酸性气体（H_2S，CO_2）的脱除及其气液传质特性的研究
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摘要
H_2S和CO_2是最常见的两种酸性气体，在天然气、炼厂气和合成气等工艺混合气净化过程中，以及工业排放尾气中，H_2S是必须去除的气体，无论是工艺气流再加工后续工段的要求，还是尾气排放环保标准的要求，H_2S的含量都控制十分严格；CO_2是温室气体的主要对象，回收和减少工业尾气中的CO_2排放是缓解“温室效应”有效手段之一。有机醇胺吸收剂脱除酸性气体是目前最有效的方法之一。本工作以气液传质理论为基础，围绕酸性气体(H_2S和CO_2)的脱除，开发高性能复合溶剂为主线，针对不同的混合气对象和性质，采用填料柱和膜接触器为吸收反应器，研究H_2S和CO_2酸性气体传质过程和特性，重点研究：1) 空间位阻胺复合溶液选择性吸收H_2S；2) MDEA基复合溶液和氨基酸基复合溶液的开发，复合溶液在膜接触器中吸收CO_2过程中对传质的增强作用和对疏水性聚丙烯膜结构形态的影响，通过数学模型对传质增强作用和形态影响进行表征。
复合溶液的高选择性可达到节能降耗和获得高纯度气体产品的目的，这在能源紧缺和消耗巨大的今天具有特别重要的意义。研究工作分别采用静态评价装置和动态评价装置，以有机醇胺与酸性气体H_2S和CO_2反应机理为基础，研究添加空间位阻胺的复合溶剂MDEA-TBEE选择性吸收H_2S的性能。在静态装置上，评价复合溶剂MDEA-TBEE的脱除率和选择性性能；在动态装置上，进一步考察各种因素对复合溶剂脱除率和选择性的影响，并与单一溶剂MDEA进行比较；同时，测定总体积传质系数K_Gα值，基于双膜理论，提出一个近似的传质模型计算总体积传质系数K_Gα。结果表明：空间位阻胺是一类具有高选择性的高性能酸性气体吸收剂，在现有的MDEA装置中添加少量位阻胺TBEE能显著地提高溶剂吸收酸性气体的性能，达到节能降耗和提高气体产品纯度的目的；传质模型的计算结果与实验结果符合较好，气速增大，总体积传质系数K_Gα增大；气相H_2S和CO_2浓度增大，总体积传质系数K_Gα减小，在较高的气相CO_2浓度下，模型值与实验值偏差增大，说明在较高的CO_2浓度下，H_2S和CO_2之间的交互作用不能忽视。
开发高效活化剂是酸性气体吸收领域重要的研究方向之一，研究工作采用一乙醇胺(MEA)为原料，氢气为反应氛围，低压下有机气相通过管式催化反应器合成活化剂哌嗪，考察合成催化剂组成和操作参数对合成反应的影响；将合成产物应用于膜吸收装置和再生装置上考察其吸收和解吸CO_2的性能。结果表明：实验室制各的合成催化剂NiCu／SiO_2+微量磷钨酸，具有良好的催化性能，哌嗪选择性达59.6％～61.3％，MEA转化率65％～78％；合成产物无需精馏分离，可直接可作为脱碳活化剂，应用于膜吸收装置以及现有的胺法脱碳装置中。
基于膜接触器气体吸收过程和原理，采用疏水性聚丙烯中空纤维膜组件作为膜接
There are most familiar acidic gases of H_2S and CO_2 in industrial gas mixtures and off-gases. Acidic gas H2S is mainly from gas mixtures in natural gas processing, hydrogen purification, refinery off-gases treating and synthesis gas for ammonia and methanol manufacturing. Impurities H_2S must be removed from the gas mixtures to meet the requirements of sequential processing or environmental regulation. CO_2 is one of primarily greenhouse gases. CO_2 recycle from industrial off-gases can availably control and diminish greenhouse effect. The technology of absorption of acidic gases into aqueous solutions of alkanolamines has been one of preferred approaches in current various technologies. This work mainly dealt with removal of acidic gases of H_2S and CO_2 and development of high performance complex solutions. Based on gas-liquid mass-transfer theory and different property of gas mixtures contained acidic gases, the processes and characteristics of mass transfer of acidic gases were investigated in packed columns and membrane contactors. This work focused on two sections: 1) selective absorption of H_2S from gas mixtures contained CO_2 into aqueous solutions of blended amines of MDEA-TBEE in a packed column. 2) development of high performance complex solutions including MDEA-based and amino-acid-based complex solutions; mass-transfer enhancement of the complex solutions on absorption of CO_2 in a membrane contactor; effect of the complex solutions on hydrophobic polypropylene (PP) membrane configuration; and characterization of the mass-transfer enhancement and the effect of membrane configuration by mathematic models.
High selectivity of blended solutions can bring on decrease of energy consumption and increase of purity of gas products which come from regeneration of blended solutions. So, there is an especial significance in the case of energy sources shortage and huge energy consumption nowadays. Based on reaction mechanism of alkanolamines with acid gases in this work, selective absorption of H_2S from mixed-gas streams into the aqueous solution of blended amines of MDEA-TBEE has been studied using a static and a dynamic evaluation setup, respectively. TBEE, a severe sterically hindered amine, was added into MDEA to form the blended amines. The acidic gases absorption performance into the aqueous solution of blended amines of MDEA-TBEE was compared with that of single amine of MDEA. A variety of effect factors on the performance were investigated by means of evaluation indexes of removal efficiency and selectivity factor. Based on the mass balance, overall mass transfer coefficient, K_Ga was determinated. An approximate model for mass
复合溶液的高选择性可达到节能降耗和获得高纯度气体产品的目的，这在能源紧缺和消耗巨大的今天具有特别重要的意义。研究工作分别采用静态评价装置和动态评价装置，以有机醇胺与酸性气体H_2S和CO_2反应机理为基础，研究添加空间位阻胺的复合溶剂MDEA-TBEE选择性吸收H_2S的性能。在静态装置上，评价复合溶剂MDEA-TBEE的脱除率和选择性性能；在动态装置上，进一步考察各种因素对复合溶剂脱除率和选择性的影响，并与单一溶剂MDEA进行比较；同时，测定总体积传质系数K_Gα值，基于双膜理论，提出一个近似的传质模型计算总体积传质系数K_Gα。结果表明：空间位阻胺是一类具有高选择性的高性能酸性气体吸收剂，在现有的MDEA装置中添加少量位阻胺TBEE能显著地提高溶剂吸收酸性气体的性能，达到节能降耗和提高气体产品纯度的目的；传质模型的计算结果与实验结果符合较好，气速增大，总体积传质系数K_Gα增大；气相H_2S和CO_2浓度增大，总体积传质系数K_Gα减小，在较高的气相CO_2浓度下，模型值与实验值偏差增大，说明在较高的CO_2浓度下，H_2S和CO_2之间的交互作用不能忽视。
开发高效活化剂是酸性气体吸收领域重要的研究方向之一，研究工作采用一乙醇胺(MEA)为原料，氢气为反应氛围，低压下有机气相通过管式催化反应器合成活化剂哌嗪，考察合成催化剂组成和操作参数对合成反应的影响；将合成产物应用于膜吸收装置和再生装置上考察其吸收和解吸CO_2的性能。结果表明：实验室制各的合成催化剂NiCu／SiO_2+微量磷钨酸，具有良好的催化性能，哌嗪选择性达59.6％～61.3％，MEA转化率65％～78％；合成产物无需精馏分离，可直接可作为脱碳活化剂，应用于膜吸收装置以及现有的胺法脱碳装置中。
基于膜接触器气体吸收过程和原理，采用疏水性聚丙烯中空纤维膜组件作为膜接
There are most familiar acidic gases of H_2S and CO_2 in industrial gas mixtures and off-gases. Acidic gas H2S is mainly from gas mixtures in natural gas processing, hydrogen purification, refinery off-gases treating and synthesis gas for ammonia and methanol manufacturing. Impurities H_2S must be removed from the gas mixtures to meet the requirements of sequential processing or environmental regulation. CO_2 is one of primarily greenhouse gases. CO_2 recycle from industrial off-gases can availably control and diminish greenhouse effect. The technology of absorption of acidic gases into aqueous solutions of alkanolamines has been one of preferred approaches in current various technologies. This work mainly dealt with removal of acidic gases of H_2S and CO_2 and development of high performance complex solutions. Based on gas-liquid mass-transfer theory and different property of gas mixtures contained acidic gases, the processes and characteristics of mass transfer of acidic gases were investigated in packed columns and membrane contactors. This work focused on two sections: 1) selective absorption of H_2S from gas mixtures contained CO_2 into aqueous solutions of blended amines of MDEA-TBEE in a packed column. 2) development of high performance complex solutions including MDEA-based and amino-acid-based complex solutions; mass-transfer enhancement of the complex solutions on absorption of CO_2 in a membrane contactor; effect of the complex solutions on hydrophobic polypropylene (PP) membrane configuration; and characterization of the mass-transfer enhancement and the effect of membrane configuration by mathematic models.
High selectivity of blended solutions can bring on decrease of energy consumption and increase of purity of gas products which come from regeneration of blended solutions. So, there is an especial significance in the case of energy sources shortage and huge energy consumption nowadays. Based on reaction mechanism of alkanolamines with acid gases in this work, selective absorption of H_2S from mixed-gas streams into the aqueous solution of blended amines of MDEA-TBEE has been studied using a static and a dynamic evaluation setup, respectively. TBEE, a severe sterically hindered amine, was added into MDEA to form the blended amines. The acidic gases absorption performance into the aqueous solution of blended amines of MDEA-TBEE was compared with that of single amine of MDEA. A variety of effect factors on the performance were investigated by means of evaluation indexes of removal efficiency and selectivity factor. Based on the mass balance, overall mass transfer coefficient, K_Ga was determinated. An approximate model for mass
引文
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