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El. knyga: Experimental Methods for Evaluation of Hydrotreating Catalysts

Edited by (Mexican Institute of Petroleum, Mexico City)
  • Formatas: PDF+DRM
  • Išleidimo metai: 10-Mar-2020
  • Leidėjas: John Wiley & Sons Inc
  • Kalba: eng
  • ISBN-13: 9781119518013
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Experimental Methods for Evaluation of Hydrotreating CatalystsDidesnis paveikslėlis
  • Formatas: PDF+DRM
  • Išleidimo metai: 10-Mar-2020
  • Leidėjas: John Wiley & Sons Inc
  • Kalba: eng
  • ISBN-13: 9781119518013
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"Experimental methods for evaluation of hydrotreating catalysts focuses on detailed descriptions of experimental procedures that are used for testing and screening of hydrotreating catalysts, making emphasis on step-by-step methodologies, calculations, treatment of data, and interpretation of results. It describes experimental procedure at different levels of experimentation, such as: glass reactor, batch reactor, small-scale tubular reactor, medium-scale tubular reactor, large-scale tubular reactor, continuous stirred tank reactor, and ebullated-bed reactor, using model compounds, middle distillates and heavy oil. Each chapter includes detailed description of the experimental setup and procedure, analytical methods, calculations, examples of catalyst testing, characterization of catalyst and liquid products, and interpretation of results. Experimental methods for evaluation of hydrotreating catalysts is oriented to be a reference book for researchers, PhD students, post-doctorate students, catalyst manufacturers, professors, to help them carry out proper experiments for catalyst evaluation at different reaction scales, as well as to cover part of the content of a series of courses of different carriers at undergraduate and postgraduate levels"--

Presents detailed information and study cases on experiments on hydrotreating catalysts for the petroleum industry

Catalytic hydrotreating (HDT) is a process used in the petroleum refining industry for upgrading hydrocarbon streams—removing impurities, eliminating metals, converting asphaltene molecules, and hydrocracking heavy fractions. The major applications of HDT in refinery operations include feed pretreatment for conversion processes, post-hydrotreating distillates, and upgrading heavy crude oils. Designing HDT processes and catalysts for successful commercial application requires experimental studies based on appropriate methodologies. Experimental Methods for Evaluation of Hydrotreating Catalysts provides detailed descriptions of experiments in different reaction scales for studying the hydrotreating of various petroleum distillates. 

Emphasizing step-by-step methodologies in each level of experimentation, this comprehensive volume presents numerous examples of evaluation methods, operating conditions, reactor and catalyst types, and process configurations. In-depth chapters describe experimental setup and procedure, analytical methods, calculations, testing and characterization of catalyst and liquid products, and interpretation of experiment data and results. The text describes experimental procedure at different levels of experimentation—glass reactor, batch reactor, continuous stirred tank reactor, and multiple scales of tubular reactors—using model compounds, middle distillates and heavy oil. This authoritative volume:

  • Introduces experimental setups used for conducting research studies, such as type of operation, selection of reactor, and analysis of products
  • Features examples focused on the evaluation of different reaction parameters and catalysts with a variety of petroleum feedstocks
  • Provides experimental data collected from different reaction scales
  • Includes experiments for determining mass transfer limitations and deviation from ideality of flow pattern
  • Presents contributions from leading scientists and researchers in the field of petroleum refining 

Experimental Methods for Evaluation of Hydrotreating Catalysts is an indispensable reference for researchers and professionals working in the area of catalytic hydrotreating, as well as an ideal textbook for courses in fields such as chemical engineering, petrochemical engineering, and biotechnology.

About the Editor xi
Notes on Contributors xiii
Preface xvii
1 Experimental Setups for Hydrotreating of Petroleum Fractions
1(10)
Jorge Ancheyta
1.1 Introduction
1(1)
1.2 Type of Operation
2(1)
1.3 Selection of the Reactor
2(1)
1.4 Experimental Considerations for the Operation of the Laboratory Reactor
3(2)
1.5 Considerations for Experimental Reactor Configuration
5(2)
1.5.1 Configuration for Batch and Semi-batch Operation Modes
5(1)
1.5.2 Configuration for Continuous Operation
6(1)
1.6 Analysis of Products
7(2)
1.6.1 Gases
7(1)
1.6.2 Liquids
7(2)
1.7 Conclusions
9(1)
References
9(2)
2 Experimentation in Glass Reactors with Model Compounds
11(36)
Mohan S. Rana
Pablo Torres-Mancera
Jorge Ancheyta
2.1 Introduction
11(3)
2.2 Glass Microreactor Design and Experimentation
14(6)
2.2.1 Experimental Setup for Catalyst Evaluation
15(2)
2.2.2 Measurement of Gas Flow
17(1)
2.2.3 Control of Gas Flow
17(1)
2.2.4 Determination of the Molar Concentration of Model Molecules Before Reaction
17(1)
2.2.5 Calculation of Partial Pressure of Thiophene under Given Conditions
18(1)
2.2.6 Reactor and Furnace Section
19(1)
2.2.7 Heating Lines (After the Reactor)
19(1)
2.2.8 Analysis (FID and TCD)
19(1)
2.3 Basic Concepts of the Reactor
20(8)
2.3.1 Reactor Model Considerations
20(2)
2.3.2 Diffusion Limitations (Heat and Mass Transfer)
22(4)
2.3.3 Experimental Procedure for HDS Thiophene Testing at Atmospheric Pressure
26(2)
2.4 Model Compound Testing Focused on Support Properties
28(1)
2.5 Model Compounds Hydro treating Setup
28(3)
2.5.1 Catalyst Activation
28(1)
2.5.2 Thiophene HDS
29(2)
2.6 Catalyst Composition and its Role in Catalytic Activity
31(2)
2.7 Chemisorption and Measurement of Catalytic Site Experiments
33(4)
2.7.1 Experimental Technology
34(1)
2.7.2 LTOC Experiments
34(3)
2.8 Relation Between Activity and Characterization
37(1)
2.9 Calculation of the Kinetics Rate and Intrinsic Activity
38(1)
2.10 Additional Data for Catalytic Activity in a Glass Reactor
39(2)
2.11 Conclusions
41(1)
References
42(5)
3 Experimentation with Model Molecules in Batch Reactors
47(20)
Pablo Torres-Mancera
Patricia Rayo
Jorge Ancheyta
3.1 Introduction
47(1)
3.2 Considerations in Heterogeneous Catalytic Reactions
47(6)
3.2.1 Integral Method
49(1)
3.2.2 Differential Method
50(2)
3.2.3 Effect of Temperature
52(1)
3.2.4 Mass Transfer Effects
52(1)
3.3 Catalytic Reaction Running Methodology
53(3)
3.3.1 Catalyst Particle Size
54(1)
3.3.2 Sulfiding Step
54(1)
3.3.3 Reaction Test
55(1)
3.3.4 Analysis of the Reaction Samples
55(1)
3.4 Example of HDS of a Model Compound
56(8)
3.4.1 Reaction
56(1)
3.4.2 Analysis of Reaction Samples
56(1)
3.4.3 Catalytic Activity
56(3)
3.4.4 Reaction Network
59(1)
3.4.5 Product Distribution
60(1)
3.4.6 Selectivity Analysis
61(1)
3.4.7 Deep Kinetic Analysis
61(2)
3.4.8 Analysis of Mass Transfer Effects
63(1)
3.5 Conclusions
64(1)
References
65(2)
4 Experimentation in Batch Reactors with Petroleum Distillates
67(30)
Gustavo Marroquin
Jose A.D. Munoz
Jorge Ancheyta
4.1 Introduction
67(1)
4.2 Batch Reactors
68(10)
4.2.1 Main Features
68(1)
4.2.2 Use of Batch Reactors for Hydrotreating
69(1)
4.2.3 Modes of Operation
70(1)
4.2.4 Data Collection
71(6)
4.2.5 Analysis of Experimental Data
77(1)
4.2.6 Profiles in the Reactor
77(1)
4.3 Experimental Study to Determine the Effectiveness Factors of Catalysts Using Petroleum Distillate
78(6)
4.3.1 Experimental
78(1)
4.3.2 Results and Discussion
79(5)
4.4 Activation Energies of Petroleum Distillates During HDS Reactions
84(9)
4.4.1 Experimental
85(1)
4.4.2 Results and Discussion
85(8)
4.4.3 Effect of Feed Properties on Kinetic Parameters
93(1)
4.5 Conclusions
93(1)
References
94(3)
5 Experimentation with Heavy Oil in Batch Reactors
97(24)
Samir K. Maity
Guillermo Centeno
Jorge Ancheyta
5.1 Introduction
97(4)
5.2 Catalysts Used in Batch Reactors
101(2)
5.2.1 Preparation of Supports
101(1)
5.2.2 Preparation of Catalysts by Impregnation
102(1)
5.3 Activation of Hydrotreating Catalysts
103(1)
5.4 Experimental Setup for a Batch Reactor
104(7)
5.4.1 Loading of Feed into the Batch Reactor
104(1)
5.4.2 Catalyst Transfer to the Batch Reactor
105(1)
5.4.3 Preparation of Experimental Setup and Leak Test
106(1)
5.4.4 Pressuring Reactor with Hydrogen Gas
106(1)
5.4.5 Test Run
106(1)
5.4.6 Sample Withdraw During Runs at Different Time Intervals
107(1)
5.4.7 Gas Sample Analysis
108(1)
5.4.8 Separation of Solid Catalyst from the Liquid Sample
108(1)
5.4.9 Cleaning of Solid Catalyst from Coke and Trapped Liquid
108(2)
5.4.10 Analysis of Liquid Sample
110(1)
5.4.11 Analysis of Coke and Used Catalyst
110(1)
5.4.12 Cleaning the Reactor for the Next Experiment
110(1)
5.5 Some Results Obtained in Batch Reactors
111(3)
5.5.1 Measurement of Product Distribution by TGA
111(1)
5.5.2 Effect of Operating Conditions on Hydrotreating Activities
112(2)
5.6 Advantages and Disadvantages of Batch Reactors
114(2)
5.6.1 Advantages
114(2)
5.6.2 Disadvantages
116(1)
5.7 Conclusions
116(1)
References
117(4)
6 Experimentation in Small-scale Continuous Fixed-bed Tubular Reactors
121(70)
Patricia Rayo
Fernando Alonso
Jorge Ancheyta
6.1 Introduction
121(1)
6.2 Experimental Setup
122(8)
6.2.1 Small-scale Unit
122(2)
6.2.2 Catalyst Loading
124(1)
6.2.3 Catalyst Activation
125(1)
6.2.4 Unloading of Catalyst
125(1)
6.2.5 Characterization of Feed and Liquid Products
125(2)
6.2.6 Characterization of Supports, and Fresh and Spent Catalysts
127(3)
6.3 Effect of Diluent Composition
130(6)
6.3.1 Experimental
130(1)
6.3.2 Results and Discussion
130(6)
6.3.3 Conclusions
136(1)
6.4 Effect of Support
136(15)
6.4.1 Synthesis of Supports
137(1)
6.4.2 Results and Discussion
138(11)
6.4.3 Conclusions
149(2)
6.5 Effect of Support Modification
151(13)
6.5.1 Synthesis of Supports
152(1)
6.5.2 Results and Discussion
153(10)
6.5.3 Conclusions
163(1)
6.6 Effect of the Additive Incorporation Method
164(14)
6.6.1 Feed and Synthesis of Supports and Catalysts
164(2)
6.6.2 Results and Discussion
166(11)
6.6.3 Conclusions
177(1)
6.7 Effect of the Incorporation Method of Ti
178(9)
6.7.1 Feed and Synthesis of Supports and Catalysts
179(1)
6.7.2 Results and Discussion
180(6)
6.7.3 Conclusions
186(1)
References
187(4)
7 Experimentation in Medium-scale Continuous Fixed-bed Tubular Reactors
191(60)
Fernando Alonso
Gustavo Marroquin
Jorge Ancheyta
7.1 Introduction
191(1)
7.2 Description of Experimental Setup and Procedure
192(9)
7.2.1 Feedstock and Characterization
192(1)
1.2.2 Description of the Pilot Plant
192(9)
7.3 Mass Transfer Limitations in TBRs
201(13)
7.3.1 Materials
201(1)
7.3.2 Catalyst and Activation Procedure
201(1)
7.3.3 Reaction Conditions
201(2)
7.3.4 Results
203(10)
7.3.5 Conclusions
213(1)
7.4 Hydrotreating of Heavy Crude Oil
214(11)
7.4.1 Materials
214(1)
7.4.2 Operating Conditions
215(1)
7.4.3 Analysis of Products
216(1)
7.4.4 Results
217(7)
7.4.5 Conclusions
224(1)
7.5 Hydrodemetallization of Heavy Crude Oil with Ni-Mo/Alumina Catalysts
225(11)
7.5.1 Materials
225(1)
7.5.2 Experimental
225(2)
7.5.3 Results
227(8)
7.5.4 Conclusions
235(1)
7.6 Hydrodesulfurization of Middle Distillates
236(13)
7.6.1 Experimental
236(5)
7.6.2 Results
241(8)
7.6.3 Conclusions
249(1)
References
249(2)
8 Experimentation in Large-scale Continuous Fixed-bed Tubular Reactors
251(44)
Guillermo Centeno
Luis C. Castaneda
Jorge Ancheyta
8.1 Introduction
251(5)
8.2 Description of the Pilot-plant Unit
256(2)
8.2.1 Feedstock Section
256(1)
8.2.2 Reaction Section
257(1)
8.2.3 Separation Section
257(1)
8.2.4 Gas Washing Section
258(1)
8.2.5 Product Stabilization Section
258(1)
8.2.6 Gas Measurement
258(1)
8.2.7 Gas Sampling and Analyzer
258(1)
8.3 Results and Discussion
258(32)
8.3.1 HDT of Hydrocracked Residue obtained from a 16°API Crude Oil
258(5)
8.3.2 Hydrotreating of Highly Aromatic Petroleum Distillates
263(1)
8.3.3 Characterization of Spent Catalyst from Residue Hydrotreating
264(20)
8.3.4 Reaction Kinetics for Hydrotreating of Residue
284(6)
8.4 Conclusions
290(1)
Nomenclature
291(1)
Greek Symbols
291(1)
Subscripts
291(1)
Superscripts
292(1)
References
292(3)
9 Experimentation in Large-scale Continuous Ebullated-bed Reactors
295(46)
Jose A.D. Munoz
Guillermo Centeno
Jorge Ancheyta
9.1 Introduction
295(6)
9.1.1 Characteristics of Ebullated Bed Reactors
295(1)
9.1.2 Parts of an Ebullated Bed Reactor
296(2)
9.1.3 Advantages and Disadvantages
298(1)
9.1.4 Catalyst
299(1)
9.1.5 Sediment Formation
300(1)
9.2 Experimental
301(11)
9.2.1 EBR Experimental Unit
301(2)
9.2.2 Catalyst Loading
303(1)
9.2.3 Catalyst Bed Expansion
303(3)
9.2.4 Operating Conditions
306(2)
9.2.5 Starting-up, Adjustment, and Stabilization of Conditions
308(4)
9.2.6 Catalyst Activation
312(1)
9.3 Results and Discussion
312(24)
9.3.1 Operating Conditions
312(1)
9.3.2 Real Conversion and Yields
312(5)
9.3.3 Effect of Pressure
317(8)
9.3.4 Effect of Hydrogen Purity
325(4)
9.3.5 Effect of LHSV
329(7)
9.3.6 Hydrogen Consumption
336(1)
9.4 Conclusions
336(1)
References
337(4)
10 Experimentation in Continuous Stirred Tank Reactors
341(58)
Luis C. Castaneda
Jose A.D. Munoz
Jorge Ancheyta
10.1 Introduction
341(2)
10.2 Hydrocracking/Hydrotreating Experiments in CSTRs
343(16)
10.2.1 Hydrocracking of an Atmospheric Residue (343°C+)
345(6)
10.2.2 Hydrocracking of an Atmospheric Residue (312°C+)
351(1)
10.2.3 Parallel Thermal and Catalytic Hydrotreating of Heavy Oil
352(6)
10.2.4 Deactivation of a Hydrotreating Catalyst in a Bench-scale CSTR
358(1)
10.3 Results and Discussion
359(31)
10.3.1 Hydrocracking of an Atmospheric Residue (343°C+)
359(2)
10.3.2 Hydrocracking of an Atmospheric Residue (312°C+)
361(8)
10.3.3 Parallel Thermal and Catalytic Hydrotreating of Heavy Oil
369(9)
10.3.4 Deactivation of a Hydrotreating Catalyst in a Bench-scale CSTR
378(12)
10.4 Conclusions
390(1)
Nomenclature
391(1)
Greek Symbols
392(1)
Subscripts
393(1)
References
394(5)
Index 399
Jorge Ancheyta is Manager of Products for Transformation of Crude Oil, Mexican Petroleum Institute, and Professor, School of Chemical Engineering and Extractive Industries, National Polytechnic Institute of Mexico. Dr Ancheyta has been awarded the highest distinction (Level III) as National Researcher by the Mexican government. He is a member of the Mexican Academy of Science and recipient of the National Award on Chemistry. He is also Associate Principal Editor of the International Journal Fuel.
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