苯胺生产过程危险介质热危险性实验模拟及其热分解机理研究
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摘要
苯胺是一种重要的有机化工原料,广泛应用于聚氨酯、染料、橡胶制剂、农药、感光化学品、医药及炸药等行业和领域。苯胺生产及其配套装置中使用大量易燃易爆、有毒有害的危险化学品,加上硝化反应和加氢反应生产工艺条件苛刻,装置及控制技术要求严格,使得苯胺生产过程事故具有突发性、灾害性的特点,成为业内公认的高危行业,稍有不慎,就会造成泄漏、爆炸等事故。近年来苯胺生产安全生产事故频频发生,给社会带来极大的灾难和损失。因此有必要系统分析苯胺生产过程存在的危害性,研究苯胺装置中各种危险介质热分解特性及热力学及动力学特性,揭示可能发生的反应性危害事故的致因机理。
本文以苯胺生产过程中存在的硝基苯、苯胺、硫酸、硝酸、硝基酚、硝基苯酚钠、二硝基苯等典型危险介质为危险性分析研究对象,主要开展以下三个部分的研究内容：
(1)使用高斯软件、实验值数据查询及简易估算法,计算和比较了危险介质各种化学键的键离解能,结果表明高斯计键能数据比实验值略低；硝基苯和硝基苯酚的热解和起爆的引发键是C-NO2键；亚硝基苯的热解引发键是C-NO键；苯胺的热解引发键为N-H键。
(2)使用了C80微量量热仪、裂解炉-气相-质谱联用仪(PY-GC-MS)等设备,研究了危险介质及可能混合物的热分解特性,为改善此类物质热化学性和加强苯胺生产本质安全水平提供相应的理论依据。主要从以下三个方面展开：硝基苯和苯胺自身热分解特性研究；硝酸、硫酸及混酸(硝酸／硫酸)对硝基苯和苯胺热分解特性的影响研究；硝基苯生产过程中存在的中间产品和副产品的热分解特性以及它们对硝基苯热分解特性的影响研究。
在硝基苯和苯胺热分解特性研究方面,使用C80微量量热仪通过等速升温实验观察了硝基苯和苯胺的热分解行为,采用气相色谱-质谱联用仪分析了纯品硝基苯、苯胺在不同裂解温度条件下的高速热分解特性及热分解过程中间产物分布情况,揭示了硝基苯和苯胺可能的热分解机理。
在硝酸、硫酸及混酸对硝基苯和苯胺热分解特性影响研究方面,主要使用C80微量量热仪获得含有不同浓度无机酸的混合物样品溶液的热流速曲线,据此求解出混合溶液的化学反应动力学和热力学参数,并结合Semenov热爆炸模型,计算并比较混合物体系的自加速分解温度(SADT),从而研究了硝酸、硫酸及混合酸等杂质对硝基苯、苯胺热分解特性的影响规律。结果表明硝酸、硫酸及混酸等杂质的导入降低了混合物体系的放热开始温度和自加速分解温度,增加了混合物体系的危险性,并揭示了微量硫酸加入硝基苯后生成的不溶杂质的产生机理。
在中间产品和副产品的热分解特性及其对硝基苯热分解特性的影响研究方面,揭示了硝基苯生产过程中间产物和副产物的产生机理,分析了硝基苯生产过程中潜在的危险性。
(3)最后利用计算和实验分析结果,探讨了一起硝基苯生产典型事故的诱发原因及发展机理。事故的诱发原因为进料系统中粗硝基苯受酸类杂质的影响,在长期过热中发生的自加速放热反应过程；事故发展机理为空气进入真空的精馏塔中,氧化其中的硝基苯酚钠等副产品,使其在较低温度下发生自加速分解反应,导致热量积累,最终引起爆炸事故。
Aniline is an important organic chemical raw material and is widely used in the production of polyurethane, dyes, rubber agents, pesticides, photographic chemicals, pharmaceutical and explosives etc. the product process of aniline is regarded as a high-risk unit not only because there are a large amount of inflammable and explosive, toxic and harmful chemicals are used on the aniline production and its supporting device, but also because of the complex processing technology and demanding strict security technology of the nitration and hydrogenation reaction process. In recent years safety accidents of production of aniline occurred frequently, which caused complete catastrophe and loss. So it is necessary to analyze the risk and hazard factor, thermal decomposition characteristics of hazard materials and its thermodynamics and kinetics characteristics of the production process of aniline in order to reveal the mechanism of possible aniline production accident.
In this paper, several hazard chemicals from the aniline production unit were selected as the object of the risk analysis. And the three part of researches were executed as follow:
(1) the calculate and comparison of the BDE of nitrobenzene, aniline, nitrosobenzene, nitrophenol, nitrophenol sodium and dinitrobenzene by the methods of Gaussian03simulate computation, and experimental value database query and estimation method. The results show Gaussian calculations are slightly lower than the experiment query value. The thermolysis trigger bond of nitrobenzene and nitrophenol is C-NO2bond. The trigger bond of nitrosobenzene and aniline are C-NO and N-H bond respectively.
(2) The researches were proceeded, using C80calorimetry, PY-GC-MS, from these three aspects:①Thermal decomposition behavior of nitrobenzene and aniline;②Influence of nitric acid, sulfuric acid and there mixed acid on Thermal decomposition behavior of nitrobenzene and aniline;③Influence of intermediate products and by-products on Thermal decomposition behavior of nitrobenzene and aniline.
In the first research topic, thermal decomposition behavior of nitrobenzene and aniline was observed under the constant heating rate experiment. A GCT gas chromatography-time of flight mass spectrography was used to analyze the thermal decomposition of pure nitrobenzene and aniline under high temperature. The thermal decomposition mechanism of nitrobenzene and its mixture with nitric acid was conjectured.
In the second topic, A CALVET calorimeter C80was used to analyze the thermal behavior of pure nitrobenzene and its mixtures with sulfuric acid and nitric acid. The chemical reaction kinetic parameters such as activation energy, frequency factor, and heat of reaction were calculated based on C80experimental data. Based on theses parameters and the Semenov thermal explosion theory, the self-accelerating decomposition temperature (SADT) of the samples were calculated and compared. The results show that the impurity of sulfuric acid, nitric acid and their mixture acid decrease the Ton-set and SADT and also increase the risk of the nitrobenzene mixture. The mechanism of new insoluble impurity after the sulfuric acid's mixture with nitrobenzene was conjectured.
In the third topic, the thermal decomposition behavior of intermediate products and by-products and their influence on the decomposition behavior of nitrobenzene were researched by using C80calorimetry.
(3) Based on results of above analysis and experiment, the cause and development mechanism of an accident was discussed. The immediate cause is the self-accelerating exothermic reaction process of raw nitrobenzene catalyzed by the impurity of acids. The follow-up mechanism is the high-risk by-products'oxidation by air and the exothermic reaction in the vacuum distillation tower, then the heat accumulation lead to an explosion accident at last.
本文以苯胺生产过程中存在的硝基苯、苯胺、硫酸、硝酸、硝基酚、硝基苯酚钠、二硝基苯等典型危险介质为危险性分析研究对象,主要开展以下三个部分的研究内容：
(1)使用高斯软件、实验值数据查询及简易估算法,计算和比较了危险介质各种化学键的键离解能,结果表明高斯计键能数据比实验值略低；硝基苯和硝基苯酚的热解和起爆的引发键是C-NO2键；亚硝基苯的热解引发键是C-NO键；苯胺的热解引发键为N-H键。
(2)使用了C80微量量热仪、裂解炉-气相-质谱联用仪(PY-GC-MS)等设备,研究了危险介质及可能混合物的热分解特性,为改善此类物质热化学性和加强苯胺生产本质安全水平提供相应的理论依据。主要从以下三个方面展开：硝基苯和苯胺自身热分解特性研究；硝酸、硫酸及混酸(硝酸／硫酸)对硝基苯和苯胺热分解特性的影响研究；硝基苯生产过程中存在的中间产品和副产品的热分解特性以及它们对硝基苯热分解特性的影响研究。
在硝基苯和苯胺热分解特性研究方面,使用C80微量量热仪通过等速升温实验观察了硝基苯和苯胺的热分解行为,采用气相色谱-质谱联用仪分析了纯品硝基苯、苯胺在不同裂解温度条件下的高速热分解特性及热分解过程中间产物分布情况,揭示了硝基苯和苯胺可能的热分解机理。
在硝酸、硫酸及混酸对硝基苯和苯胺热分解特性影响研究方面,主要使用C80微量量热仪获得含有不同浓度无机酸的混合物样品溶液的热流速曲线,据此求解出混合溶液的化学反应动力学和热力学参数,并结合Semenov热爆炸模型,计算并比较混合物体系的自加速分解温度(SADT),从而研究了硝酸、硫酸及混合酸等杂质对硝基苯、苯胺热分解特性的影响规律。结果表明硝酸、硫酸及混酸等杂质的导入降低了混合物体系的放热开始温度和自加速分解温度,增加了混合物体系的危险性,并揭示了微量硫酸加入硝基苯后生成的不溶杂质的产生机理。
在中间产品和副产品的热分解特性及其对硝基苯热分解特性的影响研究方面,揭示了硝基苯生产过程中间产物和副产物的产生机理,分析了硝基苯生产过程中潜在的危险性。
(3)最后利用计算和实验分析结果,探讨了一起硝基苯生产典型事故的诱发原因及发展机理。事故的诱发原因为进料系统中粗硝基苯受酸类杂质的影响,在长期过热中发生的自加速放热反应过程；事故发展机理为空气进入真空的精馏塔中,氧化其中的硝基苯酚钠等副产品,使其在较低温度下发生自加速分解反应,导致热量积累,最终引起爆炸事故。
Aniline is an important organic chemical raw material and is widely used in the production of polyurethane, dyes, rubber agents, pesticides, photographic chemicals, pharmaceutical and explosives etc. the product process of aniline is regarded as a high-risk unit not only because there are a large amount of inflammable and explosive, toxic and harmful chemicals are used on the aniline production and its supporting device, but also because of the complex processing technology and demanding strict security technology of the nitration and hydrogenation reaction process. In recent years safety accidents of production of aniline occurred frequently, which caused complete catastrophe and loss. So it is necessary to analyze the risk and hazard factor, thermal decomposition characteristics of hazard materials and its thermodynamics and kinetics characteristics of the production process of aniline in order to reveal the mechanism of possible aniline production accident.
In this paper, several hazard chemicals from the aniline production unit were selected as the object of the risk analysis. And the three part of researches were executed as follow:
(1) the calculate and comparison of the BDE of nitrobenzene, aniline, nitrosobenzene, nitrophenol, nitrophenol sodium and dinitrobenzene by the methods of Gaussian03simulate computation, and experimental value database query and estimation method. The results show Gaussian calculations are slightly lower than the experiment query value. The thermolysis trigger bond of nitrobenzene and nitrophenol is C-NO2bond. The trigger bond of nitrosobenzene and aniline are C-NO and N-H bond respectively.
(2) The researches were proceeded, using C80calorimetry, PY-GC-MS, from these three aspects:①Thermal decomposition behavior of nitrobenzene and aniline;②Influence of nitric acid, sulfuric acid and there mixed acid on Thermal decomposition behavior of nitrobenzene and aniline;③Influence of intermediate products and by-products on Thermal decomposition behavior of nitrobenzene and aniline.
In the first research topic, thermal decomposition behavior of nitrobenzene and aniline was observed under the constant heating rate experiment. A GCT gas chromatography-time of flight mass spectrography was used to analyze the thermal decomposition of pure nitrobenzene and aniline under high temperature. The thermal decomposition mechanism of nitrobenzene and its mixture with nitric acid was conjectured.
In the second topic, A CALVET calorimeter C80was used to analyze the thermal behavior of pure nitrobenzene and its mixtures with sulfuric acid and nitric acid. The chemical reaction kinetic parameters such as activation energy, frequency factor, and heat of reaction were calculated based on C80experimental data. Based on theses parameters and the Semenov thermal explosion theory, the self-accelerating decomposition temperature (SADT) of the samples were calculated and compared. The results show that the impurity of sulfuric acid, nitric acid and their mixture acid decrease the Ton-set and SADT and also increase the risk of the nitrobenzene mixture. The mechanism of new insoluble impurity after the sulfuric acid's mixture with nitrobenzene was conjectured.
In the third topic, the thermal decomposition behavior of intermediate products and by-products and their influence on the decomposition behavior of nitrobenzene were researched by using C80calorimetry.
(3) Based on results of above analysis and experiment, the cause and development mechanism of an accident was discussed. The immediate cause is the self-accelerating exothermic reaction process of raw nitrobenzene catalyzed by the impurity of acids. The follow-up mechanism is the high-risk by-products'oxidation by air and the exothermic reaction in the vacuum distillation tower, then the heat accumulation lead to an explosion accident at last.
引文
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