of 32
Accelerated screening of carbon dioxide capture by liquid sorbents
Ryan J.R. Jones,
a
Yungchieh Lai,
a
Kevin Kan,
a
Dan Guevarra,
a
Joel A. Haber,
a
Natalia M. Ramirez,
b
Alessandra Zito,
b
Clarabella Li,
b
Jenny Y. Yang,
b
Aaron M. Appel,
c
and John M. Gregoire*
a
a
Division of Engineering and Applied Science, California Institute of Technology, Pasadena, CA 91125, USA. E
-
mail: gregoire@caltech.edu.
b
Department of Chemistry, University of California, Irvine, California 92697, USA.
c
Institute for Integrated Catalysis, Pacific Northwest National Laboratory, Richland, Washington 99352, USA
.
Tetramethylammonium 2,3,4,5,6
-
pentafluorophenolate
The NMR and FTIR characterization are shown in Figures S1
-
S5.
Yield:
2.259
g (97 %)
.
1
H NMR (600 MHz
d
-
DMSO)
δ
3.14 (
TMA) ppm.
13
C{
1
H} NMR (151 MHz, d
-
DSMO)
δ
147.8 (
tt,
J
=14.1, 4.0 Hz), 140.9 (dtdd,
J
=231.9, 9.2, 4.6, 1.9 Hz), 138.6 (ddtd,
J
=235.9, 19.2, 10.6, 2.3 Hz), 123.7 (dtt,
J
=
222.4, 14.8, 5.4 Hz), 54.4
-
54.3 (m, TMA) ppm.
13
C{
1
H} NMR (151 MHz, D
2
O)
δ
142.0
141.7 (
m), 140.8 (dm,
J
=231.6 Hz), 138.2 (dm,
J
=240.7 Hz), 129.8 (dm,
J
=232.4 Hz), 55.3
55.2 (m, TMA) ppm.
19
F{
1
H} (565 MHz, d
-
DMSO)
δ
-
172.0
-
172.1 (m, 2F),
-
172.1
-
172.3 (m, 2F),
-
196.3
-
196.5 (m, 1F) ppm.
FTIR (ATR)/cm
-
1
v = 3032
.41 (w),
1690.86 (w), 1644.75 (w), 1599.17 (w), 1504.13 (s), 1487.98 (s), 1467.75 (s), 1248.42 (m), 1230.19 (m),
1167 (w), 1084.29 (w), 1046.34 (w), 1001.62 (s), 967.89 (s), 723.23 (w), 604.91 (w), 577.75 (w).
Figure S1:
13
C{
1
H} NMR of TMA pentafluorophenoxide in d
-
DMSO.
Electronic
Supplementary
Material
(ESI)
for
Digital
Discovery.
This
journal
is
©
The
Royal
Society
of
Chemistry
2024
Figure S2:
13
C{
1
H} NMR of TMA pentafluorophenoxide in D
2
O.
Figure S3:
1
9
F{
1
H} NMR of TMA pentafluorophenoxide in d
-
DMSO.
Figure S4:
1
H NMR of TMA pentafluorophenoxide in d
-
DMSO.
Figure S5: FTIR of TMA pentafluorophenoxide.
CCSI assembly instructions
1.
Clear Hood/Work Area
2.
Place Breadboard
3.
Wire Electrical Distribution Rack Ground and Relays, ensuring to observe proper polarity for both
Control and Load signals.
4.
Mount Main Chamber Panel (12”x12” panel) onto elevated standoffs
5.
Insert REC Chamber into Panel and Install lower TEE as shown (REC Chamber → Tee Common
port). Place Flow Selection Valve 6 on breadboard as shown. Connect the REC Chamber TEE into
the Valve 6 Common as shown. Install PEEK tubing into Valve 6 A port as show
n. Ensure the PEEK
tubing is long enough to reach the designated Waste/Used repository.
6.
Place switching valve V4 on the breadboard in approximate shown location. Connect V4
Common port to the REC Chamber Tee.
7.
Connect port V4A to the Pump Output TEE, as shown.
8.
Connect the Pump Output Tee Common port to the output of the Diaphragm Pump, as shown.
Place pump on breadboard in approximate location shown so that none of the fluidic connectors
are strained/pulled from their housing.
9.
Mount Valves V1, V2, V3, V5, and V7 on the Main Panel in the approximate locations shown.
10.
If no sorbent analyzer used, Connect port V4B to port V3B as shown. If using sorbent analyzer,
Connect port V4B to Sorbent Analyzer Inlet, and Connect port V3B to Sorbent Analyzer Outlet.
11.
Connect port V3 Common to Diagraphm Pump Inlet
12.
Connect Port V5 Common to the remaining Pump Outlet Tee Port
13.
Connect port V5A to one end of the Return Loop TEE. Connect the other Return Loop TEE port to
valve port V2 Outlet, as shown, leaving the Return Loop Tee Common open.
14.
Connect Return Loop Tee Common port, and port V1B, to the REC Chamber Lid
15.
Connect V1 Common port to port V7A
16.
Connect port V7B to Flow Selection Valve Channel 4
17.
Connect port V2 Inlet to Flow Selection Valve Common Port (center port)
18.
Connect pCO2
inlet to REC Chamber Lid
19.
Connect pCO2 outlet to port V3 Common
20.
Configure MFC’s such that they outlet into two ports of a TEE. Connect the remaining port of the
Gas Metering TEE to the REC Chamber Lid
21.
Route the tubes from V6A and V5B to the designated Waste/Used repository location to ensure
they reach.
22.
Wire all the valves to GROUND. Each valve has a pair of wires for electronic control. One wire
from each pair is used to connect each valve to a common Ground, polarity is not consequential.
As shown, the Omron 12V source Ground is wired to a Wago distribu
tion panel, which allows all
Valve Wires to connect to Ground simultaneously. Some wires may need to be extended if they
do not reach the power distribution rack.
23.
Wire all the Valves to their respective control relays. Each valve will have 1 wire available after
connecting the other to ground (previous step). Ensure this free wire is connected to the proper
control relay, observing relay load polarity to ensure prop
er function.
24.
Plumb gas lines into the hood. Connect background gas to Valve port V7 Common. Connect
Syringe Pumps to respective Multi Channel Valve Port
25.
Test all valves and connections for leaks and proper functioning.
End of assembly instructions.