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Development of Improved Iron Fischer-Tropsch Catalysts. Final Technical Report: Project 6464 - 1994

Bukur, Dragomir B., Dr.
Ledakowicx, S., Dr.
Koranne, M., Dr.
Nowicki, L., Dr.
Oktabe, K., Dr.
Skala, D., Dr.
Lang, X., Dr.
Robby, H.
Manne, R.
Wang, D.

Texas A & M Research Foundation at College Station

Table of Contents

List of Tables v
List of Figures viii

I

 Objective and Scope of Work I-1

II

 Executive Summary II-1
 

1

 Pretreatment Effect Research II-1
  1.1 Characterization Studies with 100 Fe/0.3 Cu/0.8 K Catalyst II-1
1.2 Reaction Studies with 100 Fe/0.3 Cu/0.8 K Catalyst II-3
1.3 Characterization Studies with Ruhrchemie Catalyst II-4
1.4 Reaction Studies with Ruhrchemie Catalyst II-6
1.5 Reaction Studies with 100 FE/5 Cu/4.2 K/16 SiO2 Catalyst II-7

2

 Development of Improved Iron-Silica Catalysts II-9
  2.1 Baseline Catalyst Testing II-9
2.2 Testing of Iron-Silica Catalysts Synthesized at TAMU II-10

III

 Pretreatment Effect Research III-1
  Introduction III-1

1

 Pretreatment Effect Research - Characterization Studies with 100 Fe/0.3
Cu/0.8 K Catalyst		 III-5
 

1.1

 Experimental III-5
  1.1.1 Catalyst Preparation Procedure III-5
1.1.2 Catalyst Characterization Equipment and Procedures III-5
1.1.3 Catalyst Handling and Sample Preparation III-7

1.2

 Results and Discussion III-8
  1.2.1 Atomic Absorption III-8
1.2.2 X-Ray Diffraction III-9
1.2.3 Mössbauer Effect Spectroscopy (MES) III-24
1.2.4 Isothermal Reduction Experiments III-31
1.2.5 BET Surface Area and Pore Size Distribution III-33
1.2.6 Transmission Electron Microscopy III-41
1.3 Summary III-47
1.4 References III-49

2

 Pretreatment Effect Research - Reaction Studies with 100 Fe/0.3 Cu/0.8 K
Catalyst		 III-52
  2.1 Experimental Procedure III-53
2.2 Results III-53
2.3 Discussion III-67
2.4 Stirred Tank Slurry Reactor Tests III-67
2.5 Comparison Between FBR and STSR Tests III-78
2.6 Summary III-83
2.7 References III-84

3

 Pretreatment Effect Research - Characterization Studies of Ruhrchemie
Catalyst		 III-86
 

3.1

 Experimental III-86

3.1.1

 Catalyst Characterization Techniques III-86

3.2

 Results and Discussion III-87
  3.2.1 Atomic Absorption III-87
3.2.2 X-Ray Diffraction III-88
3.2.3 Mössbauer Effect Spectroscopy III-99
3.2.4 BET Surface Area and Pore Size Distribution III-102
3.2.5 Transmission Electron Miscroscopy III-105
3.2.6 Temperature Programmed Reduction/Isothermal Reduction III-110
3.2.7 X-Ray Photoelectron Spectroscopy III-118
3.3 Summary III-123
3.4 References III-125

4

 Pretreatment Effect Research - Reaction Studies with Ruhrchemie LP
33/81 Catalyst		 III-127
  4.1 Fixed-Bed Reactor Results III-128
4.2 Discussion III-140
4.3 Stirred Tank Slurry Reactor Tests III-145
4.4 Comparison Between FBR and STSR Tests III-149
4.5 Summary III-155
4.6 References III-157

5

 Pretreatment Effect Research - Reaction Studies with 100 FE/5 Cu/ 4.2 K/
16SiO2 Catalyst		 III-159
  5.1 Experimental Procedure III-159
5.2 Results and Discussion III-162
5.3 Summary III-185
5.4 References III-186

IV

 Development of Improved Iron-Silica Catalysts IV-1
  Introduction IV-1

1

 Baseline Catalyst Testing IV-4
 

1.1

 Testing if UCI Catalysts IV-4
  1.1.1 Run SA-3391 with UCI L-3950 Catalyst IV-5
1.1.2 Run SA-1532 with UCI 1207-175A Catalyst IV-18
1.1.3 Run SA-2502 with UCI L-3950 (Batch 3) Catalyst IV-18
1.2 Comparison of Baseline Catalysts IV-22
1.3 Summary IV-32
1.4 References IV-34

2

 Testing of Iron-Silica Catalysts Synthesized at TAMU IV-35
  2.1 Run SA-1371 with 100 Fe/3 Cu/3 K/8 SiO2 Catalyst IV-37
2.2 Run SB-0931 with 100 Fe/3 Cu/4 K/8 SiO2 Catalyst IV-45
2.3 Run SB-1910 with 100 Fe/5 Cu/4.2 K/8 SiO2 Catalyst IV-55
2.4 Run SB-1910 with 100 Fe/3 Cu/4 K/16 SiO2 Catalyst IV-63
2.5 Run SB-1910 with 100 Fe/5 Cu/4.2 K/16 SiO2 Catalyst IV-73
2.6 Run SB-1910 with 100 Fe/5 Cu/4.2 K/16 SiO2 Catalyst IV-81
2.7 Run SB-1910 with 100 Fe/5 Cu/6 K/24 SiO2 Catalyst IV-91
2.8 Run SB-1910 with 100 Fe/5 Cu/8 K/24 SiO2 Catalyst IV-100
2.9 Comparison of Catalyst Performance IV-107
2.10 Summary IV-113
2.11 References IV-115

V

 Recommendations for Further Study V-1

VI

 Acknowledgements VI-1
Appendix 1.  Fixed Bed and Slurry Reactors and Product Analysis System A-1