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Development of Precipitated Iron Catalysts With Improved Stability
Final Report, September 1987--September 1992 - 1993

Abrevaya, Hayim

UOP, Inc.

Table of Contents

Section 1
Event Summary 4
Objective 4
Tasks in the Program 5
Key Results 5
  Draining of Liquid Products from Slurry Autoclave 5
Reference Iron Catalysts 6
Iron Catalyst Preparation Parameters 7
Iron Catalyst Performance in Fixed-Bed Reactor 9
  Iron Catalyst Preparation Plant 10
Iron Catalyst Performance in a Slurry Reactor 11
Deactivation Chemistry for Iron Catalysts and Modifications of Catalysts 12
Contract Objective 12
Introduction 12
Conversion and Selectivity Calculations 14
Results and Discussion 16
Task 1. Upgrade of the Existing Pilot Plants 16
Task 2. Performance of Reference Catalysts 18
  Iron Catalyst from Mobil 19
  Fixed-Bed Run 52 20
Fixed-Bed Run 53 21
Section 2
Task 3. Construction of a Catalyst Preparation Plant and Development of a Baseline Catalyst 23
  Determination of pH's for Precipitating Fe and Cu 23
Description of DSC and TGA Experiments 24
Description of TPR Experiments 26
Use of DSC for Determining Calcination Temperature Requirement for Fe-Cu Catalysts 28
Effect of Calcination Temperature 30
Effect of pH 32
Effect of Cu Level 35
Effect of Potassium 37
Catalysts Precipitated with NH4OH 38
Summary of the Effect of the Catalyst Preparation Plant 41
Catalysts Prepared in the Catalyst Preparation Plant 41
  Catalyst Preparation Plant 41
Drying, Calcination, Impregnation, and Calcination 42
Catalysts Prepared in the Plant 43
Example of Catalyst Characterization 44
Details of Preparation for Catalyst 6616-18 44
Experimental Fe Catalyst Evaluation in Fixed-Bed 46
Shakedown of Slurry Pilot Plant 49
Section 3
Evaluation of a Ceramic Filter in the Autoclave 51
Evaluation of Filter with Large Pore Sizes 53
Evaluation of Different Filtration Procedures 56
Evaluation of Baseline Fe Catalyst in Run 19 60
  Performance during the First 1,250 Hours 61
Effect of Conversion Level on Reaction Rate 63
Catalytic Performance after Return to early Test Conditions 64
Effect of Conversion Level on Catalytic Selectivity 65
Predicting Catalytic Performance in a Slurry Bubble-Column Reactor 65
Catalytic Performance after Restart-Up following Cold Shutdown 66
Product Distribution 68
Conclusions 68
References 69
  Tables 413kb