MINISTRY OF EDUCATION AND TRAINING MINISTRY OF NATIONAL DEFENCE ACADEMY OF MILITARY SCIENCE AND TECHNOLOGY PHAM VAN CHINH INVESTIGATION OF SIMULATION AND OPTIMIZATION FOR NITROGEN GAS GENERATOR USING PRESSURE SWING ADSORPTION PhD THESIS IN TECHNIQUE Hanoi – 2021 MINISTRY OF EDUCATION AND TRAINING MINISTRY OF NATIONAL DEFENCE ACADEMY OF MILITARY SCIENCE AND TECHNOLOGY PHAM VAN CHINH INVESTIGATION OF SIMULATION AND OPTIMIZATION FOR NITROGEN GAS GENERATOR USING PRESSURE SWING ADSORPTION Specialization: Chemical Engineering Code: 9520301 PhD THESIS IN TECHNIQUE Supervisors: Assoc Prof Dr Vu Dinh Tien Dr Le Quang Tuan Hanoi – 2021 i COMMITMENT I hereby declare that this is my own research The research results presented in the thesis and is completely honest Scientific conclusions have never been published in any other work by any authors, reference data are fully cited March, 19th , 2021 PhD Candidate Pham Van Chinh ii ACKNOWLEDGEMENTS First of all, I would like to express my sincere gratitude to my supervisors Associate Professor.Dr Vu Dinh Tien and Dr Le Quang Tuan for their enthusiastically guidance and helping me to complete this thesis They sincere cooperation at every stage of my research work, their valuable advice and assistance always guided me to conduct my research smoothly Secondly, I would like to thank Head of Academy of Military Science and Technology, Training Department of Academy of Military Science and Technology, Head of Institute of Chemistry - Materials, Department of Physical Chemistry, Department of Machinery and Equipment for Chemical Industrial, School of Chemical Engineering, Hanoi University of Technology, Head of Institute of Technology/General Department of Defense Industry, Department of Chemical Technology have always enthusiastically guided and helped me in all aspects of the thesis implementation process Finally, I am in debt of my families, friends and relatives for their love and encouragement and motivation in the process of implementing the thesis PhD Candidate Pham Van Chinh iii TABLE OF CONTENTS Page NOMENCLATURE vi LIST OF TABLES .xi LIST OF FIGURES xii INTRODUCTION CHAPTER I - OVERVIEW 1.1 Air composition and separation technichques 1.1.1 Air composition 1.1.2 Air separation techniques 1.2 Absorbent 17 1.2.1 Introduction of adsorption and adsorbent 17 1.2.2 Molecular sieve adsorbent 19 1.3 Theoretical background of adsorption, desorption and nitrogen gas generator using pressure swing adsorption 25 1.3.1 Theoretical background of adsorption and desorption processes 25 1.3.2 Structure of adsorption column 28 1.3.3 Mechanism of adsorption process .29 1.3.4 Structure and principle of N2 gas generator using pressure swing adsorption 31 1.4 Mathematical model, simulation and optimization for a single fixed bed 34 1.4.1 Mathematical models to describe a single fixed bed 34 1.4.2 Simulation for process and equipment in adsorption 38 1.4.3 Optimization of nitrogen gas generator 39 1.5 The results recently 42 1.5.1 In the world 42 1.5.2 In Vietnam 45 CHAPTER II - OBJECTS AND METHODOLOGY 49 2.1 Object and scope 49 2.2 Materials, chemicals and equipment 49 iv 2.2.1 Carbon Molecular Sieve 49 2.2.2 Analytical equipment for investigating characteristics of adsorbent 49 2.2.3 A complete experimental system is N2 gas generator using PSA cycle 50 2.3 Methodology .50 2.3.1 Introduction .50 2.3.2 General method 51 2.3.3 Studying method about carbon molecular sieve 51 2.3.4 Methods of a building experimental systems for air separator by PSA 52 2.3.5 Determining method of diffusion coefficient 54 2.3.6 Determining method of pressure drop through particle layer of a bed .55 2.3.7 Methods establish a mathematical models to describe a single fixed bed 57 2.3.8 Simulation and optimization of air separator 61 2.3.9 Experimental method .63 2.2.10 Method scale-up of industry 64 CHAPTER III - RESULTS AND DISCUSSION 65 3.1 Specifications of CMS-240 65 3.1.1 Some general specifications of CMS-240 65 3.1.2 Thermal analysis DSC and TG of CMS-240 66 3.1.3 Composition and structure of CMS-240 67 3.1.4 Specific surface of CMS-240 .71 3.2 Manufacturing an experimental system to separate nitrogen gas from air 74 3.2.1 Calculation characteristics and basic dimensions of a single fixed bed 74 3.2.2 Maximum adsorption capacity calculation of a single fixed bed 75 3.2.3 Manufacturing an experimental system to generate nitrogen gas 77 3.3 Calculation, measure and analyze pressure drop of particle layer .83 3.3.1 Pressurization 84 3.3.2 Adsorption 84 3.3.3 Descrease pressure .85 3.3.4 Desorption 85 3.4 Mathematical models describe a single fixed bed by partial pressure 89 v 3.5 Determine velocity and diffusion coefficient 90 3.5.1 Velocity of air flow through a single fixed bed, uc (m/s) 91 3.5.2 Molecular diffusion coefficient, DAB (cm2/s) 91 3.5.3 Determination membrane diffusion coefficient (Knudsen), Dk (cm2/s) 92 3.5.4 Axial diffusion coefficient, DL (cm2/s) 92 3.6 Summary parameters of nitrogen gas generator 95 3.7 Simulation and optimization for nitrogen gas generator 97 3.7.1 Simulation and optimization for a single fixed bed 97 3.7.2 Investigation of simulation and optimization for N2 gas generator using PSA 122 3.7.3 Simulation and experimental comparision of a single fixed bed and two beds 145 3.8 Scale-up industry for equipment and applications 147 3.8.1 Scale-up industry for equipment with different productivity 148 3.8.2 Application of N2 gas generators for production of RDX explosive 152 CONCLUSSIONS 157 THE SCIENTIFIC PUBLICATIONS 161 REFERENCES 163 vi NOMENCLATURE ai,1 Coefficient a1 isothermal bi-Langmuir of component i [-] ai,2 Coefficient a2 isothermal bi-Langmuir of component i [-] bi,1 Coefficient b1 isothermal bi-Langmuir of component i [l.g-1] bi,2 Coefficient b2 isothermal bi-Langmuir of component i [l.g-1] DL Axial diffusion coefficient (adsorption bed) Dia Diameter of bed F Feed raw materials into bed IP1 Isothermal constant in Aspen Adsorption [-] IP2 Isothermal constant in Aspen Adsorption [-] ki Mass transfer coefficient of component i [1s-1] Ki Equilibrium constant of the component i [-] L, H Height of bed [m] Z Axial distance across bed (from top to bottom of bed) [m] ΔP Pressure drop [bar] ΔPi Partial pressure drop of component i [bar] Pe Standard number Peclet of adsorbent particles qi Amount of gas absorbed in adsorbent of component i [g.g-1] q*i Amount of gas absorbed in adsorbent of component i in equilibrium [g.g-1] rp Particle radius [µm] S Cross-sectional area of bed [cm2] Vbed Volume of bed [cm3] U Theoretical velocity of air flow [m.s-1] [cm2.phút-1] [cm] Nm3/ph, L/ph [-] vii VDj Volume of dead zone in bed XFac Volume correction factor [-] ΔPj Pressure drop in partial j [bar] ΔPmax Maximum pressure drop through bed [bar] VT Total empty column volume Vx Empty volume between particles Vp Empty volume inside particles εi Intergranular porosity (internal porosity) [cm3] m3void m3 m void m3 m3void m3 m void m3 m3void m3 m3void m3 εp Porosity inside particles (particle porosity) εt Internal and intergranular porosity (total porosity) µ Viscosity of liquids, gases ψ Coefficient of particle shape ϕ Pressure drop coefficient bar.min cm P Pressure of gas [mmHg, kG/cm2] V Volume of gas [m3] T Absolute temperature of gas [K] Rk Constant of dry air Rhn Constants of water vapor Ci Concentration of component i in gas mixture t Time [cP]3 [-] 2,153 [mmHg.m3/k g.K] 3,461 [mmHg.m3/k g.K] [mol/cm3] [s] viii U Velocity inside bed [m/s] ρb Buld density of adsorbent [g/cm3] ρp Particle density of adsorbent [g/cm3] ρs Solid density of adsorbent [g/cm3] KL Coefficient of thermal conductivity along axis T Temperature [K] Tw Temperature of wall [K] Tatm Temperature of ambient [K] ρg Density of gas [g/cm3] ρb Bulk density of adsorbent [g/cm3] ρw Density of wall material [g/cm3] Cpg Specific heat capacity of gas [J/g.K] Cps Specific heat capacity of adsorbent [J/g.K] Cpw Specific heat capacity of wall material [J/g.K] [J/cm.s.K] [J/mol ] ΔH Thermal effect of adsorption process hi Coefficient of internal heating [J/cm2.K.s] ho Coefficient of external heating [J/cm2.K.s] RBi The inner diameter of bed [cm] RBo Diameter outside of bed [cm] Rp Diameter of particle [cm] Aw Cross-sectional area of wall [cm2] B Parameter equations Langmuir extended [kPa-1] qm Equilibrium parameter for extended Langmuir equation [mol/kg] 157 CONCLUSSIONS * The main results of the thesis The thesis has identified basic characteristics of carbon molecular sieve adsorbent CMS-240 what supplier does not provide such as bulk density, particle density, solid density, particle size distribution, porosity, specific surface, composition and structure of adsorbent by analysis and calculation methods available in Vietnam The results show that the main component of the adsorbent is carbon, cylindrical particles, two-layer structure They are fabricated by impregnation, extrution and drum coating and activation at very high velocity and strictly controlled conditions There are a lot of macropores, mesopores and micropore uniformly, total porosity of the adsorbent is εt = 0.615, specific surface result is determined by calculation according to capacity of bed Sr = 1146 m2/g is quite reliable compared to the actual yield obtained; to has built a completely experimental system of N2 gas generator successfully as pilot scale, with high level of automation to study purposes, It has productivity from 10 L/min to 14 L/min N2 gas ≥ 99.5% at standard conditions It is installed a full range of measuring insttruments (pressure, temperature, flow and concentration sensors) with high accuracy (pressure sensors are installed according to height of bed, mass flow I/O flow sensor and S7-1200 PLC control system, real-time accurate data acquisition monitoring and monitoring (SCADA) can import and export data easy experiments; to calculated, analyzed and measured of pressure drop through particle layer of bed, depending on velocity of gas flow through section of bed and diffusion process in the adsorption and desorption processes In fact, the pressure drop through particle layer is not linearly dependent on velocity in the adsorption and desorption processes due to pore attraction The thesis has established a mathematical model describing rules of adsorption and desorption processes in a single fixed bed according to partial pressure of oxygen depending on time and height of bed with initial condition and boundary conditions as working mode of bed and equipment according to pressure 158 swing adsorption (PSA); to have calculated to determine a set of model parameters to program and simulate the established mathematical model; to has determined the important model parameters by calculation such as the parameters of materials, bed and equipment, equilibrium constants and especially velocity and diffusion coefficient; contemporaneous, to chose a hidden back OLE algorithm to program and simulate a single fixed bed and equipment using Matlab software Sequently, to used Presto software to simulate movement through bed and Aspen Adsorption software to optimize the simulation to achieve the highest productivity, stable product concentration; to studied the rules of changes in technological parameters of pressure, flow and concentration, especially pressure drop and factors affecting productivity and purity product Study on the factors affecting the adsorption process, optimize a single fixed bed to optimize for N2 gas generator on a experimental system that has achieved N2 purity ≥ 99.5% stable with the highest product recovery The mathematical model and simulation results are compatible with the built experimental system, with acceptable errors The thesis has studied industrial scale-up this equipment successfully by calculating and simulating on softwares at different productivity for specific applications in manufacturing and storage Contemporaneous, the thesis has built a complete method by simulating and optimizing for air separators by molecular sieve adsorbent using the adsorption cycles * New contributions of the thesis The thesis has clarified the rule of pressure change in a single fixed bed and N2 gas generator according to the height of bed and time in a working cycle by a mathematical model is described by partial pressure of O2 (component is adsorbed), which is simulated by commercial and self-contained softwares successfully for N2 gas generator is a small capacity (pi-lot) Having studied industry scaled-up for specific applications at suitable capacity successfully, that is achieving good results by calculation combined with simulation of separating technique by adsorption using pressure swing adsorption cycle and carbon molecular sieving adsorption material completely 159 In addition, the thesis has built a systematic approach to simulate, optimize and scale-up of separator using molecular sieve adsorbents and the pressure swing adsorption cycle: from studying characteristics and structure of carbon molecular sieve adsorbents, calculating, design of a single fixed bed or equipment and calculation and analysis of pressure drop, velocity and diffusion coefficient for simulation and optimization of nitrogen gas generator by math model and software This method can be applied to study other separative processes and equipments using molecular sieve adsorbents and adsorption cycles * Further directions Results of the thesis, which shows that investigation of simulation and optimization for separative equipments to separate gase components from its mixture using PSA cycle and molecular sieve adsorption materials Nowaday, this issue is very attractive in terms of science as well as practice and application in practice These research results and methods have great potential for applications in chemical and petrol refinery industries, especially in substance separation techniques Because this method can give results quickly, accuratetly and effectively Some directions can be deployed to solve necessary science and fact problems in as follows, for example: - Investigate on simulating of temperature during adsorption and desorption processes in a single fixed bed of N2 gas generator using pressure swing adsorption - Study on improving product purity and capacity of N2 gas generators using pressure swing adsorption by heterogeneous reaction technique to reduce O2 by H2 gas after nitrogen gas generator - Investigation of simulation and optimization for O2 gas generator using pressure swing adsorption and zeolite 5A, 13X molecular sieve adsorbent to medical, supporting treatment for patients with Covid-19 in Vietnam - Investigation of simulation and optimization for separation processes by PSA, VSA, TSA to separate CO2, H2, C2H5OH gases for fuel preparation, gas processing and other industrial components 160 - Investigation of simulation and optimization for absolute alcohol production equipment by zeolite 3A using pressure swing adsorption Because, simulation is a best method for deploying processes and equipment of chemical engineering This method can give shorten time and high economic efficiency Separation technique using the adsorption cycle and molecular sieve adsorbent is a potential field in the future In addition, this method can be used to simulate and optimize the existing production line and other dissociation processes by Aspen Plus software 161 THE SCIENTIFIC PUBLICATIONS Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2018) Assembling of an experimental system to investigate and optimize of nitrogen gas generator using pressure swing adsorption to separate nitrogen gas from the air Journal of Military Science and Technology (ISSN 1859-1043), no 56, p 157-165 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2018) Design a measuring and control system to investigate and optimize of nitrogen gas generator using pressure swing adsorption Journal of Military Science and Technology (ISSN 1859-1043), special issue 08, p 269-275 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2019) Investigation of Simulation and optimization for nitrogen gas generator using pressure swing adsorption (PSA) by Aspen Adsorption Software Journal of Military Science and Technology (ISSN 1859-1043), no.61, p.140-149 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2019) Study comparative and selection of 4-step and 6-step using pressure swing adsorption to generate N2 gas Journal of Catalytic and Adsorption Viet Nam (ISSN 0866-7411), Volume 8, Issue 3, p25-31 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2019) Study on the carbon molecular sieve adsorbent CMS-240 used in the N2 gas generator Journal of Military Science and Technology (ISSN 1859-1043), no.62, p97-105 Pham Van Chinh, Nguyen Tuan Hieu, Nguyen Tan Y, Nguyen Hoang Nam, Do Van Thom, Ngo Thi Anh, Vu Dinh Tien (2019) Simulation and experiment study of a single fixed bed model of nitrogen gas generator working by pressure swing adsorption Special Issue “Chemical Process Design, Simulation and Optimization” of Journal Processes (ISSN 2227-9717) Processes 2019, (10), 654; https://doi.org/103390/pr7100654 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2019) Establish a mathematical model to describe pressure swing adsorption in N2 gas 162 generator Journal of Military Science and Technology (ISSN 1859-1043), special issue FEE – October, p357-364 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2019) Study on simulation about partial pressure of oxygen in a single fixed bed of nitrogen gas generator using pressure swing adsorption Journal of Military Science and Technology (ISSN 1859-1043), no.64 – December, p132-139 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2019) Study on caculation and simulation of pressure drop through a single fixed bed of nitrogen gas generator using pressure swing adsorption CASEAN-6 Proceedings (ISBN 978-604-913-088-5), p60-66 10 Pham Van Chinh, Nguyen Tuan Hieu, Le Quang Tuan, Vu Dinh Tien (2020) Study on calculating the kinetic parameters of the mathematical model describing the adsorption process of a single fixed bed of N2 gas generator using pressure swing adsorption (PSA) and carbon molecule sieve adsorbent CMS-240 Journal of Catalytic and Adsorption Viet Nam (ISSN 0866-7411), Volume 9, Issue 1, p1-7 163 REFERENCES Vietnamese Võ Văn Bang, Vũ Bá Minh (2004) Q trình thiết bị Cơng nghệ Hóa học & Thực phẩm – Tập 3, Truyền khối Nhà xuất Đại học Quốc gia – TP Hồ Chí Minh Nguyễn Bin (2008) Các trình, thiết bị cơng nghiệp hóa chất thực phẩm, Tập 4: Chưng luyện, hấp thụ, hấp phụ, trích ly, sấy Nhà xuất Khoa học Kỹ thuật Lê Văn Cát (2002) Hấp phụ trao đổi ion trong kỹ thuật xử lý nước & nước thải Nhà xuất Thống kê Trần Đức Cường (1976) Giáo trình Quá trình thiết bị chuyển khối Nhà xuất Đại học Bách khoa Hà nội Đặng Vũ Chí, Hồng Kiều Hưng (2013) 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