硫酸铵结晶过程的研究及其固—液多相流的计算流体力学研究
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摘要
硫酸铵是一种重要的氮肥。工业上硫酸铵通常是由炼钢的焦炉气被硫酸吸收后得到,或者是从生产己内酰胺的副产品中提取。为了改善饱和器结晶硫酸铵过程中,生成的晶体颗粒较小,粒度分布不均匀,色度不理想,并伴有晶体聚结现象发生等问题。本文对硫酸铵结晶工艺进行了系统的研究,并在此基础上,运用计算流体力学方法,对硫酸铵结晶器进行了模拟和优化,并对硫酸铵结晶过程进行了多相模拟。
使用激光法测定了硫酸铵在纯水、硫酸和硫酸铁溶液中的溶解度,以及硫酸铵在纯水、硫酸和硫酸铁溶液中的超溶解度和介稳区。并应用Apelblat双对数经验方程关联了硫酸铵在不同溶剂中的溶解度随温度的变化关系。
采用间歇动态法对硫酸铵蒸发结晶过程的动力学进行了实验测定。测得了硫酸铵晶体的粒度分布,并回归得到了硫酸铵在纯水溶液和原料液中的成核速率及生长速率方程的参数。讨论了溶液酸度以及杂质离子对于结晶动力学的影响。
考察了投加晶种,搅拌速率,蒸发温度,pH值等操作参数,对结晶过程最终产品粒度分布和晶形质量的影响,确定了硫酸铵结晶工艺的最优的操作条件。利用实验得到的物性参数和优化的工艺条件,对实验室尺寸、2.5L小试尺寸和456.78m3工业尺寸进行了硫酸铵的结晶器的流场模拟。考察了不同尺寸结晶器内流体流动的速度大小、方向和剪切率,计算出搅拌桨的理论单位体积输入功率。同时还比较了使用PBT搅拌桨和三叶推进式搅拌桨的流场变化。
在实验的基础上,使用欧拉-欧拉多相模型,在工业尺寸的间歇DTB结晶器中对硫酸铵结晶过程多相流进行了模拟。采用分组法求解硫酸铵结晶过程的粒数衡算方程,建立并推导了关联硫酸铵结晶过程成核速率和生长速率的相间质量传递模型,对硫酸铵的晶体粒度分布,进行了直接的模拟,并得到了工业尺寸DTB结晶器内硫酸铵的粒度分布数据。
依据间歇DTB结晶器欧拉法多相模拟的结果,优化工业尺寸的硫酸铵连续DTB结晶器,并讨论了搅拌速率对连续结晶器内流场的影响。应用拉哥朗日离散相模型,考察了粒度为10μm、800μm和2000μm的硫酸铵晶体在连续结晶器内的悬浮效果。
Ammonium sulphate is an important nitrogenous fertilizer for agriculture. It is usually precipitated from coke oven gas (COG) of steelworks and the byproduct of caprolactam production in industry. There are many problems in precipitating ammonium sulphate from a saturator, such as small crystal size, non-uniform crystal size distribution (CSD), nonstandard chroma and aggregation of crystals. A systematic study on the crystallization process of ammonium sulphate has been performed in this thesis. Computational Fluid Dynamics (CFD) simulations and optimization of the crystallizers have been carried out in conjunction with multi-phase model.
The solubility, supersolubility and metastable zone of ammonium sulfate in pure water, sulfuric acid solution and ferric sulfate solution have been experimentally determined using a laser monitoring observation technique. The experimental data can be correlated with temperature by a double logarithmic empirical equation, Apelblat.
An unsteady state method was employed to measure the nucleation and growth kinetics. The CSD of ammonium sulphate has been measured, consequnently, the paratmeters of equations of nucleation and growth rate in pure water and raw mather liquid has been estimated by regression. The effects of acidity of solution and impurity in the raw material on nucleation and growth rate were investigated.
The effects of parameters, such as seeds added, agitation speed, evaporation temperature, pH of solution etc., on the product quality have been studied. And an optimal operating condition of crystallization of ammonium sulphate has been determined.
CFD modellings, based on the physical properties and optimal operation conditions from experiments, have been carried out to simulate (NH4)2SO4 crystallizations in a pilot scale crystallizer (2.5L) and an industrial crystallizer drafted tube baffled (DTB) (456.78m3). The velocity magnitude, vector and shear rate of fluid inside the different scale crystallizers have been observed, form which the theoretical inputting power of impellers has been calculated. The effects of impeller types (a PBT impeller and a marine propeller) on the processes have also been studied.
Multi-phase CFD simulations of the crystallization process of ammonium sulphate in an industrial batch DTB crystallizer have been performed using Euler-Euler method. A multi-group method has been developed to solve the population balance equation of crystallization, in which an interphase mass transfer model has been established and deduced to involve the nuclear rate and growth rate equations into CFD calculation.
An industrial continuous DTB crystallizer of ammonium sulphate has been optimized through the results of Euler multi-phase simulation of the batch DTB. The flow fields and solid concentrations at different agitation speeds have been studied. Lagrange Discrete phase model has been employed to trace the trajectories of crystal particles at different diameters of 10μm, 800μm and 2000μm in order to understand crystals’bahaviour inside the continuous DTB.
使用激光法测定了硫酸铵在纯水、硫酸和硫酸铁溶液中的溶解度,以及硫酸铵在纯水、硫酸和硫酸铁溶液中的超溶解度和介稳区。并应用Apelblat双对数经验方程关联了硫酸铵在不同溶剂中的溶解度随温度的变化关系。
采用间歇动态法对硫酸铵蒸发结晶过程的动力学进行了实验测定。测得了硫酸铵晶体的粒度分布,并回归得到了硫酸铵在纯水溶液和原料液中的成核速率及生长速率方程的参数。讨论了溶液酸度以及杂质离子对于结晶动力学的影响。
考察了投加晶种,搅拌速率,蒸发温度,pH值等操作参数,对结晶过程最终产品粒度分布和晶形质量的影响,确定了硫酸铵结晶工艺的最优的操作条件。利用实验得到的物性参数和优化的工艺条件,对实验室尺寸、2.5L小试尺寸和456.78m3工业尺寸进行了硫酸铵的结晶器的流场模拟。考察了不同尺寸结晶器内流体流动的速度大小、方向和剪切率,计算出搅拌桨的理论单位体积输入功率。同时还比较了使用PBT搅拌桨和三叶推进式搅拌桨的流场变化。
在实验的基础上,使用欧拉-欧拉多相模型,在工业尺寸的间歇DTB结晶器中对硫酸铵结晶过程多相流进行了模拟。采用分组法求解硫酸铵结晶过程的粒数衡算方程,建立并推导了关联硫酸铵结晶过程成核速率和生长速率的相间质量传递模型,对硫酸铵的晶体粒度分布,进行了直接的模拟,并得到了工业尺寸DTB结晶器内硫酸铵的粒度分布数据。
依据间歇DTB结晶器欧拉法多相模拟的结果,优化工业尺寸的硫酸铵连续DTB结晶器,并讨论了搅拌速率对连续结晶器内流场的影响。应用拉哥朗日离散相模型,考察了粒度为10μm、800μm和2000μm的硫酸铵晶体在连续结晶器内的悬浮效果。
Ammonium sulphate is an important nitrogenous fertilizer for agriculture. It is usually precipitated from coke oven gas (COG) of steelworks and the byproduct of caprolactam production in industry. There are many problems in precipitating ammonium sulphate from a saturator, such as small crystal size, non-uniform crystal size distribution (CSD), nonstandard chroma and aggregation of crystals. A systematic study on the crystallization process of ammonium sulphate has been performed in this thesis. Computational Fluid Dynamics (CFD) simulations and optimization of the crystallizers have been carried out in conjunction with multi-phase model.
The solubility, supersolubility and metastable zone of ammonium sulfate in pure water, sulfuric acid solution and ferric sulfate solution have been experimentally determined using a laser monitoring observation technique. The experimental data can be correlated with temperature by a double logarithmic empirical equation, Apelblat.
An unsteady state method was employed to measure the nucleation and growth kinetics. The CSD of ammonium sulphate has been measured, consequnently, the paratmeters of equations of nucleation and growth rate in pure water and raw mather liquid has been estimated by regression. The effects of acidity of solution and impurity in the raw material on nucleation and growth rate were investigated.
The effects of parameters, such as seeds added, agitation speed, evaporation temperature, pH of solution etc., on the product quality have been studied. And an optimal operating condition of crystallization of ammonium sulphate has been determined.
CFD modellings, based on the physical properties and optimal operation conditions from experiments, have been carried out to simulate (NH4)2SO4 crystallizations in a pilot scale crystallizer (2.5L) and an industrial crystallizer drafted tube baffled (DTB) (456.78m3). The velocity magnitude, vector and shear rate of fluid inside the different scale crystallizers have been observed, form which the theoretical inputting power of impellers has been calculated. The effects of impeller types (a PBT impeller and a marine propeller) on the processes have also been studied.
Multi-phase CFD simulations of the crystallization process of ammonium sulphate in an industrial batch DTB crystallizer have been performed using Euler-Euler method. A multi-group method has been developed to solve the population balance equation of crystallization, in which an interphase mass transfer model has been established and deduced to involve the nuclear rate and growth rate equations into CFD calculation.
An industrial continuous DTB crystallizer of ammonium sulphate has been optimized through the results of Euler multi-phase simulation of the batch DTB. The flow fields and solid concentrations at different agitation speeds have been studied. Lagrange Discrete phase model has been employed to trace the trajectories of crystal particles at different diameters of 10μm, 800μm and 2000μm in order to understand crystals’bahaviour inside the continuous DTB.
引文
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