新型溶剂高效吸收净化高酸性石油天然气技术开发研究
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摘要
近几年来我国石油天然气工业发展迅速。新开发的川东北普光气田是世界上罕见的高酸性气田。为适应严格的天然气净化要求,确保川气东送的质量,研发我国具有自主知识产权的高选择性吸收脱除H2S、有机硫等杂质组分的溶剂,是中国石油化工股份有限公司确定的“第二道防火墙”。这对于高酸性石油天然气高效脱硫溶剂的国产化,对于我国天然气净化装置“安稳长满优”运行均具有重要意义。
本文以提高有机硫化物在溶剂中的溶解和传质性能为导向,借助热力学和动力学分析以及量子化学理论计算方法,设计了明显能动改进溶剂脱除有机硫性能的复配溶剂UDS组成的基本构成,得到的新型UDS溶剂在高效脱除H2S的同时能够显著提高有机硫脱除效率。
动力学分析和量子化学计算结果表明,UDS溶剂中具有环状结构的MOR组分能够有效促进COS-Am两性离子的脱质子反应,并能够显著提高COS的水解反应速率,改善COS的化学脱除率,SUL组分则对COS和硫醇等有机硫分子具有良好的物理溶解性能,两种因素的共同作用赋予了UDS溶剂良好的有机硫脱除性能。
随后,本文在静态平衡测定装置和填料塔中研究了羰基硫、甲硫醇、乙硫醇、异丙硫醇和正丙硫醇5种模型化合物在UDS溶液中的溶解平衡行为和传质性能。结果表明,在相同的气相分压条件下,各硫醇平衡溶解度的大小顺序为：甲硫醇>乙硫醇>异丙硫醇>正丙硫醇。有机硫化物在UDS溶剂中的亨利常数小于MDEA溶剂.,传质性能因子大于MDEA溶剂,表明有机硫化物在UDS溶剂中的溶解和传质两方面性能均高于MDEA溶剂。
此外,本文还分别研究了UDS溶液对不同金属材质的腐蚀性和抗发泡性能。结果表明,缓蚀剂的添加促进了金属表面钝化膜的形成,有效降低了UDS溶液对不锈钢和碳钢的腐蚀速率,相同条件下的腐蚀性低于MDEA溶液。通过向UDS溶液中添加20 ppm的DF-E后,其抗发泡性能能够得到有效改善。
同时,在不同压力条件下进行了UDS溶剂净化模拟试验和以实际高酸性石油天然气为原料的侧线试验。试验结果均表明,UDS溶剂不仅表现出与国外引进MDEA溶剂同等的H2S脱除效果,而且具有明显优越的有机硫脱除性能,当UDS-F含量在20%以上时,UDS溶剂对有机硫的脱除率较MDEA溶剂高出30-40个百分点。UDS溶剂对CO2的脱除效果同时能够满足净化指标要求。
在模试和侧线试验所取得的良好脱硫效果的基础上,在普光天然气净化厂进行了UDS溶剂的工业应用试验。结果表明,在工业装置目前操作条件下,维持尾气处理单元投用的完整工艺流程,应用UDS和MDEA溶剂,经一级吸收后COS含量分别约为165mg/m3和220 mg/m3。在停用水解反应器的工艺条件下,应用UDS溶剂,净化气中COS含量在135 mg/m3以下,产品气质量满足二类天然气指标要求。UDS溶剂对COS的总体脱除率较MDEA溶剂高出约20～27个百分点。达到相近再生效果的情况下,UDS和MDEA溶剂所需再生蒸汽单耗相当。在相近的操作条件下,应用UDS溶剂的净化装置的闪蒸气流量和闪蒸气中有机硫含量均低于MDEA。
With the fast development of domestic petroleum natural gas industry in the past few years, the Puguang natural gas field which is extremely rare in worldwide gas fields because of its high sour components contents, has been observed and is being developed. As "the second fire wall", the purification solvent with high absorption selectivity for the impurities such as H2S and organosulfurs needs to be developed in order to meet the strict purification requirement. Furthermore, it is of great significance to develop the purification solvent with independent intellectual property rights in the consideration of the localization of desulfurization solvent as well as smooth and steady running of domestic purification plants.
The composition design of a novel solvent oriented by enhancing solubility and mass transfer properties of organosulfurs absorption into solvent was conducted by using thermodynamics and kinetics analysis methods as well as the quantum chemistry calculation method. Based on the basic formation, the novel UDS solvent shows not only the perfect removal performance for H2S but also high removal efficiency for organosulfurs.
The results of dynamics analysis and the quantum chemistry calculation indicate that MOR component with ringed structure can accelerate the zwitterion deprotonation reaction and significantly catalyze the COS hydrolysis reaction, thus, improved the chemical removal efficiency of COS in solvent. Meanwhile, SUL component increases the physical solubility of COS and mercaptans in solvent. As a result, the UDS solvent displays an excellent performance for removing organosulfurs from high sour petroleum natural gas.
Hereafter, the equilibrium behavior and mass transfer property of COS, methyl mercaptan (MeSH), ethyl mercaptan (EtSH), iso-propyl mercaptan (i-PrSH) as well as n-propyl mercaptan (n-PrSH) in UDS solutions were measured at static equilibrium apparatus and the packed column. The solubilities of five organosulfur compounds in UDS solutions show the turns as:MeSH>EtSH>i-PrSH>n-PrSH. As compared with MDEA solvent, the smaller Henry constants and the larger mass transfer factors have been observed for UDS solvent, suggesting the higher solubility and the better transfer performance of organosulfurs absorption in UDS solvent.
In addition, the corrosivity and the foam behavior of UDS solution were investigated. By adding corrosion inhibitor into UDS solvent, the passive film is formed in the surface of the metal and the corrosion rates of stainless steel and carbon steel exposed to UDS solutions are reduced significantly. In the same condition, UDS solution indicates lower corrosivity as compared to MDEA solution. Meanwhile, UDS solution shows the low foaming trend after adding 20 ppm DF-E.
Then, the absorption experiments for purifying high sour petroleum natural gas using UDS solvent were executed at simulation and side-stream absorption units, respectively. The purification results indicate that UDS solvent have equivalent removal performance for H2S and higher removal efficiencies for organosulfurs as compared with MDEA solvent. The organosulfurs removal efficiencies of UDS solvent are 30～40% higher than MDEA solvent as the content of UDS-F component is above 20%. Moreover, UDS solvent also shows the satisfactory removal efficiency for CO2.
Based on the excellent desulfurization performance obtained from simulation and side-stream experiments, the industrial application test of UDS solvent was carried out in Puguang Natural Gas Plant. Under the present operation conditions of industrial plants and keeping the whole purification process, the COS contents in natural gases from the top of the first absorption column are 165 and 220 mg/m3 as using UDS and MDEA, respectively. For UDS solvent, the COS content in purified natural gas is 135 mg/m3 while the hydrolysis reactor is shut down. The quality of purified natural gas met the second-class standard. The organosulfur removal efficiency of UDS solvent is 20～27% higher than that of MDEA solvent. The steam consumption for regenerating UDS solvent seems to be similar to the consumption for MDEA solvent. As compared to MDEA solvent, the flow and organosulfur contents of flashing gas from the purification plant using UDS solvent are lower under the similar conditions.
本文以提高有机硫化物在溶剂中的溶解和传质性能为导向,借助热力学和动力学分析以及量子化学理论计算方法,设计了明显能动改进溶剂脱除有机硫性能的复配溶剂UDS组成的基本构成,得到的新型UDS溶剂在高效脱除H2S的同时能够显著提高有机硫脱除效率。
动力学分析和量子化学计算结果表明,UDS溶剂中具有环状结构的MOR组分能够有效促进COS-Am两性离子的脱质子反应,并能够显著提高COS的水解反应速率,改善COS的化学脱除率,SUL组分则对COS和硫醇等有机硫分子具有良好的物理溶解性能,两种因素的共同作用赋予了UDS溶剂良好的有机硫脱除性能。
随后,本文在静态平衡测定装置和填料塔中研究了羰基硫、甲硫醇、乙硫醇、异丙硫醇和正丙硫醇5种模型化合物在UDS溶液中的溶解平衡行为和传质性能。结果表明,在相同的气相分压条件下,各硫醇平衡溶解度的大小顺序为：甲硫醇>乙硫醇>异丙硫醇>正丙硫醇。有机硫化物在UDS溶剂中的亨利常数小于MDEA溶剂.,传质性能因子大于MDEA溶剂,表明有机硫化物在UDS溶剂中的溶解和传质两方面性能均高于MDEA溶剂。
此外,本文还分别研究了UDS溶液对不同金属材质的腐蚀性和抗发泡性能。结果表明,缓蚀剂的添加促进了金属表面钝化膜的形成,有效降低了UDS溶液对不锈钢和碳钢的腐蚀速率,相同条件下的腐蚀性低于MDEA溶液。通过向UDS溶液中添加20 ppm的DF-E后,其抗发泡性能能够得到有效改善。
同时,在不同压力条件下进行了UDS溶剂净化模拟试验和以实际高酸性石油天然气为原料的侧线试验。试验结果均表明,UDS溶剂不仅表现出与国外引进MDEA溶剂同等的H2S脱除效果,而且具有明显优越的有机硫脱除性能,当UDS-F含量在20%以上时,UDS溶剂对有机硫的脱除率较MDEA溶剂高出30-40个百分点。UDS溶剂对CO2的脱除效果同时能够满足净化指标要求。
在模试和侧线试验所取得的良好脱硫效果的基础上,在普光天然气净化厂进行了UDS溶剂的工业应用试验。结果表明,在工业装置目前操作条件下,维持尾气处理单元投用的完整工艺流程,应用UDS和MDEA溶剂,经一级吸收后COS含量分别约为165mg/m3和220 mg/m3。在停用水解反应器的工艺条件下,应用UDS溶剂,净化气中COS含量在135 mg/m3以下,产品气质量满足二类天然气指标要求。UDS溶剂对COS的总体脱除率较MDEA溶剂高出约20～27个百分点。达到相近再生效果的情况下,UDS和MDEA溶剂所需再生蒸汽单耗相当。在相近的操作条件下,应用UDS溶剂的净化装置的闪蒸气流量和闪蒸气中有机硫含量均低于MDEA。
With the fast development of domestic petroleum natural gas industry in the past few years, the Puguang natural gas field which is extremely rare in worldwide gas fields because of its high sour components contents, has been observed and is being developed. As "the second fire wall", the purification solvent with high absorption selectivity for the impurities such as H2S and organosulfurs needs to be developed in order to meet the strict purification requirement. Furthermore, it is of great significance to develop the purification solvent with independent intellectual property rights in the consideration of the localization of desulfurization solvent as well as smooth and steady running of domestic purification plants.
The composition design of a novel solvent oriented by enhancing solubility and mass transfer properties of organosulfurs absorption into solvent was conducted by using thermodynamics and kinetics analysis methods as well as the quantum chemistry calculation method. Based on the basic formation, the novel UDS solvent shows not only the perfect removal performance for H2S but also high removal efficiency for organosulfurs.
The results of dynamics analysis and the quantum chemistry calculation indicate that MOR component with ringed structure can accelerate the zwitterion deprotonation reaction and significantly catalyze the COS hydrolysis reaction, thus, improved the chemical removal efficiency of COS in solvent. Meanwhile, SUL component increases the physical solubility of COS and mercaptans in solvent. As a result, the UDS solvent displays an excellent performance for removing organosulfurs from high sour petroleum natural gas.
Hereafter, the equilibrium behavior and mass transfer property of COS, methyl mercaptan (MeSH), ethyl mercaptan (EtSH), iso-propyl mercaptan (i-PrSH) as well as n-propyl mercaptan (n-PrSH) in UDS solutions were measured at static equilibrium apparatus and the packed column. The solubilities of five organosulfur compounds in UDS solutions show the turns as:MeSH>EtSH>i-PrSH>n-PrSH. As compared with MDEA solvent, the smaller Henry constants and the larger mass transfer factors have been observed for UDS solvent, suggesting the higher solubility and the better transfer performance of organosulfurs absorption in UDS solvent.
In addition, the corrosivity and the foam behavior of UDS solution were investigated. By adding corrosion inhibitor into UDS solvent, the passive film is formed in the surface of the metal and the corrosion rates of stainless steel and carbon steel exposed to UDS solutions are reduced significantly. In the same condition, UDS solution indicates lower corrosivity as compared to MDEA solution. Meanwhile, UDS solution shows the low foaming trend after adding 20 ppm DF-E.
Then, the absorption experiments for purifying high sour petroleum natural gas using UDS solvent were executed at simulation and side-stream absorption units, respectively. The purification results indicate that UDS solvent have equivalent removal performance for H2S and higher removal efficiencies for organosulfurs as compared with MDEA solvent. The organosulfurs removal efficiencies of UDS solvent are 30～40% higher than MDEA solvent as the content of UDS-F component is above 20%. Moreover, UDS solvent also shows the satisfactory removal efficiency for CO2.
Based on the excellent desulfurization performance obtained from simulation and side-stream experiments, the industrial application test of UDS solvent was carried out in Puguang Natural Gas Plant. Under the present operation conditions of industrial plants and keeping the whole purification process, the COS contents in natural gases from the top of the first absorption column are 165 and 220 mg/m3 as using UDS and MDEA, respectively. For UDS solvent, the COS content in purified natural gas is 135 mg/m3 while the hydrolysis reactor is shut down. The quality of purified natural gas met the second-class standard. The organosulfur removal efficiency of UDS solvent is 20～27% higher than that of MDEA solvent. The steam consumption for regenerating UDS solvent seems to be similar to the consumption for MDEA solvent. As compared to MDEA solvent, the flow and organosulfur contents of flashing gas from the purification plant using UDS solvent are lower under the similar conditions.
引文
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