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Executive Summary
Supercritical Fluids Technologies, Inc. designs, manufactures, and implements supercritical fluid
extractors that serve to extract pure oils. SFT provides a full range of services in order to meet
the specific needs in supercritical fluid extraction and reaction science. The company currently
uses CO2 drawn from cylinders that contain 40 L of useable CO2 in the liquid phase. Issues have
been brought up due to the cost of the tank and the space occupied by cumbersome liquid
tanks. The approach to this problem is to use a vapor draw Dewar tank of CO2, which contains
300 L of CO2 mixture, at a fraction the cost of liquid tanks. In order to use the Dewar tank, CO2
will be drawn into a distillation system that will precede the SFT machinery. The primary
function of this design is to condense the CO2 to a liquid of high purity. Considerations for
safety and delivery conditions will shape the other aspects of the design. When completed, SFT
will be delivered a working prototype for use in their lab, with the potential for future
commercialization.
Table of Contents
Executive Summary
Table of Contents
Introduction/Background
Project Scope
Refined Metrics
Concept Overview
Methods
Subsystem Engineering
Design Specifications
Design Layout
Test Procedure
Results
10
10
10
11
Conclusions
11
Path Forward
12
Future Testing
12
12
Appendices
13
2
Metric
Delivery Temperature
Delivery Pressure
Cost of System
CO2 Delivery Time
Flow Rate
Size of System (Volume)
Weight of System
Target Value
10C - 22C
>80 bar
$20,000.00 $5,000.00
<30 min
Variable up to 250 ml/min
< 3ft x 3ft x 6ft
Can move on wheels
Metrics were based upon the wants and constraints dictated by the sponsor as well as competitive
benchmarked products in the market. Downstream machinery was also considered. For example, the
CO2 delivery temperature and pressure were given a specified range for which the SFT machinery will
accept. Metrics will be validated following completion of proof of concept
3
Liquid CO2
17 bar, -30C
Liquid CO2
80 bar, -30C
The intermediary fluid to be used between the chiller and condenser is a 75Wt.% Ethylene Glycol/
25Wt.% Water mixture. With a freezing point of -50C, this fluid will remain a liquid at the low
temperatures being reached by the chiller. The flow rate of this fluid is 6 gallons per minute, as dictated
by the recirculation of the chiller.
The condenser to be used should be a heat exchanger with a transfer area of at least 0.34 m2 (3.7 ft2).
The CO2 will run through the inner side, and the chilled intermediary fluid through the outer side. This
transfer area was calculated for a heat transfer of 1.4 kW between the two fluids, assuming the CO2 is
running at 250 mL/min for maximum demand. A conservative estimate of 230 was used for the Heat
Transfer value (U). A sample cooler from Madden has been specified as the condenser with a transfer
area of 0.35m2 (3.8 ft2).
Pump
The pump to be used should increase pressure from 250 psi to 1160 psi, and deliver at variable flow
rates up to 250 mL/min. It is necessary to reach the critical pressure of CO2 (1160 psi), so that
vaporization will not occur in the downstream heater. The SSI Prep250 VFR Diaphragm pump meets
these needs and is specified for this application.
Pulse Dampener
Immediately following the pump, a pulse dampener will serve to smooth out the fluid delivery and
reduce the fluid pulse caused by the pump. This dampener will be made by using an oversized section
of tubing. Given a stroke volume of 0.4525 mL (from pump specifications) and a recommended
dampener volume to stroke factor of 350, a stainless steel, 1 diameter, 1 ft, schedule 10 was specified.
Heater
Final output of the delivery system must be at a temperature in the range of C
10to 22C (room
temperature) to be accepted by the downstream SFT machinery. 500 W of power is required to heat the
5
Figure 4 Process and Instrumentation diagram of the design concept. This drawing represents a critical
piece of the drawing package and is a key deliverable. The P&I diagram specifies technical aspects of the
design and provides a basis for design replication.
Quantity
Manufacturer/Description
Model Number
Cost
Chiller
RC210C0
$14,575.00
Condenser
SC106
$835.00
Pump
Prep-250
$4,100.00
Chiller Tubing
15 ft
5545K14
$12.15
8673T22
$127.33
Pressure Gauge
Stock # 36287
$94.82
Temperature Gauge
RTD-NPT-72-E-DUAL-1/4-MTP
$230.00
Alarm
CN1A-RTD-230VAC
$168.00
SS 1/4 in Pipe
20 ft
Swagelok
$123.80
SS 1 in Pipe
1 ft
Swagelok
SS-T16-S-083-20, 26.37/ft+2CutChge
$273.70
Dewar Fitting
N832A
$17.80
Swagelok
SS-400-1-4
$20.70
Chiller Fitting
Swagelok
SS-600-1-4
$19.00
SC Fitting
Swagelok
SS-600-1-6
$22.00
Gauge Attachments
Swagelok
SS-400-3-4TTF
$94.20
Pump Fitting
Swagelok
SS-400-1-2
$6.60
Swagelok
SS-1610-6-4
$167.40
Swagelok
SS-400-6-2
$11.00
Relief Valve
5026K51
$61.85
T-Fitting
Swagelok
SS-400-3-4TTF
$31.40
25ft
Chromalox
SRM/E 20-1CT
$230.00
Power Connection
Chromalox
RTPC
$56.10
Chromalox
RTBC
$194.70
End Seal
Chromalox
RTES
$6.05
Copper Tubing
50ft Coil
8955K26
$156.38
Heater Fittings
Swagelok
S-600-6-4
$9.50
Fiberglass Wrap
4478K1
$16.59
PolyU. Insulation
5431K15
$8.93
Alarm
CN1A-RTD-230VAC
$168.00
Total:
$21,838.00
Table 2 Bill of Materials indicating the total design cost as well as individual component
specifications and purchasing information.
Figure 5 Preliminary design layouts, showing spatial relations and basis for future
commercialization of housing design.
Pressure Test
1. This test must be performed using CO2 because the tank pressure of butane is not great enough
to open the check valves on the pump. Connect chiller to in/out feeds of the condenser and set
to -35C. Allow to drop to temperature.
2. At the outlet of the condenser, connect temperature and pressure gauges, followed the pump.
After the pump, the second pressure gauge and a temperature sensor should be in place.
3. Ensure digital temperature gauge is working correctly. Use compressed air to pressurize the
system, ensuring it is free of leaks.
4. When chiller reaches temperature, open the CO2 flow to the inlet of the condenser.
5. Monitor the temperature gauge following the condenser. When temperature and pressure
indicate saturation, turn on the pump.
6. Monitor the downstream pressure gauge to ensure that the pump is reaching the specified
pressure. Also monitor the downstream temperature gauge to determine if there is a significant
temperature change across the pump.
10
10C - 22C
>80 bar
$20,000.00 $5,000.00
<30 min
Variable up to 250 ml/min
< 3ft x 3ft x 6ft
Can move on wheels
22C
80 bar
$21,838
1 min
210 ml/min
3 x 4 x 5 ft
Yes
Table 3 Refined design metrics, ranked in order of importance, with measured results at right.
The final deliverables of the project were sufficiently completed in accordance with SFT. The primary
function of the system, the condenser capability, has been validated using proof of concept tests. The
other deliverable expected as a result of this project is a functional prototype that SFT will be able to use
in their lab for supercritical extractions. Accommodations for complete system assembly will be made so
that this deliverable will be completed in the scope of this project. The pump, framing, and remaining
11
Prototype
Commercial Product
Function
Detail thermodynamics of process and determine
Optimized process parameters after seeing
cost of system
performance
Define most inefficient aspects of process
Minimize excess at each instrument
Reduce sponsors costs in liquid CO2 tanks
Eliminate sponsors need to buy purified CO2 and
sell to others
Cost
Buying all instruments at single item list price
Negotiation of bulk or repeat discount possible
Each process not necessarily optimized
Table 4 Differences between the prototype and the future commercial product,
outlined in terms of function and cost.
12
13
14
15
16
17
18
19
20
21
22
23
Power (W) at
Cooling Temp.
60
400
1200
2000
600
2700
1000
3000
Approx. Flow
Rate Possible
(mL/min)
20
40
210
250
150
350
250
650
Manufacturer
Model
FTS Systems
RS33LT
FTS Systems
MC100LT
FTS Systems
RC210
FTS Systems
UC500LT1
Julabo
FP52-SL
FTS Systems
RC311
Julabo
FPW55-SL
Brooks/Polycold
n/a
Notes:
1. Costs may be approximate.
2. Cooling Temperature is given because cooling power may not be available for 35C exactly.
3. For flow rate greater than 100mL/min, an additional $700 is added to the Total
System
Cost to accommodate an electrical post-heater.
Chiller
Cost ($)
$4,700
$9,500
$15,000
$20,000
$23,600
$25,000
$25,600
$35,000
Approx. Total
System Cost ($)
$11,500
$16,300
$22,500
$27,500
$31,100
$32,500
$33,100
$42,800
600
500
400
300
200
Largest Jump
in
Performance
100
0
$0
$5,000 $10,000$15,000$20,000$25,000$30,000$35,000$40,000
Chiller Cost ($)
24
This page includes an expanded summary of all findings on chiller vendors, pricing, and
performance. Links to the respective websites and contact information are also included.
FTS Systems 845.687.5359 Terry
o RS - http://www.ftssystems.com/rschillerback.htm
RS33LT does 195W at -30C, 60W at -40C. $4700
o Maxi-cool Series - http://www.ftssystems.com/maxicool.htm
100LT does 400W at -30C. $9500
o Ultra-cool - http://www.ftssystems.com/ultracool.htm
UC500LT1 does 3600W at -30C, 2000W at -35C, 1100W at -40C. $19,500
o ULT - http://www.ftssystems.com/ultseries.htm
RC311 does 2700W at -40C. $22k-25k
RC210 does 1200W at -35C. $15000
o Note: LT model numbers indicate Low-Temp
o Terry confirmed that chillers in the range we are looking for are uncommon, but that is
really FTS niche.
http://www.julabo.com/us/p_datasheet.asp?Produkt=FPW55-SL
o
http://www.julabo.com/us/p_datasheet.asp?Produkt=FP52-SL
http://www.brooks.com/pages/2149_polycold%C2%AE_systems_cryogenic_refrigeration.cfm
For our application (chiller cooling a heat exchanger/condenser), the appropriate Polycold
chiller is in the $35k range.
Polycold is in the cryogenics business. Their recirculating chillers have temperature ranges of
-30 or -40 to -150, and can produce around 3 kW at these low temps.
Chris Beckey confirmed that there is a gap between the common chiller industry (temps of 10C) and the cryogenics industry (typically -100C). Estimated that a chiller didnt exist that
would provide 1.4 kW at -35C without being a cryogenic chiller, however, said he has limited
knowledge of the non-cryogenic chiller field.
o
o
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Appendix E: Condenser
Condenser calculations and selection
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29
30
31
32
33
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Appendix I: Electrical
Electrical Diagram
35
36
Appendix J: Piping
Friction Loss Calculations
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38
39
40
41
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