Post on 01-Dec-2021
Safety ManagementSafety Management
DSC • Determination of: - Temperature of decomposition- Energy of decomposition- Material compatibility • Determination of: - Heat of reaction
- Maximum Temperature of Synthesis Reaction - Thermal accumulation
DSC
Tp: Temperature of ProcessMTSR: Maximum Temperature for Synthesis ReactionTMRad: Time to reach maximal rate of decomposition
ASSESSMENT PROCESS SAFETYPROCESS SAFETY
If high energy of decomposition is detected, complementary tests are needed:• Thermokinetic modeling of decomposition reaction• Shock sensitiveness• Friction sensitivity• Sensitivity to intense heat under confinement...
PROCESS DEVELOPMENT
Safety report Meeting R&D, HSE, production
Evaluation of customer process safety data
PROCESS OPTIMIZATION SCALE-UP PRODUCTIONTECHNICAL
PACKAGE
Safety data acquisition
Transfer protocol
ModelingScale-up evaluation
TD24: Temperature at which time to maximum rate is 24h (decomposition temperature)
ΔTad: Adiabatic Temperature Rise
CALORIMETRIC STUDIESCALORIMETRIC STUDIES
Temperature / °C
DSC / (W/g)
Energy: 1637 J/gOnset: 111°CPeak: 140°CPower: 8.8 W/g
5010
10
5
5
0
100 150 200 250 300 350
Safety ManagementSafety Management
DSC • Determination of: - Temperature of decomposition - Energy of decomposition - Material compatibility
DSC
SCALE-UP EVALUATION
Tp: Temperature of ProcessMTSR: Maximum Temperature for Synthesis ReactionTMRad: Time to reach maximal rate of decomposition
ASSESSMENT PROCESS SAFETYPROCESS SAFETY
Determination of: • Heat of reaction • Maximum Temperature
of Synthesis Reaction • Thermal accumulation
RC1 is equiped for low temperature reactions assessment.Optimax, Easymax
If high energy of decomposition is detected, complementary tests are needed:
• Criticality index assessment• Determination of temperature and feed rate
• Cooling capacities assessment for an exothermic reaction • Evaluation of heat transfer at production scale
• Risk analysis performed on site (HAZOP)• Definition of safety barriers during reaction, work-up, distillation, drying
PREVENT
Desiredreaction
Indesiredreaction
(Decomposition)
MITIGATE
OPERATE
TIME
TEMPERATURE
Normal process
Cooling failure
t0
Tproess
TMRad
MTSR
t2t1
Tadr
Tadd
• Thermokinetic modeling of decomposition reaction• Shock sensitiveness• Friction sensitiveness• Sensitivity to intense heat under confinement...
PROCESS DEVELOPMENT
Safety report Meeting R&D, EHS, production
Evaluation of customer process safety data
PROCESS OPTIMISATION SCALE-UP PRODUCTIONTECHNICAL
PACKAGE
Safety data acquisition
Transfer protocol
ModellingScale-up evaluation
TD24: Temperature at which time to maximum rate is 24h (decomposition temperature)
ΔTad: Adiabatic Temperature Rise
SCALE-UP EVALUATION
• RC1, Optimax, EasymaxCALORIMETRIC STUDIESCALORIMETRIC STUDIES
Desired reaction
Undesired reaction(Decomposition)
SCALE-UP EVALUATIONSCALE-UP EVALUATION
• Criticality index assessment• Determination of temperature and feed rate
• Cooling capacities assessment for an exothermic reaction • Evaluation of heat transfer at production scale
• Risk analysis performed on site (HAZOP)• Definition of safety barriers during reaction, work-up, distillation, drying
55
50
45
40
35
30
25
20
15
10
5
0
-5
002:40:00
Ti (°
C), T
r (°C
)
Acetic anhydride. Total Mass (g)
Thermal Conversion (qr_hf)2(%
)
qr_h
f(W)
16
24
32
20
28
38
18
26
34
36
22
30
4028
26
24
22
20
18
16
14
12
10
8
6
4
2
0
-2
100
90
80
70
60
50
40
30
20
10
0
002:50:00 003:00:00 003:10:00 003:20:00 003:30:00 003:40:00 003:50:00 004:00:00
Thermal conversion
Heat of reaction
Reaction temperature
Jacket temperature
Reagent dosing
RC1Optimax Easymax