净化黄磷尾气部分变换制合成气催化过程研究
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摘要
经过深度净化后的黄磷尾气是一种极佳的碳一化工原料气,利用其富含高浓度CO(>85%)的特点,若能将其通过CO水气变换反应制得高质量的合成气(H2和CO),再用成熟的CO催化加氢技术来生产甲醇,即可减少污染又可实现废物资源回收利用。本文针对黄磷尾气CO变换制甲醇合成气的关键问题,在课题组前期研究基础上,设计制作了一套适合含高浓度CO净化黄磷尾气变换制氢的小试装置,在模拟净化后黄磷尾气为原料气的条件下,对适合高浓度CO变换的B112型工业催化剂的活性影响因素、工艺条件、本征动力学和催化剂PH3中毒等方面进行了系统研究。主要研究成果如下：
(1)选取影响催化剂活性的主要影响因素温度、汽气比及空速作为研究对象,采用单因素实验方法进行实验,考察了温度350-530℃、汽气比0.6-3.3和空速1000～3100 h-1范围内各种操作条件变化对CO变换率的影响规律。实验结果表明在高浓度CO变换反应过程中,由于发生副反应存在一个最佳温度；水蒸气造成催化剂暂时失活,存在一个最佳汽气比；在变换工艺条件下,空速越小,越有利于反应的充分进行。对失活前后的催化剂进行SEM、XPS和XRD表征分析,得出催化剂失活的主要原因是催化剂活性中心被积碳所覆盖。
(2)采用均匀实验设计方法,对变换工艺条件进行深入研究,对实验结果建模分析,并进行反复实验论证,最终确定含高浓度CO净化黄磷尾气变换制氢的最佳工艺条件。通过回归分析,得到影响因素贡献率由大到小顺序为：反应温度>空速>汽气比>C02含量。根据实验结果并结合实际确定最佳工艺条件为：反应温度490℃,空速1000 h-1,汽气比2.5,CO2含量1%,在此条件下,CO变换率大于89%,并能满足催化剂高活性和长寿命的要求,变换率大小可以以此为依据来进行精确调控。
(3)在常压,温度350～450℃和反应器入口气体组成(摩尔分数)CO 0.75～0.95、CO2 0.01～0.10、H2 0.01～0.08,其余为N2的条件下,对高浓度变换催化剂的本征动力学特性进行了系统的实验研究。以目标函数估值法对实验数据进行非线性参数估值,建立了幂函数型高浓度CO变换催化剂常压本征动力学模型,该模型与实验数据吻合较好。
(4)利用HSC Chemistry 5.0热力学计算软件及其附带的热力学数据库软件包,根据Gibbs自由能最小原理,从理论上推断达到平衡时催化剂的活性成分Fe304的PH3中毒过程中可能发生的反应及产物。得出反应生成的焦磷酸盐和积碳会覆盖在催化剂的表面造成催化剂的可逆中毒；而磷铁化合物则使催化剂活性中心被占据,造成其结构的破坏,导致不可逆中毒。
(5)对高浓度CO变换催化剂进行PH3 5.12～955.41 mg/m3浓度的抗毒性实验和PH3 955.41 mg/m3浓度下中毒时间2-50 h的强制性中毒实验,并对强制中毒下的催化剂表面形态、元素组成、物相等进行SEM、XPS和XRD表征,分析其中毒机理。得到工业高浓度CO变换催化剂PH3中毒过程中,PH3的最高允许浓度为400.05 mg/m3,在此浓度以下催化剂活性会受到不同程度的影响,但经过一段时间稳定后,其活性仍能达到变换要求,相反会导致催化剂活性大幅下降；PH3中毒机理的研究结果表明：PH3会加速焦磷酸盐和积碳的产生并覆盖于催化剂的表面,因生成的键较弱,造成可逆性中毒；可溶性磷酸盐会进一步与铁基高温变换催化剂发生反应,生成非溶性的物相与磷铁化合物,使得催化剂活性中心被占据,造成其结构的永久破坏导致不可逆中毒。
Highly purified yellow phosphorus exhaust is excellent good source of Cl gas. Based on the high volume fraction of CO (>85%) and the technology of CO catalytic hydrogenation, the yellow phosphorus exhaust would be developed to directly produce methanol synthesis gas with appropriate ratio of H2/CO. It helps reduce air pollution and reuse resources. In order to prepare the synthesis gas for methanol from purified yellow phosphorus exhaust by water gas shift reaction based on previous work. The activity influencing factors including process conditions, intrinsic kinetics and catalyst poisoning of PH3 of B112 industrial catalyst were further studied under the condition that the purified yellow phosphorus exhaust is the material gas. The main conclusions are as follows:
(1) Accoding to literature review we selected the catalytic activity factors: temperature, steam to gas ratio and space velocity as the object of study; used single-factor experimentwithtemperature 350～530℃, steam to gas ratio from 0.6 to 3.3 and space velocity 1000～3100 h-1 respectively to investigate the patterns of CO conversion rate. Obtained in high concentrations of CO shift reaction process of reaction rate due to the occurrence of side effects and there is an optimum temperature;due to water vapor will cause a temporary deactivation of the catalyst reasons there is an optimum steam-gas ratio; in changing technological conditions in, space velocity the smaller the reactants in the reactor where the longer the stay, the more favorable reaction to the full. Deactivation of the catalyst before and after the SEM, XPS and XRD characterization analysis resulted in a normal catalyst deactivation by carbon deposition on the catalyst active sites.
(2) Study on highly concentrated CO tail gas of purification yellow phosphorus transformation process conditions with B112-type high-temperature shift catalyst based on test results of influnce factors. The results showed that affect its transformation efficiency of the factors in decreasing order as follows:reaction temperature, space velocity, steam to gas ratio, CO2 concentration. The uniform design was applied to optimize reaction conditions, and a regression equation was established to describe the influences of reaction temperature, space velocity, steam to gas ratio, and CO2 content on CO transformation efficiency. The calculation results of the regression equation agree well with the experimental data. Through optimized model and experimental verification, combined with industrial practices, the optimal process conditions for CO transformation efficiency is 88.9 % at 490℃, space velocity 1000h-l,steam to gas ratio and 1% CO2 content by uniform design. It maintains high catalytic activity and logevity requirements, based on which the changing rate can be accurately adjusted.
(3)Under the atmospheric pressure, the temperature at (350～450℃), and the inlet gas fractions as CO 0.75～0.95, CO2 0.01～0.10, H2 0.01～0.08.The rest being N2, this research focuses on the intrinsic kinetics features of high concentration CO shift catalyst with the quartz glass tube reactor. By the use of objective function estimated value method, it nonlinear parameter estimated values the experimental data, and the power function model high concentration CO shift catalyst atmospheric pressure intrinsic kinetics is established. Results from parameter estimation showed high confidence level of the kinetic equations.
(4)Using thermodynamics software HSC Chemistry 5.0 and its Database Software, based on the principle of Gibbs free energy minimum, we inferred theoretically that the compounds, spontaneity and reaction competitive force may produced during the poisoning process of the active constituent Fe3O4 of high concentration CO shift catalyst in PH3.It is observed that the generated pyrophosphate and carbon deposition will cover the outside of catalyst,so that it will bring about the reversible poisoning of catalyst because the phosphorus and iron compound made the active centers of the catalyst occupied, the structure was irreversibly destroyed poisoning.
(5) The poison resistance experiment for high concentration CO shift catalyst in the concentration of PH3 5.12～955.41 mg/m3 and the coerciveness poisoning experiment in the concentration of PH3 955.41 mg/m3 in 2～50 h was conducted. We also present the characterizations of the surface morphology the elemental composition and phase of the enforcement poisoning catalyst by SEM、XPS and XRD, and the mechanism of its poisoning was analyzed. We found that conclude that in the poisoning process of industry high concentration CO shift the maximum allowable concentration of PH3 is 400.05mg/m3. The catalyst activity will be affected below the maximum concentration, but after a while, the catalyst activity will still meet the requirement while reducing the catalyst activity. The mechanism of PH3 poisoning is as following. First, PH3 poisoning will made pyrophosphate and carbon deposition cover the outside of catalyst and the reversible poisoning occurred out of the weakness of chemical bond. Second, the solvable phosphate and iron-based high temperature conversion catalyst will produce some insoluble phase and phosphorus & iron compound, and this made the active centers of the catalyst occupied, the structure destroyed and so that the irreversible poisoning occurred.
(1)选取影响催化剂活性的主要影响因素温度、汽气比及空速作为研究对象,采用单因素实验方法进行实验,考察了温度350-530℃、汽气比0.6-3.3和空速1000～3100 h-1范围内各种操作条件变化对CO变换率的影响规律。实验结果表明在高浓度CO变换反应过程中,由于发生副反应存在一个最佳温度；水蒸气造成催化剂暂时失活,存在一个最佳汽气比；在变换工艺条件下,空速越小,越有利于反应的充分进行。对失活前后的催化剂进行SEM、XPS和XRD表征分析,得出催化剂失活的主要原因是催化剂活性中心被积碳所覆盖。
(2)采用均匀实验设计方法,对变换工艺条件进行深入研究,对实验结果建模分析,并进行反复实验论证,最终确定含高浓度CO净化黄磷尾气变换制氢的最佳工艺条件。通过回归分析,得到影响因素贡献率由大到小顺序为：反应温度>空速>汽气比>C02含量。根据实验结果并结合实际确定最佳工艺条件为：反应温度490℃,空速1000 h-1,汽气比2.5,CO2含量1%,在此条件下,CO变换率大于89%,并能满足催化剂高活性和长寿命的要求,变换率大小可以以此为依据来进行精确调控。
(3)在常压,温度350～450℃和反应器入口气体组成(摩尔分数)CO 0.75～0.95、CO2 0.01～0.10、H2 0.01～0.08,其余为N2的条件下,对高浓度变换催化剂的本征动力学特性进行了系统的实验研究。以目标函数估值法对实验数据进行非线性参数估值,建立了幂函数型高浓度CO变换催化剂常压本征动力学模型,该模型与实验数据吻合较好。
(4)利用HSC Chemistry 5.0热力学计算软件及其附带的热力学数据库软件包,根据Gibbs自由能最小原理,从理论上推断达到平衡时催化剂的活性成分Fe304的PH3中毒过程中可能发生的反应及产物。得出反应生成的焦磷酸盐和积碳会覆盖在催化剂的表面造成催化剂的可逆中毒；而磷铁化合物则使催化剂活性中心被占据,造成其结构的破坏,导致不可逆中毒。
(5)对高浓度CO变换催化剂进行PH3 5.12～955.41 mg/m3浓度的抗毒性实验和PH3 955.41 mg/m3浓度下中毒时间2-50 h的强制性中毒实验,并对强制中毒下的催化剂表面形态、元素组成、物相等进行SEM、XPS和XRD表征,分析其中毒机理。得到工业高浓度CO变换催化剂PH3中毒过程中,PH3的最高允许浓度为400.05 mg/m3,在此浓度以下催化剂活性会受到不同程度的影响,但经过一段时间稳定后,其活性仍能达到变换要求,相反会导致催化剂活性大幅下降；PH3中毒机理的研究结果表明：PH3会加速焦磷酸盐和积碳的产生并覆盖于催化剂的表面,因生成的键较弱,造成可逆性中毒；可溶性磷酸盐会进一步与铁基高温变换催化剂发生反应,生成非溶性的物相与磷铁化合物,使得催化剂活性中心被占据,造成其结构的永久破坏导致不可逆中毒。
Highly purified yellow phosphorus exhaust is excellent good source of Cl gas. Based on the high volume fraction of CO (>85%) and the technology of CO catalytic hydrogenation, the yellow phosphorus exhaust would be developed to directly produce methanol synthesis gas with appropriate ratio of H2/CO. It helps reduce air pollution and reuse resources. In order to prepare the synthesis gas for methanol from purified yellow phosphorus exhaust by water gas shift reaction based on previous work. The activity influencing factors including process conditions, intrinsic kinetics and catalyst poisoning of PH3 of B112 industrial catalyst were further studied under the condition that the purified yellow phosphorus exhaust is the material gas. The main conclusions are as follows:
(1) Accoding to literature review we selected the catalytic activity factors: temperature, steam to gas ratio and space velocity as the object of study; used single-factor experimentwithtemperature 350～530℃, steam to gas ratio from 0.6 to 3.3 and space velocity 1000～3100 h-1 respectively to investigate the patterns of CO conversion rate. Obtained in high concentrations of CO shift reaction process of reaction rate due to the occurrence of side effects and there is an optimum temperature;due to water vapor will cause a temporary deactivation of the catalyst reasons there is an optimum steam-gas ratio; in changing technological conditions in, space velocity the smaller the reactants in the reactor where the longer the stay, the more favorable reaction to the full. Deactivation of the catalyst before and after the SEM, XPS and XRD characterization analysis resulted in a normal catalyst deactivation by carbon deposition on the catalyst active sites.
(2) Study on highly concentrated CO tail gas of purification yellow phosphorus transformation process conditions with B112-type high-temperature shift catalyst based on test results of influnce factors. The results showed that affect its transformation efficiency of the factors in decreasing order as follows:reaction temperature, space velocity, steam to gas ratio, CO2 concentration. The uniform design was applied to optimize reaction conditions, and a regression equation was established to describe the influences of reaction temperature, space velocity, steam to gas ratio, and CO2 content on CO transformation efficiency. The calculation results of the regression equation agree well with the experimental data. Through optimized model and experimental verification, combined with industrial practices, the optimal process conditions for CO transformation efficiency is 88.9 % at 490℃, space velocity 1000h-l,steam to gas ratio and 1% CO2 content by uniform design. It maintains high catalytic activity and logevity requirements, based on which the changing rate can be accurately adjusted.
(3)Under the atmospheric pressure, the temperature at (350～450℃), and the inlet gas fractions as CO 0.75～0.95, CO2 0.01～0.10, H2 0.01～0.08.The rest being N2, this research focuses on the intrinsic kinetics features of high concentration CO shift catalyst with the quartz glass tube reactor. By the use of objective function estimated value method, it nonlinear parameter estimated values the experimental data, and the power function model high concentration CO shift catalyst atmospheric pressure intrinsic kinetics is established. Results from parameter estimation showed high confidence level of the kinetic equations.
(4)Using thermodynamics software HSC Chemistry 5.0 and its Database Software, based on the principle of Gibbs free energy minimum, we inferred theoretically that the compounds, spontaneity and reaction competitive force may produced during the poisoning process of the active constituent Fe3O4 of high concentration CO shift catalyst in PH3.It is observed that the generated pyrophosphate and carbon deposition will cover the outside of catalyst,so that it will bring about the reversible poisoning of catalyst because the phosphorus and iron compound made the active centers of the catalyst occupied, the structure was irreversibly destroyed poisoning.
(5) The poison resistance experiment for high concentration CO shift catalyst in the concentration of PH3 5.12～955.41 mg/m3 and the coerciveness poisoning experiment in the concentration of PH3 955.41 mg/m3 in 2～50 h was conducted. We also present the characterizations of the surface morphology the elemental composition and phase of the enforcement poisoning catalyst by SEM、XPS and XRD, and the mechanism of its poisoning was analyzed. We found that conclude that in the poisoning process of industry high concentration CO shift the maximum allowable concentration of PH3 is 400.05mg/m3. The catalyst activity will be affected below the maximum concentration, but after a while, the catalyst activity will still meet the requirement while reducing the catalyst activity. The mechanism of PH3 poisoning is as following. First, PH3 poisoning will made pyrophosphate and carbon deposition cover the outside of catalyst and the reversible poisoning occurred out of the weakness of chemical bond. Second, the solvable phosphate and iron-based high temperature conversion catalyst will produce some insoluble phase and phosphorus & iron compound, and this made the active centers of the catalyst occupied, the structure destroyed and so that the irreversible poisoning occurred.
引文
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