炼化废液热解与燃烧动力学及结渣形成过程研究
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摘要
化工、冶金、造纸等行业在生产过程中产生大量可生化性低、毒性高、成分复杂的有机废液；如果这些废液未经任何处理而直接排放到环境中,会对生态环境造成严重污染；而采用常规的生化处理手段也很难达到彻底、安全的处理目的。焚烧法作为一种能真正实现资源化、减量化和无害化的处理方式,已经越来越广泛地应用于高浓度含盐工业有机废液的处理中。但是在实际应用中,废液焚烧处理仍面临着一系列的技术和操作难题,这主要体现在：(1)废液成分的复杂性以及各组分含量的波动容易引起焚烧过程的不稳定,从而使得废液中有毒有害物质不能完全分解、降解；同时焚烧过程的波动也容易引起二次污染物(如NOX、SO,)排放的增大,从而再次对环境产生危害。(2)由于生产过程的带入,废液中含有的不可燃无机物质在高温燃烧区释放、转变形成了具有独特物理状态和化学性质的灰形成组分,这些灰形成组分通过高温烟气的夹带进入余热回收通道,从而在受热面(如换热管表面)黏附、累积,形成了能够降低换热效率、引起烟道堵塞甚至停炉的积灰／结渣物,增加了设备运行的非安全因素。
本文以典型化工废液为研究对象,利用实验分析手段和数值计算方法,对化工废液焚烧过程可能出现的技术和操作问题进行深入研究,主要的研究内容和成果如下：
(1)利用热分析法研究了典型化工废液的热解和燃烧特性,并建立了相应的反应动力学模型。结果表明,化工废液具有良好的点火性能,提高升温速率能够改善挥发分的综合释放特性；也能够增强化工废液燃烧的稳定性和燃尽性,从而提高综合燃烧性能。无论热解还是燃烧,在挥发分析出阶段,化学反应的进程与化工废液自身的物性参数有关,而与所处的环境气氛关系不大,热解和燃烧反应的动力学参数比较接近,随着升温速率的增大,挥发分析出阶段的反应活化能逐渐降低；而在反应后期,热解和燃烧反应的活化能均随着升温速率的升高而逐渐增大,说明需要通过较高的反应温度激发并维持；在固定碳燃烧阶段,活化能则再次表现出随着升温速率的提高而降低的特性。
(2)采用XRF、XRD、SEM-EDS、AFT以及STA等实验方法对化工废液焚烧装置典型位置的积灰／结渣物进行了系统分析,获得了灰组分中典型矿物质元素沿烟气流动的沉积分布特征,不同环境下可能出现的矿物质转化和微观形貌改变现象,以及积灰／结渣物在升温过程中的灰熔融特性。结果表明：高温段沉积物总体呈层状结构,沉积粒子的外形由于聚集、烧结的发生而极不规则,主要矿物质相为Na2SO4、NiO和Fe2O3;随着烟气温度的降低,中温段沉积物的微观形貌呈晶枝生长特征,主要矿物质相为低熔点共晶体Na3Fe(SO4)3和Na2Ni(SO4)2·4H2O,并出现了高温腐蚀现象；而在低温段,沉积物呈熔融、熔合特征,主要矿物质为典型的低温腐蚀产物Na3H(SO4)2。灰熔融实验显示：积灰／结渣物的熔融温度沿烟气流动方向呈现了先增长继而逐渐下降的趋势；而根据同步热分析结果,由于中、低温段积灰/结渣物的熔融现象首先发生于含量较多、熔点更低的共晶体矿物质,因此其熔融过程的温度范围在650-710℃之间,比高温段积灰/结渣物的熔融吸热温度范围提前200℃左右。
(3)在对典型化工废液所完成的热重实验基础上,对1台工业规模化工废液焚烧装置建立了三维数值计算模型,对炉内复杂的物理化学反应过程所涉及的相关模型进行了介绍和讨论,分析了关键参数对炉内湍流流动、燃烧和传质传热过程以及NOx和SOx的形成过程、分布情况的影响。结果表明：无论烟气流动流线还是燃烧粒子运动轨迹,均表现出复杂的湍流反应流特征,能够促进废液粒子与燃烧空气的混合,确保废液中有毒有害物质的充分分解。综合考虑化工废液的燃尽特性和NOx、SOx的排放特征,认为过量空气系数为1.25时为最佳燃烧工况,此时烟气在焚烧炉内的平均驻留时间为5.80s,废液粒子的平均驻留时间为5.51s,与烟气的驻留时间相当；同时焚烧装置出口附近的NOx排放浓度较低,SOx排放浓度也处于可接受范围。
(4)分别利用热动力平衡模拟软件FactSage和同步热分析法获得了典型化工废液焚烧产生的富(碱)盐飞灰沉积物的熔融曲线,并分析了两个曲线在评价富(碱)盐飞灰粒子黏附过程的合理性。同时建立了余热锅炉二维数学模型,提出了适用于富(碱)盐型飞灰粒子的黏附沉积模型,预测了不同运行工况下飞灰粒子的沉积、分布特性以及飞灰沉积物对余热锅炉换热过程的影响；通过对典型位置的沉积物进行取样和现场测量,验证本文提出的飞灰沉积模型的可靠性,从而为该类型废液焚烧装置的稳定、安全运行提供有益的参考。粒子尺寸是影响沉积分布的主要因素,大粒子在惯性作用下主要沉积于凝渣管排迎风侧,而小粒子由于受到热泳、湍流波动的影响能够沉积于换热管的迎风和背风侧。
Industries, such as petroleum refineries, petrochemical plants, as well as pulp and paper mills are a major anthropogenic source of hazardous industrial wastewater, which can pose serious and wide-ranging effects to the environment and human health. The incineration method is a well established technology which is often used to dispose industrial wastewater with highly toxicity, poor biodegradability, and complex composition. However, in actual applications, wastewater incineration treatment still faces many technical challenges, which include:(1) Owing to the complexity of chemical compositions and fluctuation of contents, wastewater incineration process is usually not stable, and then it can lead to incomplete thermal degradation of hazardous organic substances, even result in an undesirable increase in emissions of secondary pollutants.(2) Release and transformation of incombustible inorganic substances during wastewater incineration form a large number of ash-forming species which can cause some severe operation-related problems, such as fouling and slagging, which lead to low heat transfer and can, in serious cases, even result in unscheduled shutdown.
In the present work, experimental analysis and numerical studies have been performed to investigate such technical difficulties during wastewater incineration process in order to obtain some useful mechanism conclusions, and they are:
(1) Thermogravimetric analysis has been employed to investigate pyrolysis and combustion characteristics of the typical petrochemical industrial wastewater (PIW) and to establish the kinetic models of reactions. The results indicate that PIW is easy to achieve its ignition, and high heating rate enhances the stability of wastewater pyrolysis and combustion, furthermore improve synthetic combustion performance. The physical properties of wastewater have important role on reaction progress for both pyrolysis and combustion; thus, the kinetic parameters of pyrolysis and combustion are somehow similar. With increasing in heating rate, the activation energy of devolatilization stage decreases gradually, while the activation energy of the second devolatilization stage increases. Furthermore, the activation energy of fixed carbon combustion stage decreases with increasing heating rate.
(2) Ash deposits characterization has been performed to investigate ash transformation and deposition behavior in a large-scale PIW incineration plant using XRF, SEM-EDS, and XRD for elemental composition, morphology, and mineralogy. The results show that this volatile element has a dominated contribution to form varied ash deposits in a wide temperature range. At high temperature section, ash deposits show a typical layer structure with major minerals of Na2SO4、NiO和Fe2O3. In the intermediate temperature range, eutectic mixtures such as Na3Fe(SO4)3and Na2Ni(SO4)2·4H2O which are temperature-dependent are formed in the molten phase and an "evolving" branched structure which indicates the formation of sintered deposits and high temperature corrosion is detected. Acidic salt sodium sesquisulfate is generated at low temperatures and should be responsible for low temperature corrosion. In addition, ash fusion tests (AFTs) show that ash fusion temperatures increase from sample1to sample2first, and then decrease gradually. Simultaneous thermal analysis (STA) indicates that typical melting process of ash samples collected at intermediate-and low-temperature sections is in a temperature range from650-710℃, which is about200℃lower than that of ash sample collected at high-temperature section. It can be explained by the fact that ash deposits at intermediate-and low-temperature sections have a high level of eutectic mixture whose melting temperature is much lower than each component.
(3) The characteristics of the flow, combustion, temperature and NOx/SOx emissions in a large-scale PIW incineration plant have been numerically studied using FLUENT6.3.26. The results show that both air streamlines and combusting particle trajectories illustrate very complicated three-dimensional flow characteristics which promote the mixing of the air and combusting particles, and enhance thermal degradation of hazardous organic substances. On the basis of burn out characteristic as well as NOx and SOx emissions, the optimal operating condition is at ER=1.25. The average residence time of combusting particles and combustion air is5.80s and5.51s, respectively. Meanwhile, NOx emissions at the outlet of incineration plant are also relatively low and SOx emissions are at an acceptable level.
(4) The melting curves of ash particles rich in alkali salts have been obtained by using FactSage thermochemical software and databases as well as XRD coupled with STA. And then numerical simulations of characteristics of ash particle deposition and distribution in an industrial-scale HRSG of the wastewater incinerator have been performed using the proposed numerical deposition model. Field measurements and ash samplings from an industrial-scale HRSG of the wastewater incinerator have been used to validate the model. The predicted results under different operating conditions are in good agreement with the measured data. The results show that ash deposition and distribution have significant particle size and temperature dependence, and high temperature will accelerate ash particle deposition in the furnace.
本文以典型化工废液为研究对象,利用实验分析手段和数值计算方法,对化工废液焚烧过程可能出现的技术和操作问题进行深入研究,主要的研究内容和成果如下：
(1)利用热分析法研究了典型化工废液的热解和燃烧特性,并建立了相应的反应动力学模型。结果表明,化工废液具有良好的点火性能,提高升温速率能够改善挥发分的综合释放特性；也能够增强化工废液燃烧的稳定性和燃尽性,从而提高综合燃烧性能。无论热解还是燃烧,在挥发分析出阶段,化学反应的进程与化工废液自身的物性参数有关,而与所处的环境气氛关系不大,热解和燃烧反应的动力学参数比较接近,随着升温速率的增大,挥发分析出阶段的反应活化能逐渐降低；而在反应后期,热解和燃烧反应的活化能均随着升温速率的升高而逐渐增大,说明需要通过较高的反应温度激发并维持；在固定碳燃烧阶段,活化能则再次表现出随着升温速率的提高而降低的特性。
(2)采用XRF、XRD、SEM-EDS、AFT以及STA等实验方法对化工废液焚烧装置典型位置的积灰／结渣物进行了系统分析,获得了灰组分中典型矿物质元素沿烟气流动的沉积分布特征,不同环境下可能出现的矿物质转化和微观形貌改变现象,以及积灰／结渣物在升温过程中的灰熔融特性。结果表明：高温段沉积物总体呈层状结构,沉积粒子的外形由于聚集、烧结的发生而极不规则,主要矿物质相为Na2SO4、NiO和Fe2O3;随着烟气温度的降低,中温段沉积物的微观形貌呈晶枝生长特征,主要矿物质相为低熔点共晶体Na3Fe(SO4)3和Na2Ni(SO4)2·4H2O,并出现了高温腐蚀现象；而在低温段,沉积物呈熔融、熔合特征,主要矿物质为典型的低温腐蚀产物Na3H(SO4)2。灰熔融实验显示：积灰／结渣物的熔融温度沿烟气流动方向呈现了先增长继而逐渐下降的趋势；而根据同步热分析结果,由于中、低温段积灰/结渣物的熔融现象首先发生于含量较多、熔点更低的共晶体矿物质,因此其熔融过程的温度范围在650-710℃之间,比高温段积灰/结渣物的熔融吸热温度范围提前200℃左右。
(3)在对典型化工废液所完成的热重实验基础上,对1台工业规模化工废液焚烧装置建立了三维数值计算模型,对炉内复杂的物理化学反应过程所涉及的相关模型进行了介绍和讨论,分析了关键参数对炉内湍流流动、燃烧和传质传热过程以及NOx和SOx的形成过程、分布情况的影响。结果表明：无论烟气流动流线还是燃烧粒子运动轨迹,均表现出复杂的湍流反应流特征,能够促进废液粒子与燃烧空气的混合,确保废液中有毒有害物质的充分分解。综合考虑化工废液的燃尽特性和NOx、SOx的排放特征,认为过量空气系数为1.25时为最佳燃烧工况,此时烟气在焚烧炉内的平均驻留时间为5.80s,废液粒子的平均驻留时间为5.51s,与烟气的驻留时间相当；同时焚烧装置出口附近的NOx排放浓度较低,SOx排放浓度也处于可接受范围。
(4)分别利用热动力平衡模拟软件FactSage和同步热分析法获得了典型化工废液焚烧产生的富(碱)盐飞灰沉积物的熔融曲线,并分析了两个曲线在评价富(碱)盐飞灰粒子黏附过程的合理性。同时建立了余热锅炉二维数学模型,提出了适用于富(碱)盐型飞灰粒子的黏附沉积模型,预测了不同运行工况下飞灰粒子的沉积、分布特性以及飞灰沉积物对余热锅炉换热过程的影响；通过对典型位置的沉积物进行取样和现场测量,验证本文提出的飞灰沉积模型的可靠性,从而为该类型废液焚烧装置的稳定、安全运行提供有益的参考。粒子尺寸是影响沉积分布的主要因素,大粒子在惯性作用下主要沉积于凝渣管排迎风侧,而小粒子由于受到热泳、湍流波动的影响能够沉积于换热管的迎风和背风侧。
Industries, such as petroleum refineries, petrochemical plants, as well as pulp and paper mills are a major anthropogenic source of hazardous industrial wastewater, which can pose serious and wide-ranging effects to the environment and human health. The incineration method is a well established technology which is often used to dispose industrial wastewater with highly toxicity, poor biodegradability, and complex composition. However, in actual applications, wastewater incineration treatment still faces many technical challenges, which include:(1) Owing to the complexity of chemical compositions and fluctuation of contents, wastewater incineration process is usually not stable, and then it can lead to incomplete thermal degradation of hazardous organic substances, even result in an undesirable increase in emissions of secondary pollutants.(2) Release and transformation of incombustible inorganic substances during wastewater incineration form a large number of ash-forming species which can cause some severe operation-related problems, such as fouling and slagging, which lead to low heat transfer and can, in serious cases, even result in unscheduled shutdown.
In the present work, experimental analysis and numerical studies have been performed to investigate such technical difficulties during wastewater incineration process in order to obtain some useful mechanism conclusions, and they are:
(1) Thermogravimetric analysis has been employed to investigate pyrolysis and combustion characteristics of the typical petrochemical industrial wastewater (PIW) and to establish the kinetic models of reactions. The results indicate that PIW is easy to achieve its ignition, and high heating rate enhances the stability of wastewater pyrolysis and combustion, furthermore improve synthetic combustion performance. The physical properties of wastewater have important role on reaction progress for both pyrolysis and combustion; thus, the kinetic parameters of pyrolysis and combustion are somehow similar. With increasing in heating rate, the activation energy of devolatilization stage decreases gradually, while the activation energy of the second devolatilization stage increases. Furthermore, the activation energy of fixed carbon combustion stage decreases with increasing heating rate.
(2) Ash deposits characterization has been performed to investigate ash transformation and deposition behavior in a large-scale PIW incineration plant using XRF, SEM-EDS, and XRD for elemental composition, morphology, and mineralogy. The results show that this volatile element has a dominated contribution to form varied ash deposits in a wide temperature range. At high temperature section, ash deposits show a typical layer structure with major minerals of Na2SO4、NiO和Fe2O3. In the intermediate temperature range, eutectic mixtures such as Na3Fe(SO4)3and Na2Ni(SO4)2·4H2O which are temperature-dependent are formed in the molten phase and an "evolving" branched structure which indicates the formation of sintered deposits and high temperature corrosion is detected. Acidic salt sodium sesquisulfate is generated at low temperatures and should be responsible for low temperature corrosion. In addition, ash fusion tests (AFTs) show that ash fusion temperatures increase from sample1to sample2first, and then decrease gradually. Simultaneous thermal analysis (STA) indicates that typical melting process of ash samples collected at intermediate-and low-temperature sections is in a temperature range from650-710℃, which is about200℃lower than that of ash sample collected at high-temperature section. It can be explained by the fact that ash deposits at intermediate-and low-temperature sections have a high level of eutectic mixture whose melting temperature is much lower than each component.
(3) The characteristics of the flow, combustion, temperature and NOx/SOx emissions in a large-scale PIW incineration plant have been numerically studied using FLUENT6.3.26. The results show that both air streamlines and combusting particle trajectories illustrate very complicated three-dimensional flow characteristics which promote the mixing of the air and combusting particles, and enhance thermal degradation of hazardous organic substances. On the basis of burn out characteristic as well as NOx and SOx emissions, the optimal operating condition is at ER=1.25. The average residence time of combusting particles and combustion air is5.80s and5.51s, respectively. Meanwhile, NOx emissions at the outlet of incineration plant are also relatively low and SOx emissions are at an acceptable level.
(4) The melting curves of ash particles rich in alkali salts have been obtained by using FactSage thermochemical software and databases as well as XRD coupled with STA. And then numerical simulations of characteristics of ash particle deposition and distribution in an industrial-scale HRSG of the wastewater incinerator have been performed using the proposed numerical deposition model. Field measurements and ash samplings from an industrial-scale HRSG of the wastewater incinerator have been used to validate the model. The predicted results under different operating conditions are in good agreement with the measured data. The results show that ash deposition and distribution have significant particle size and temperature dependence, and high temperature will accelerate ash particle deposition in the furnace.
引文
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