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Liquid Phase Methanol Process Development Unit: Installation, Operation, and Support Studies. Task 5 LaPorte LPMEOH PDU Renovation, Installation and Shakedown (Run-F-1) - 1985

Air Products and Chemicals, Inc.

Table of Contents

Abstract ii

I

 Executive Summary 1

II

 Introduction 2

III

 Laporte LPMEOH PDU Description 3
 

A

 Background 3

B

 Process Design Basis 4

C

 Process Description 9

D

 Design Features 13

E

 Data Acquisition System 17

IV

 Commissioning Highlights 27
 

A

 General 27

B

 Exotherm Problems and Solution 28

C

 Nuclear Density Gauge Calibration 29

D

 Two-Phase Gas Holdup Data 37

V

 10-Day Shakedown Run (Run F-1) 46
 

A

 Objectives 46

B

 Catalyst Reduction 47

C

 Catalyst Bed Studies 47

D

 Methanol Synthesis Operation 71

VI

 Conclusions and Recommendations 90

VII

 References 92

VIII

 Appendices 93
 

A

 Exotherm Problem and Solution 93

B

 Sample Gas/Liquid/Solids Profile Calculation 106

C

 Shakedown Run F-1 Detailed Data Acquisition System Sheets 114

List of Tables

III-1 LaPorte LPMEOH PDU Major Process Equipment List by Source 5
III-2 Range of Operting Variables for LaPorte LPMEOH PDU 7
III-3 LaPorte LPMEOH PDU Feed Gas Compositions 8
III-4 LaPorte Gas Chromatograph Analyses: Components, Range, and Accuracy 22
III-5 LaPorte Liquid Chromatograph Methanol Product Analyses:  Components, Range, and Accuracy 24
III-6 LaPorte Trace Component Gas Analyses 25
III-7 LaPorte Catalyst Analyses 26
IV-1 Nuclear Density Gauge Readings of Empty Reactor 31
IV-2 Nuclear Density Gauge "Zero" Readings 32
IV-3 Nuclear Density Gauge Calibration Ratios 33
IV-4 Specific Absorbances of LPMEOH Process Materials 35
IV-5 Relative Specific Absorbances 36
IV-6 Two-Phase Gas Holdup Data on N2/Freezene-100 Oil 38
IV-7 Two-Phase Gas Holdup Data on Balanced Gas/Freezene-100 Oil 43
IV-8 Variation of Gas Holdup With Reactor Height 45
V-1 Catalyst R71/OF12-26 (EPJ-19LR) Particle Properties 48
V-2 LaPorte LPMEOH PDU Catalyst Reduction Chronology with Catalyst R71/OF12-26 (EPJ-19LR) 49
V-3 NDG Measurements of Oxide Bed Density 52
V-4 NDG Measurements of Dry Catalyst Bed Density After Bulk Reduction 53
V-5 NDG Measurements of Dry Catalyst Bed Density After Polishing Reduction 54
V-6 Reduced Catalyst Properties 55
V-7 Initial Wet Settled Bed Density Measurements - NDG Survey No. BE-01-AD 56
V-8 Summary of Bed Expansion Test Results 62
V-9 Shakedown Run Three-Phase Gas Holdup for N2 73
V-10 LaPorte LPMEOH PDU Shakedown Run (F-1) Operating Conditions 75
V-11 LaPorte LPMEOH PDU Shakedown Run (F-1) Chronology with Catalyst R71/OF12-26 (EPJ-19LR) 76
V-12 LaPorte LPMEOH PDU Shakedown Run Catalyst Sample Analyses 88
A-1 Exotherm Event #1 - 12 December 1983 96
A-2 Chronology of Events of 12-13 December 1983 97
A-3 Exotherm Event #2 - 18 December 1983 99
A-4 Chronology of Events of 18 December 1983 100
A-5 Potential Reactions in LaPorte LPMEOH PDU Exotherm Events 102
B-1 Raw Data for NDG Survey No. F-1-09 107
B-2 Physical Properties for NDG Survey No. F-1-09 108
B-3 Calculated Bed Density Profile for NDG Survey No. F-1-09 111
b-4 Numerical Integration for cS8 FOR NDG Survey No. F-1-09 112

List of Figures

III-1 Simplified Process Flowsheet for LaPorte LPMEOH PDU 10
III-2 LaPorte LPMEOH PDU Reactor 11
III-3  LaPorte LPMEOH PDU Data Acquisition System:  Integrated Computer/Analytical Hardware Configuration 19
IV-1 LaPorte LPMEOH PDU Nuclear Density Gauge Voltage/Density Calibration 30
IV-2 Gas Holdup for N2/Freezene-100 LaPorte LPMEOH Reactor 40
IV-3 Gas Holdup for N2/Freezene-100 Comparison with Hikita/Asai Correlation 41
IV-4 Two-Phase Gas Holdups from LaPorte LPMEOH PDU 44
V-1 Initial Wet Settled Bed Height 57
V-2 Wet Settled Bed Height After Bed Expansion Study 59
V-3 Expanded Bed Profiles:  N2 63
V-4 Expanded Bed Profiles:  N2 (cont'd) 64
V-5 Expanded Bed Profiles:  N2 (cont'd) 65
V-6 Expanded Bed Height as Function of Superficial Liquid and Gas Velocity 67
V-7 Expanded Bed Profiles:  Balanced Gas 68
V-8 Expanded Bed Profiles:  Balanced Gas (cont'd) 69
V-9 Expanded Bed Profiles: CO-rich Gas 70
V-10 Expanded Bed Profiles: CO-rich Gas (cont'd) 74
V-11 Two-Phase and Three-Phase Gas Holdup:  N2 74
V-12 LaPorte PDU Performance Compared to Lab PDU, Autoclaves, and Model:  Balanced Gas 80
V-13 LaPorte PDU Performance Compared to Lab PDU, Autoclaves, and Model:  Co-rich Gas 81
V-14 Increase in Slurry Solids Loading during LaPorte PDU Shakedown Run 82
V-15 Carbonyl Survye of LaPorte PDU 85
V-16 Materials of Construction and Operating Conditions of LaPorte PDU 86
A-1 Simplified Process Flowsheet for LaPorte LPMEOH PDU - Original Configuration 94