Академический Документы
Профессиональный Документы
Культура Документы
• ARC Data
• Vessel characterization
• RC1 data analysis and modeling
– Minimum addition times
– Hydrogenation
• DynoChem Challenges
• Final Thoughts
• Examples
– Fed-batch reactions - What is the minimum addition time?
• Reaction rates limited by feed rate (dosing-controlled)
• Reaction rate limited by reaction kinetics (kinetic-controlled)
– Hydrogenation
• Build-up of potentially unstable intermediate
NaOH + 2 H2O
+ 2 NaOCl
R
+ 2 NaI MeOH/H2O I R + 2 NaCl
0°C
OH OH
• Large scale – Less efficient heat transfer and minimum jacket temp of 0oC
(Estimate for new reactor)
I
12 Same addition 12
10
rate as RC1
10
8 Max T > 10oC
45 min Feed Reaction Temp
6 RC1 Reaction Temp 8 3 hr Feed Reaction Temp
Temperature (°C)
Temperature (°C)
RC1 Jacket Temp
4 RC1 Jacket Temp Temp
C19 Reaction
C19 Jacket Temp 6
2
0
4X RC1 Add Time
4
-2
RC1 Tr Max T < 4oC
-4 Max T < 0.1oC 2
-6
0 10 20
20 30
30 40
40 50
50 6060 7070 8080 0
0 50 100 150 200 250
Time
Time(min)
(min)
Tim e (m in)
• Implication
– Wall thickness effect, Stirring Speed Effect
3rd Process Safety Forum © 2008 Abbott
October14, 2008
Minimum Addition Time:
Kinetic controlled reaction
O
N2H4 H2O HN
R NMe2 N R
2.5
2
Heat Flow (W)
RC1 Data
1.5
Model
0.5
0
0 50 100 150 200
Time (min)
2
Heat Flow (W)
RC1 Data
1.5
Model
k2 833.00 0
0 50 100 150 200
Time (min)
Potential to 25 75
Reflux
Instantaneous ATR (°C)
20 70
Temperature (°C)
15 65
5 55
0 50
0 50 100 150 200
Time (min)
0.14
H2 Uptake (mol)
0.1
Experimental
Fitted Uptake
• k2 = 1.67 L/mol/s CI 1.4% 0.08
Nitro
Amine
0.06 Hydroxylamine
0.04
0.02
Value Time Scale [s] 0
Experimental
• ΔHrxn,1=-341.3 kJ/mol 4 Fitted Model
• ΔHrxn,2=-100.6 kJ/mol 2
(CI 14.9%)
1
0
0 50 100 150 200 250
• Possible scenarios to investigate Time (min)
• Time
– Learning curve – Practice, practice, practice…
– Data entry – Using templates
• Complexity
– Natural tendency (for me, at least) to start at overly detailed models