一氧化碳还原分解磷石膏的研究
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摘要
磷石膏是湿法磷酸生产磷酸过程中的副产品,磷石膏的大量产生和排放对环境造成了潜在危害,同时浪费了巨大的人力、物力和财力。面对经济上的损失和环境保护政策的压力,磷石膏的大规模资源化已成为磷化工行业实现持续发展的关键。磷石膏分解制酸是磷石膏最具潜力的资源化途径之一,但是磷石膏分解温度高能耗大,因此本文主要针对这一问题进行了一氧化碳还原分解磷石膏的研究,为磷石膏的资源化技术提供了基础数据和理论参考。
采用化工热力学软件HSC Chemistry探讨了一氧化碳还原分解磷石膏的热力学行为。利用Reaction Equation模块计算了一氧化碳还原分解磷石膏过程中可能涉及的20个化学反应的摩尔Gibbs自由能变(△rGm)、摩尔焓变(△rHm)、摩尔熵变(△rSm),结果表明这些化学反应大部分为吸热型反应,这也是磷石膏还原分解高能耗的主要原因。利用Equilibrium Composition模块模拟了一氧化碳还原分解磷石膏的热力学平衡组分,认为反应过程中发生的反应大部分是两个甚至更多反应的耦合,而不是彼此独立的逐个发生,其中CaS04(s)+4CO(g)=CaS(s)+4C02(g)与CaS04(s)+1/3CaS(s)=4/3CaO(s)+4/3S02(g)以及CaS04(s)+1/3CaS(s)=4/3CaO(s)与CaS(s)+3C02(g)=CaO(s)+S02(g)+3CO(g)的耦合发生是整个反应过程的主线。
通过扫描电镜(SEM)观察了磷石膏的微观形貌,结果表明磷石膏为不规则的片状颗粒,颗粒间有较强的团聚现象,团聚颗粒有大量的空隙。通过X射线能谱(EDS)分析了磷石膏的元素组成,结果表明磷石膏的主要元素成分为氧、硫、硅和钙4种,但是不同的微区成分也不尽相同。通过X射线粉末衍射(XRD)表征了磷石膏的物相组成,结果表明磷石膏的主要物相为CaS04·2H20,此外还有少量SiO2。通过激光粒度分析仪测定了磷石膏的颗粒粒度,结果表明磷石膏的颗粒粒度近似成正态分布。
利用热分析技术进行了一氧化碳还原分解磷石膏的影响因素,结果表明还原性气氛有利于磷石膏的分解；在一氧化碳气氛中,磷石膏的分解包括两个阶段,第一阶段为磷石膏的脱水阶段,第二阶段为磷石膏的还原分解阶段,5wt.%CaCl2外加剂有利于磷石膏在一氧化碳中的还原分解。
研究了一氧化碳气氛中磷石膏还原分解阶段的动力学行为,认为整个过程为化学反应所控制,动力学方程为动力学补偿效应为lnA=0.1115E+0.0211,反应活化能随磷石膏转化百分率的增大而减小。
Phosphogypsum is a by-product from wet-processes for phosphoric acid. It brings in environmental hazards for massive production and discharge, while wasting enormous human, materials and financial resources. Facing economic loss and environmental double pressure, it is large-scale resource utilization of phosphogypsum that has become the key of realizing sustainable development in phosphorous chemical industry. It is one of the best influential utilization approaches for phosphogypsum to product sulfuric acid through decomposition of it. However, it will need a high temperature and lots of energies for the process, so the decomposition of phosphogypsum under carbon monoxide atmosphere was studied concerning the problem in the paper. The results of the study could provide the basic data and theoretical reference for utilization technology about phosphogypsum.
It was discussed with chemical thermodynamics software HSC Chemistry that thermodynamic behavior of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere. Molar Gibbs free energy change (△,Gm), molar enthalpy change (△rHm) and molar enthalpy change (△rSm) of the twenty probable reactions were all calculated with the reaction equation module of HSC software, which were involved in the reductive decomposition of phosphogypsum under carbon monoxide atmosphere. It shows that these most reactions are endothermic, and that is why the reductive decomposition of phosphogypsum needs lots of energies. It was simulated with the equilibrium composition module of HSC software that the equilibrium composition of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere. It shows that most reactions of the process are coupled with others, instead of one by one being unaided. and what is more, reaction coupled by CaSO4(s)+4CO(g)=CaS(s)+4CO2(g) and CaSO4(s)+1/3CaS(s)= 4/3CaO(s)+4/3SO2(g) and the reaction coupled by CaSO4(s)+1/3CaS(s)=4/3CaO(s) and CaS(s)+3CO2(g)=CaO(s)+SO2(g)+3CO(g) are the main lines.
Microstructure of phosphogypsum was observed with scanning electron microscope (SEM), and it shows that phosphogypsum particles are erose sheets and there are lots of gaps between different particles which are sticked together. Elemental composition of phosphogypsum was achieved with help of Energy Dispersive Spectrometer (EDS), it shows that different regions have different elements with oxygen, Sulfur, silicon and calcium as main elements. Phase of phosphogypsum was characterized with X-ray powder diffractometer (XRD), and it shows CaSO4·2H2O is main and SiO2 is a little in it. Particle size of phosphogypsum was measured with particulate size description analyzer, and it shows that the particle size distribution of phosphogypsum is the approximate normal distribution.
With the help of thermal Analysis, the influencing factors were investigated, and the result shows that reductive atmosphere is of advantage to the reductive decomposition of phosphogypsum; there are two stages in the process of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere, one is the dehydration stage, and the other is the reductive decomposition stage; 5wt.% CaCl2 added is of advantage to the reductive decomposition of phosphogypsum under carbon monoxide atmosphere.
It was investigated that the kinetics behaviors of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere, and it shows that the process is under the control of chemical reaction, and kinetic equation of the reductive decomposition stage isand the kinetic compensation effect isIn,A= 0.1115E+0.0211, and the activation energy value increases the conversion percentage of phosphogypsum.
采用化工热力学软件HSC Chemistry探讨了一氧化碳还原分解磷石膏的热力学行为。利用Reaction Equation模块计算了一氧化碳还原分解磷石膏过程中可能涉及的20个化学反应的摩尔Gibbs自由能变(△rGm)、摩尔焓变(△rHm)、摩尔熵变(△rSm),结果表明这些化学反应大部分为吸热型反应,这也是磷石膏还原分解高能耗的主要原因。利用Equilibrium Composition模块模拟了一氧化碳还原分解磷石膏的热力学平衡组分,认为反应过程中发生的反应大部分是两个甚至更多反应的耦合,而不是彼此独立的逐个发生,其中CaS04(s)+4CO(g)=CaS(s)+4C02(g)与CaS04(s)+1/3CaS(s)=4/3CaO(s)+4/3S02(g)以及CaS04(s)+1/3CaS(s)=4/3CaO(s)与CaS(s)+3C02(g)=CaO(s)+S02(g)+3CO(g)的耦合发生是整个反应过程的主线。
通过扫描电镜(SEM)观察了磷石膏的微观形貌,结果表明磷石膏为不规则的片状颗粒,颗粒间有较强的团聚现象,团聚颗粒有大量的空隙。通过X射线能谱(EDS)分析了磷石膏的元素组成,结果表明磷石膏的主要元素成分为氧、硫、硅和钙4种,但是不同的微区成分也不尽相同。通过X射线粉末衍射(XRD)表征了磷石膏的物相组成,结果表明磷石膏的主要物相为CaS04·2H20,此外还有少量SiO2。通过激光粒度分析仪测定了磷石膏的颗粒粒度,结果表明磷石膏的颗粒粒度近似成正态分布。
利用热分析技术进行了一氧化碳还原分解磷石膏的影响因素,结果表明还原性气氛有利于磷石膏的分解；在一氧化碳气氛中,磷石膏的分解包括两个阶段,第一阶段为磷石膏的脱水阶段,第二阶段为磷石膏的还原分解阶段,5wt.%CaCl2外加剂有利于磷石膏在一氧化碳中的还原分解。
研究了一氧化碳气氛中磷石膏还原分解阶段的动力学行为,认为整个过程为化学反应所控制,动力学方程为动力学补偿效应为lnA=0.1115E+0.0211,反应活化能随磷石膏转化百分率的增大而减小。
Phosphogypsum is a by-product from wet-processes for phosphoric acid. It brings in environmental hazards for massive production and discharge, while wasting enormous human, materials and financial resources. Facing economic loss and environmental double pressure, it is large-scale resource utilization of phosphogypsum that has become the key of realizing sustainable development in phosphorous chemical industry. It is one of the best influential utilization approaches for phosphogypsum to product sulfuric acid through decomposition of it. However, it will need a high temperature and lots of energies for the process, so the decomposition of phosphogypsum under carbon monoxide atmosphere was studied concerning the problem in the paper. The results of the study could provide the basic data and theoretical reference for utilization technology about phosphogypsum.
It was discussed with chemical thermodynamics software HSC Chemistry that thermodynamic behavior of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere. Molar Gibbs free energy change (△,Gm), molar enthalpy change (△rHm) and molar enthalpy change (△rSm) of the twenty probable reactions were all calculated with the reaction equation module of HSC software, which were involved in the reductive decomposition of phosphogypsum under carbon monoxide atmosphere. It shows that these most reactions are endothermic, and that is why the reductive decomposition of phosphogypsum needs lots of energies. It was simulated with the equilibrium composition module of HSC software that the equilibrium composition of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere. It shows that most reactions of the process are coupled with others, instead of one by one being unaided. and what is more, reaction coupled by CaSO4(s)+4CO(g)=CaS(s)+4CO2(g) and CaSO4(s)+1/3CaS(s)= 4/3CaO(s)+4/3SO2(g) and the reaction coupled by CaSO4(s)+1/3CaS(s)=4/3CaO(s) and CaS(s)+3CO2(g)=CaO(s)+SO2(g)+3CO(g) are the main lines.
Microstructure of phosphogypsum was observed with scanning electron microscope (SEM), and it shows that phosphogypsum particles are erose sheets and there are lots of gaps between different particles which are sticked together. Elemental composition of phosphogypsum was achieved with help of Energy Dispersive Spectrometer (EDS), it shows that different regions have different elements with oxygen, Sulfur, silicon and calcium as main elements. Phase of phosphogypsum was characterized with X-ray powder diffractometer (XRD), and it shows CaSO4·2H2O is main and SiO2 is a little in it. Particle size of phosphogypsum was measured with particulate size description analyzer, and it shows that the particle size distribution of phosphogypsum is the approximate normal distribution.
With the help of thermal Analysis, the influencing factors were investigated, and the result shows that reductive atmosphere is of advantage to the reductive decomposition of phosphogypsum; there are two stages in the process of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere, one is the dehydration stage, and the other is the reductive decomposition stage; 5wt.% CaCl2 added is of advantage to the reductive decomposition of phosphogypsum under carbon monoxide atmosphere.
It was investigated that the kinetics behaviors of the reductive decomposition of phosphogypsum under carbon monoxide atmosphere, and it shows that the process is under the control of chemical reaction, and kinetic equation of the reductive decomposition stage isand the kinetic compensation effect isIn,A= 0.1115E+0.0211, and the activation energy value increases the conversion percentage of phosphogypsum.
引文
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[3].杨沛浩.磷石膏的综合利用[J].中国资源综合利用,2009,27(1)：13-15
[4]. Moreira Cavalcanti Canut,Vanusa Maria Feliciano Jacomino et al. Micro structural analyses of phosphogypsum generated by Brazilian fertilizer industries[J].Materials Characterization,2008,59(4):365-373
[5]. Manjit Singh. Treating waste phosphogypsum for cement and plaster manufacture [J].Cement and Concrete Research,2002,32(7):1033-1038
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