CH2-)连接。制得的CNTs的产率为56.82%,具有中空结构,外径～338nm,壁厚～86nm,长度达几微米；制得的多孔炭产率为38.05%,表面存在大量的孔隙结构,孔边缘清晰,对氮气的吸附等温线属于典型的I型吸附等温线,以微孔为主,比表面积达1214m2/g,总孔容积为0.64cm3/g。
Printed circuit board (PCB) waste is a major constituent in electronic waste, which is very difficult to treat compared with other components. Mechanical treatment which employs crushing and separation processes for PCB recovery is becoming more popular and widely used in industrial practice. However, the characteristics of PCB with high hardness and tenacity, compact cohesion between metal and non-metal, could lead to secondary pollution, low efficiency, high-energy consumption and over-pulverization during mechanical crushing process.
PCB waste mainly contains organic materials, metals and glass fiber. Pyrolysis is considered as a promising technique to recycle PCB waste. In pyrolysis process, the organic resin in PCB was decomposed into gas and liquid, thus weakening the binding force between the metal and non-metal layer and achieving efficient dissociation of metal and non-metal. Addtionally, the liquid and gas produced during pyrolysis could be reused as chemical feedstock or fuel. Based on the advantages of PCB pyrolysis listed above, a new process for recycling PCB waste defined as'pre-pyrolysis method'was proposed in this study, that is PCB waste was pyrolyzed, and then the metal separation occurred, with the aim to improve the liberation efficiency of metal and non-metal and reduce the energy consumption. The following works are carried out and the main conclusions are as follows in this dissertation:
(1) The mechanical liberation characteristics of PCB waste were studied. A two-step crushing process which combined with a coarse-crushing step and a fine-pulverizing step was adopted. The liberation situation of the crushed products was observed. Properties of the crushed products, such as morphology, particle size distribution were determined. The results indicated that the crushing process of PCB could be divided into two stages, including metal dissociation and particle size adjustment. The suitable particle size for mechanical dissociation of PCB should be controlled in the range of0.59-0.15mm. The major elements in PCB include Si, Ca, Cu, Br except C, H, O. Copper was the most dominating metal in PCB and reached its maximum content in0.42-0.25mm particle size, about32.32%. The calorific values of PCB in different size changed in the range of8.07-11.69MJ/kg. The ash content was between53.87%and80.45%.
(2) Thermogravimetric analysis on a self-designed laboratory scale thermo-balance (called Macro-TG) with more sample loading was carried out. The pyrolysis characteristics of typical components of e-waste, wire, keyboard and PCB waste, were investigated. The results were compared with those obtained in common thermo-gravimetric measurements (called common TG). The kinetic mechanism function of samples both in Macro-TG and common TG was determined. Additionally, the corresponding kinetic parameters of each sample were also obtained. The results indicated that large particles existed a pyrolysis reaction retardarce compared to fine one. And smaller activation energy were found in pyrolysis reaction occurred in Macro-TG. Distributed activation energy model analysis revealed that activation energy did not show a constant value during the pyrolysis process, and it changed with the rate of weight loss. Due to the composition difference, pyrolysis behaviors of wire, keyboard and PCB waste were different. In the same pyrolysis conditions, the sequence of thermal stability for the three studied species is described as:wire
(4) Batch pyrolysis of PCB waste was conducted on a laboratory scale tubular furnace reactor, the influences of final pyrolysis temperature (FPT) and heating ways on the product yields and product property were investigated. The qualitative analysis of the pyrolysis products were carried out using GC, oxygen bomb calorimeter, FTIR,1H-NMR, and GC-MS. The results indicated that about76.13%solid product,14%pyrolysis liquid and9.86%pyrolysis gas were obtained at600℃. When the FPT above600℃, the char yields reach a constant value. The rise of FPT lead to the change of the ratio of the oil to gas. The yield of pyrolysis liquid obtained at fast pyrolysis was higher than that in slow pyrolysis. The decomposition of the resin binder weaken the binding force between the metal and nonmetal layer, and the metal and nonmetal in PCB achieve100%dissociation at coarse particle size after pyrolysis. The liberated glass fiber was in the form of flaky rather than pulverous. Additionally, the gas products contained combustible components like H2, CO, CH4, heating values of the gases were in the range of11.24-15.21MJ/Nm3. The pyrolysis liquids contained high proportion of phenolic compounds like phenol, isopropylphenol whose heating values were in the range of24.5-27.5MJ/kg.
(5) The reutilization methods of the PCB pyrolysis oil were discussed. As the pyrolysis oil contained high concentration of phenol and phenol derivatives, pyrolysis oil was substituted for phenol as the raw material for preparing pyrolysis oil-based resin, which was then used as a precursor to prepare carbon nanotubes (CNTs) and porous carbon. The CNTs was prepared by catalytic pyrolysis of the oil-based resin with ferrocene at900℃. The porous carbon was prepared from carbonization of KOH-treated resin at700℃. Morphologies and structures of the resulting products were characterized by FTIR,1H-NMR, TG, XRD, SEM, TEM, N2-adsorption isotherm techniques. The results indicated that the oil could be polymerized into pyrolysis oil-based resin with formaldehyde. The aromatic nuclei in the oil were linked by-CH2-O-CH2-or-CH2-after polymerization. The yield of CNTs was56.82%. The products were hollow-centered CNTs with outer diameter of～338nm and wall thickness of-86nm. The length of the prepared tubules reached several micrometers. The prepared resin carbonized to porous carbons at yield of38.05%and its external surface covered cavities. All existing pores were predominance of microporosity. A type I isotherm was observed for the prepared porous carbon. The BET surface area, micropore volume and total pore volume of the porous carbons were1214m2/g,0.41cm3/g and0.64cm3/g, respectively.
引文
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