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1、申请硕士学位论文炭基吸附剂选择性催化氧化低温脱硫工艺基础Basic Study on Hot Gas Desulfurization with Carbon Based Sorbents by Selective Catalytic OxidationA Dissertation Submitted toGraduate University of Chinese Academy of SciencesAs a Requirement for Admission to the Master Degreeof Chemical Engineering摘 要我国是世界上以煤为主要能源的大国，煤炭资
2、源丰富而缺油少气，决定了洁净煤技术在我国未来能源发展中重要的战略地位。近年来，以煤气化为基础的联合循环发电技术（IGCC）和多联产技术，因其高效率、低污染越发受到人们的青睐。其中干法热煤气脱硫净化技术是关键组成部分，具有简化工艺流程，降低设备投资，提高系统效率的优点。当前，热煤气脱硫技术和工艺的研究集中在350550之间，而大规模加压气化水洗后煤气温度在 150250，在此低温下，炭基吸附剂选择性氧化脱硫具有一定的应用潜力，然而有关低温炭基吸附剂的性质对脱硫性能的影响及其工艺影响因素等认识尚不深入。因此，本论文旨在考察炭基吸附剂的物理化学性质和工艺条件对低温脱硫及再生性能的影响，为热煤气炭基吸
3、附剂选择性催化氧化脱除 H2S 新工艺的开发提供理论依据和技术支持。论文包括以下六个章节：第一章为文献综述及课题选择。对煤气净化方法中湿法脱硫和干法脱硫的研究及应用现状进行了综述，重点比较了高温干法脱硫和中低温干法脱硫的优缺点，阐明了活性炭（焦）低温脱硫技术的优点，并对目前该技术的发展和研究现状进行了分析，在此基础上提出了课题选择的依据和主要的研究内容。第二章为本研究所用实验装置和主要测试手段。介绍了实验设备、分析方法和表征手段。第三章考察了脱硫剂的物理化学性质对脱硫及再生性能的影响。借助 BET、XPS 等分析表征手段发现脱硫剂的脱硫性能与其 BET 比表面积、微孔面积、总孔容、微孔容等织构
4、参数的大小以及表面含氧官能团的含量相关性较差，而与孔径大小和表面碱性位含量有良好的相关性，即适宜低温脱硫的孔径为34nm，脱硫性能与表面碱性位含量成正比。通过脱硫及再生综合性能考察，发现新华活性焦为较理想的吸附剂。第四章考察了脱硫剂改性后的脱硫及再生性能。由于低温下单一的活性焦活性差、脱硫效率低，因此采用负载金属方法改性，选用含钒溶液以及不同浓度的碳酸钠、碳酸钾溶液作为活性焦的改性浸渍液，改性脱硫剂的脱硫活性明显改善，随着浸渍液浓度的增加，脱硫剂的脱硫效率并未单调增加，而是存在一个最佳浸渍浓度，并且发现浸渍 K、Na 的活性焦的再生性能差，而浸渍 V 的活性焦的再生性能良好。第五章考察了脱硫工
5、艺条件对脱硫剂脱硫性能的影响，包括空速、O2/H2S 比、H2 以及水蒸气含量的影响。实验结果表明，空速在20006000h-1范围内对脱硫精度和硫容影响较小；H2 对脱硫剂脱硫性能有负面影响，而水蒸气对脱硫剂的脱硫性能有促进作用；同时发现 O2/H2S 比值大于化学反应计量系数比时脱硫性能增加较少，而生成 SO2 量增加。最后进行了脱硫剂的循环硫化再生性能评价。第六章为工作总结和展望。对论文工作进行总结，指出了论文的创新点及有待进一步深入研究的问题，指明了今后工作的方向。关键词关键词：热煤气脱硫，活性炭（焦） ，改性，H2S ，催化氧化ABSTRACTBasic Study on Hot G
6、as Desulfurization with Carbon Based Sorbents by Selective Catalytic OxidationWu Bo (Chemical Engineering)Directed by：Professor Huang JiejieChina is one of the largest countries using coal as the chief energy sources. The feature of Chinese energy resource rich in coal but lacking for oil and gas ma
7、kes the clean coal technology an important status for the energy development strategy in the future. In recent years, integrated gasification combined cycle (IGCC) and multi-production technologies based on coal gasification have been attracting more and more attention for the high efficiency and lo
8、w pollution, in which the hot gas desulfurization is a key component with the advantages of simplifying the process, reducing the equipment investment and improving the system efficiency. At present, the desulfurization processes development is focused on the temperature window of 350550. However, f
9、or the larger scale pressurized gasifiers, the gas temperature through water scruber is between 150and 250 that is in the desulfurization temperature range of carbon based sorbents by selective catalytic oxidation; and the effects of the characteristics of sorbents and operating parameters on the de
10、sulfurization performance at lower temperature are less investigated. So the main objective of this research is to have a clear insight of the effects of physical and chemical properties of sorbents and operating parameters on desulfurization and regeneration performance , and to support the process
11、 development.The dissertation includes six chapters：Chapter covers the literature review and research needs. It provides an overview of wet desulfurization and dry desulfurization. And the advantages and disadvantages of the higher temperature desulfurization and the moderate and lower temperature d
12、esulfurization are mainly compared. The potential of developing the hot gas desulfurization with activated carbon (coke) is elucidated. Finally, the objective and the contents of the research are proposed.In chapter , the experimental apparatuses, measurement and analysis methods are described. In c
13、hapter , the effect of physical and chemical properties of sorbents on their desulfurization and regeneration performance is studied. With the aid of BET and XPS, it was found that there is no close relevancy among the desulfurization activity, texture parameters and oxygenic groups, but the desulfu
14、rization activity is dependent on the pore size distribution and alkaline on the surface.Chapter includes the investigation of the effects of sorbent modification on the desulfurization and regeneration properties. The active coke was modified by impregnant of Na2CO3 , K2CO3 with different concentra
15、tions and vanadium-contained solution. It was found that all the modified active cokes have a higher sulfidation activity, but the regeneration performance of the active coke modified by Na2CO3 and K2CO3 is poor, and that modified by vanadium-contained solution is better.Chapter investigates the eff
16、ects of experimental parameters on desulfurization performance, including space velocity, ratio of O2/H2S , H2 and steam. Experimental results showed that the space velocity has less effects on desulfurization precision and sulfur capacity at the range of 20006000h-1. Meanwhile, steam has a positive effect on desulfurization process, but H2 has a negative effect. When the ratio of O2/H2S is more than stoichiometric coefficient of chemical reaction, it has less effect on th
