Continuous Cooling Crystallization in a Coiled Flow Inverter Crystallizer Technology—Design, Characterization, and Hurdles
Abstract
:1. Introduction
2. Materials and Methods
2.1. Substance Systems
2.2. Design, Setup, and Process Parameters
2.3. Analytics
2.4. Experimental Procedure
2.4.1. Residence Time Distribution for the CFIC
2.4.2. Crystal Growth Experiments in the CFIC
2.4.3. Anti-Plugging Strategies
2.4.4. Suspension Detection with Inline Sensor
2.4.5. Combination: Nucleation and Crystal Growth
3. Results
3.1. Residence Time Distribution
3.2. Crystal Growth Experiments
3.2.1. l-Alanine
3.2.2. Glycine
- Feasibility of another substance system shall be shown;
- A higher solid amount should be reached due to the higher dependency of solubility of glycine in water than l-alanine in water;
- Its structure is similar to l-alanine.
3.3. Anti-Plugging Strategies and Suspension Detection
3.4. Combination: Nucleation and Crystal Growth
4. Discussion
5. Conclusions
- Residence time distribution (RTD) for different phases and particle sizes;
- Crystal growth for different sieved seed particle sizes, seed amount, and two different amino acids;
- For combined nucleation in an ultrasonic bath and crystal growth units in continuous flow.
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
Abbreviations
Symbols | Dimensionless Numbers | ||
coefficients | Bodenstein number | ||
heat capacity | Frd,crit | critical densimetric Froude number according to a empirical correlation | |
inner tube diameter | densimetric Froude number | ||
friction factor | Reynolds number | ||
distribution sum curve | Indices | ||
gravitational constant | * | saturated (equilibrated) | |
mean growth rate | ambient | ||
heat transfer coefficient | 0,tracer | tracer concentration | |
length | l-alanine | ||
mass flow rate | cooling agent | ||
pressure loss | (time) until crystals are visible | ||
crystal size distribution sum curve | experimental (time) | ||
gravimetrically determined saturation | glycine | ||
time | liquid phase | ||
actual residence time | logartithmic normal size distribution | ||
temperature | process | ||
mean temperature | product crystal | ||
mean flow velocity | relative | ||
volume | suspension | ||
volume flow rate | solution | ||
mass fraction | solvent | ||
mean mass fraction | Abbreviations | ||
particle mass fraction | CFI | coiled flow inverter | |
particle size | CFIC | coiled flow inverter crystallizer | |
mass loading | CG | crystal growth | |
yield | combi | combined experiments with nucleation and crystal growth | |
mean yield | CSD | crystal size distribution | |
Greek Symbols | CU | crystallization unit | |
difference | DTB | Draft Tube Baffle | |
dynamic viscosity | erf | error function | |
dimensionless time | FEA | Functional Equipment Assemblies | |
mean dimensionless time | FEP | fluorinated ethylene propylene | |
density | MSMPR | Multistage Continuous Mixed-Suspension, Mixed-Product Removal | |
density liquid | MZW | meta stable zone width | |
density difference between solid and liquid phase | RTD | residence time distribution | |
standard deviation | SFC | slug flow crystallizer | |
hydraulic residence time |
Appendix A
l-alanine [42] | −1.4024∙10−2 | 3.2451∙100 | −6.0342∙10−4 | 3.2874∙10−1 |
glycine | 7.8260∙10−3 | 1.6994∙100 | −8.6319∙10−4 | 4.3729∙10−1 |
Equipment | Model | Manufacturer | Country | Name (in the Flowchart) |
---|---|---|---|---|
peristaltic pump | LabDos® Easy-Load | HiTec Zang GmbH | Germany | - |
peristaltic pump head | Masterflex L7s Easy-Load® | Cole-Parmer GmbH | US | - |
gear pump | ISMATEX REGLO-Z Digital | Cole-Parmer GmbH | US | - |
gear pump head | ISMATEC GA-X21.CFS.C | Cole-Parmer GmbH | US | - |
flow control | mini CORI-FLOW™ | Bronkhorst High-Tech B.V. | Netherlands | FI_F01 |
scale | Kern 572 | KERN & SOHN GmbH | Germany | WI_W01 |
process control system | LabManager® | HiTec Zang GmbH | Germany | - |
resistance thermometers | RM-Typ WL-1,5-1Pt-B-100-2 | RÖSSEL-Messtechnik GmbH | Germany | TI_ambient, TI_00, TI_USB, TI_01-41 |
thermocouple | type-K | OMEGA Engineering | US | TI_TIin, TI_TIout, TI_02-42 |
cryostat (1–3) | Pilot ONE ministat 125 | Peter Huber Kältemaschinenbau AG | Germany | - |
magnetic valve | Typ 6626–TwinPower | Bürkert GmbH & Co. KG | Germany | magnetic valve A and B |
pressure sensor | A-10 | WIKA Alexander Wiegand SE & Co. KG | Germany | PIA+_P01 |
stirrer plate | MR 3001 | Heidolph Instruments GmbH & Co. KG | Germany | - |
microscope | Bresser Science ADL 601P | Bresser GmbH | Germany | - |
camera | Z6 | Nikon GmbH | Japan | - |
separation analyzer | LUMiReader® PSA 453 | LUM GmbH | Germany | - |
scale | MS1003S/01 | Mettler-Toledo GmbH | US | - |
Sample (-) | (g·min−1) | (g·min−1) | (°C) | (°C) | (°C) |
---|---|---|---|---|---|
seed90–125 1 | 18.6 ± 0.4 | 19.5 ± 0.2 | 30.9 | 23.3 | 24.0 |
seed90–125 2 | 19.8 ± 0.7 | 20.2 ± 0.2 | 30.4 | 23.9 | 22.9 |
seed125–180 1 | 17.6 ± 0.6 | 20.4 ± 0.1 | 30.4 | 23.8 | 23.8 |
seed125–180 2 | 17.9 ± 0.5 | 21.5 ± 0.1 | 30.3 | 23.7 | 23.7 |
seed90–180 1 | 15.6 ± 0.5 | 19.9 ± 0.1 | 30.0 | 23.2 | 25.9 |
seed90–180 2 | 18.8 ± 0.6 | 21.3 ± 0.1 | 30.5 | 23.9 | 23.6 |
seed90–125 3 | 15.4 ± 0.3 | 16.3 ± 0.1 | 30.1 | 23.4 | 23.3 |
seed90–125 4 | 16.3 ± 0.4 | 17.7 ± 0.1 | 30.0 | 23.4 | 23.3 |
glycine90–125 | 26.0 ± 0.9 | 20.1 ± 0.2 | 30.4 | 25.0 | 23.1 |
01 | wait until !PERISTALTICPUMP.ON = 1 {pump needs to be turned on} | |
02 | repeat | |
03 | T1 | !MAGNETIC_VALVE_A=0 {rinse with solvent(water)} |
04 | wait 10 seconds | |
05 | s=current_time | |
06 | repeat | |
07 | if (!PI_00<1250) and (!PI_00>20) and (!PERISTALTICPUMP.ON=1) then | |
08 | !MAGNETIC_VALVE_A=1 {pump suspension} | |
09 | wait 1 second | |
10 | suspension=current_time - s | |
11 | end if | |
12 | until (suspension>00:13:00) or (!PI_00>1250) or (!PI_00<20) | |
13 | !MAGNETIC_VALVE_A=0 | |
14 | if (!PI_00>1250) or (!PI_00<20) then | |
15 | wait until (!PI_00<900) and (!PI_00>500) | |
16 | else | |
17 | continue with T1 | |
18 | end if | |
19 | until !PERISTALTICPUMP.ON=0 | |
20 | !MAGNETIC_VALVE_A=0 |
01 | wait until !PERISTALTICPUMP.ON=1 |
02 | !MAGNETIC_VALVE_A=0 {rinse with solvent(water)} |
03 | wait 30seconds |
04 | if (!PI_00<1250) and (!PI_00>20) and (!PERISTALTICPUMP.ON=1) then |
05 | !MAGNETIC_VALVE_A=1 {pump suspension} |
06 | t_start = current_time |
07 | wait until (!PI_00>1250) or (!PI_00<20) |
08 | !MAGNETIC_VALVE_A=0 |
09 | rinse_time = current_time – t_start {time till clogging} |
10 | wait until !PI_00<800 {stabillization of the pressure} |
11 | else |
12 | rinse_time=00:13:00 {error condtion} |
13 | end if |
14 | repeat |
15 | ! MAGNETIC_VALVE_A=0 {rinse with solvent (water)} |
16 | wait 60 seconds |
17 | t=current_time |
18 | repeat |
19 | if (!PI_00<1250) and (!PI_00>20) and (!PERISTALTICPUMP.ON=1) then |
20 | ! MAGNETIC_VALVE_A=1 {pump suspension} |
21 | wait 1 second |
22 | duration=current_time-t |
23 | end if |
24 | until (duration=rinse_time) or (!PI_00>1250) or (!MASSFLOWRATE.A<0) then |
25 | ! MAGNETIC_VALVE_A=0 |
26 | if (!MASSFLOWRATE.A>1.5) or (!MASSFLOWRATE.A<0) then |
27 | wait until (!PI_00<900) and (!PI_00>500) |
28 | end if |
29 | until (!PERISTALTICPUMP.ON=0) |
30 | ! MAGNETIC_VALVE_A=0 |
01 | wait until (!MAGNETIC_VALVE_A=1) and (!PERISTALTICPUMP.ON=1) |
02 | repeat |
03 | if (!ARDUINO.RESISTOR<1567) and (!PI_00<1250) then |
04 | !MAGNETIC_VALVE_B=1 {product tank} |
05 | wait until (!ARDUINO.RESISTOR>1567) or (!PERISTALTICPUMP.ON=0) or (!PI_00>1250) |
06 | !MAGNETIC_VALVE_B=0 {waste tank} |
07 | wait until (!ARDUINO.RESISTOR<1567) or (!PERISTALTICPUMP.ON=0) |
08 | end if |
09 | until !PERISTALTICPUMP.ON=0 |
10 | !MAGNETIC_VALVE_B=0 |
Sample | (g·min−1) | (g·min−1) | (°C) | (°C) | (°C) | (°C) | (°C) |
---|---|---|---|---|---|---|---|
combi 1 | 17.9 ± 0.5 | 19.5 ± 0.1 | 54.3 | 18.3 | 20.0 | 18.9 | 24.2 ± 0.2 |
combi 2 | 17.4 ± 0.5 | 19.9 ± 0.1 | 54.6 | 18.3 | 20.1 | 20.1 | 24.3 ± 0.2 |
combi 3 | 16.4 ± 0.5 | 19.7 ± 0.1 | 54.6 | 19.9 | 21.2 | 19.9 | 23.8 ± 0.2 |
combi 4 | 17.3 ± 1.1 | 18.1 ± 0.1 | 53.9 | 12.6 | 19.9 | 21.8 | 26.1 ± 0.4 |
combi 5 | 17.2 ± 0.8 | 18.4 ± 0.1 | 53.6 | 12.5 | 19.7 | 23.0 | 26.3 ± 0.4 |
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Sample Name | Investigation | Seed/Tracer Particles | |
---|---|---|---|
Sieve Size (µm) | Solid Weight Fraction (Set Point) (w.%) | ||
RTDS,90–125 | RTD | 90–125 | 1 |
RTDS,125–180 | RTD | 125–180 | 1 |
RTDS,90–180 | RTD | 90–180 | 1 |
RTDL | RTD | - | 0 |
seed90–125 1 | CG | 90–125 | 1 |
seed90–125 2 | CG | 90–125 | 1 |
seed125–180 1 | CG | 125–180 | 1 |
seed125–180 2 | CG | 125–180 | 1 |
seed90–180 1 | CG | 90–180 | 1 |
seed90–180 2 | CG | 90–180 | 1 |
seed90–125 3 | CG | 90–125 | 0.1 |
seed90–125 4 | CG | 90–125 | 0.1 |
glycine90–125 | CG | 90–125 | 1 |
combi 1 | nucleation + CG | - | 0 |
combi 2 | nucleation + CG | - | 0 |
combi 3 | nucleation + CG | - | 0 |
combi 4 | nucleation + CG | - | 0 |
combi 5 | nucleation + CG | - | 0 |
Sample Name | (g∙min−1) | (s) | τ (s) | (-) | (-) |
---|---|---|---|---|---|
RTDS, 90–125 | 16.2 ± 0.3 | 256 ± 1 | 266 ± 5 | 0.960 | 308 ± 73 |
RTDS, 125–180 | 16.5 ± 0.1 | 248 ± 2 | 260 ± 2 | 0.951 | 286 ± 20 |
RTDS, 90–180 | 17.3 ± 0.5 | 240 ± 1 | 249 ± 6 | 0.962 | 353 ± 65 |
RTDL | 16.6 ± 0.5 | 227 ± 8 | 226 ± 7 | 1.006 | 383 ± 5 |
Sample | (μm∙s−1) | Clogging | ||||||
---|---|---|---|---|---|---|---|---|
seed90–125 1 | 0.00802 | 0.00872 | 66 ± 3 | 31.5 | 0.148 | 3.55 | 115 | no |
seed90–125 2 * | 0.00628 | 0.00868 | 60 ± 8 | 29.4 | 0.147 | 3.34 | 66 | no |
seed125–180 1 | 0.00984 | 0.00725 | 65 ± 4 | 36.4 | 0.161 | 3.76 | 57 + 20 | yes |
seed125–180 2 | 0.00759 | 0.00570 | 55 ± 9 | 37.8 | 0.170 | 3.69 | 10 + 37 | yes |
seed90–180 1 | 0.00828 | 0.00659 | 51 ± 6 | -6 | -0.024 | 4.24 | 23 | yes |
seed90–180 2 ** | 0.01158 | 0.00394 | 58 ± 11 | 18.5 | 0.088 | 3.52 | 35 + 8 + 6 + 16 | yes |
seed90–125 3 | 0.00144 | 0.00127 | 18 ± 5 | 66.0 | 0.256 | 4.29 | 39 | yes |
seed90–125 4 | 0.00112 | 0.00042 | 7 ± 2 | 71.5 | 0.294 | 4.05 | 45 | yes |
glycine90–125 ** | 0.00615 | 0.01457 | 71 ± 4 | 39.9 | 0.248 | 2.69 | 32 | yes |
Sample | l-Alanine Batch Number | |||
---|---|---|---|---|
1 | 1941180707 | 1.371 | 3.6 | 18 |
2 | 1941180707 | 1.356 | 3.4 | 12 |
3 | 1941180707 | 1.314 | 3.5 | 20 |
4 | 1941200315 | 1.352 | 3.4 | 9 |
5 | 1941200315 | 1.328 | 3.3 | 7 |
Criterion | CFIC (This Work and Reference [56]) | CFI Hohmann et al. [42] | SFC Termühlen et al. [44] |
---|---|---|---|
Inner Diameter (mm) | 1.6 | 4 | 3.18 |
Tube Length (m) | 7.8 ∙ number.CU | 6.54 | 7, 13.25 and 26.5 |
Flow Rate | ≈16 g min−1 | 30, 40 g min−1 | 20, 40 mL min−1 |
Residence Time (min) | ≈1 ∙ number.CU | 2.75, 2.15 | 10.5, 5.25 |
Cooling Strategy | tube-in-tube counter-current (with water) | housed tube counter-current (with gas) | tube-in-tube co-current (water as active insulation) |
Crystal Growth Rate (µm s−1) | 0.088–0.170 (seed90–180 1 excluded) | 0.055 to 0.079 | 0.127 to 0.411 |
Operation Time | 2.6τ to 30τ 10–115 min | ≥3τ | 3.8τ to 7.6τ 40 min |
Tendency to Clogging | relatively high | stable | seems stable |
Other Factors |
|
| |
|
Criterion | USU+CFIC (This Work) | Eder et al., 2012 [23] | Besenhard et al., 2015 [24] | Han et al., 2018 [19] Ultrasonicated Conditions Only |
---|---|---|---|---|
Substance System | l-alanine in water | acetylsalicylic acid in ethanol | phthalic acid in water | |
Inner Diameter (mm) | 1.6 | 2 | 4 | |
Tube Length (m) | 6 + 15.6 | 3 + 27 | 15 | 12/18 |
Tube Material | FEP | polysiloxane | stainless steel | |
Flow Rate | ≈16 g min−1 | 15 mL min−1 | 22 (feed) + 4–11 (seed) mL min−1 | 50–150 mL min−1 |
Residence Time (s) | ≈45 + 120 | ≈215, 265 | ≈100 | 60–271 |
Cooling Strategy | cooled USU and tube-in-tube counter-current in the CFIC (with water) | step-wise (7 levels) (with cryostats) | step-wise (6 levels) (with cryostats) | step-wise (2 levels) (with cryostats) |
Operation Mode |
|
|
|
|
Ultrasound Device | ultrasonic bath, 37 kHz, | ultrasonic bath, 35 kHz | ultrasonic baths, 35 kHz | |
Operation Time | 7–20 min | ≈25 min | 5 ∙ (10 min + 2.5 min rinsing) = 60 min | three to four residence times |
Location of Crystal Samples | non-invasive inline | crystallizers outlet (filtrated, washed, dried) | online in an external chamber | after filtering and drying |
Particle Size (µm) | 69–215 | 50–190 | 90–130 | seed ≈ 11 product ≈ 10–400 |
Tendency to Clogging | relatively high and variable | n/a | no clogging occurred | operation time for three or four residence times was defined as feasible |
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Schmalenberg, M.; Kreis, S.; Weick, L.K.; Haas, C.; Sallamon, F.; Kockmann, N. Continuous Cooling Crystallization in a Coiled Flow Inverter Crystallizer Technology—Design, Characterization, and Hurdles. Processes 2021, 9, 1537. https://doi.org/10.3390/pr9091537
Schmalenberg M, Kreis S, Weick LK, Haas C, Sallamon F, Kockmann N. Continuous Cooling Crystallization in a Coiled Flow Inverter Crystallizer Technology—Design, Characterization, and Hurdles. Processes. 2021; 9(9):1537. https://doi.org/10.3390/pr9091537
Chicago/Turabian StyleSchmalenberg, Mira, Stephanie Kreis, Lena K. Weick, Christian Haas, Fabian Sallamon, and Norbert Kockmann. 2021. "Continuous Cooling Crystallization in a Coiled Flow Inverter Crystallizer Technology—Design, Characterization, and Hurdles" Processes 9, no. 9: 1537. https://doi.org/10.3390/pr9091537