Adsorption Unit Operating Procedures: CO2 Adsorption on to Activated Carbon Background Safety Concerns Description of the Unit Switching the Unit On Preparation of the Unit Configuration of the Unit for Solid-Gas Adsorption Configuration of the Unit for Solid-Gas Desorption Adsorption of Carbon Dioxide on Activated Carbon or Zeolites Data Collection Stopping the Unit In an emergency At the end of an experiment Instructions in RED are new and must be vetted by any team running the ADS Unit Brown, Herman, & West (edited by S. Rochelle, H.J. Toups) 1 3/28/2018
Switching the Unit On Adsorption Unit Operating Procedures: CO2 Adsorption on to Activated Carbon Check the gas supply by ensuring that the cut-off valves V13 (CO2) and V15 (air) are closed. Open the CO2 feed cylinder; a pressure of ~2 bar (30 psi) should read on the cylinder s leftmost gauge. Check that the gas input pressure does not exceed 1 bar on PI6 and PI7 when air and CO2 are flowing. Honeywell Station System: o Open Honeywell s Station application from a UOLAB virtual machine o Search ads in the command window at the top o Click the Trend 900 button to see the Honeywell DCS trend plot (with the fastest rate of 5-second data) o Load the Excel data collector file for this experiment (at this location: X:\CHE4162\CHE4162-HW Excel Data Recorders\snr) o Set the data rate to 1-second readings o Start transferring data from Honeywell to the Excel file before running any adsorption and do not perform any other Excel functions while collecting data Prepping the Unit All remaining valves should be closed unless otherwise specified in the procedure All flow rates are manipulated using the control panel on the right side of the unit Check that the control panel temperature indicators display room temperature Prepping the Analyzer o To test initial concentration of CO2, close V17, and open V18. Alternatively, one might rely on the end-of-adsorption composition. o Open valve V15 and run air through the CO2 analyzer, then switch on the CO2 analyzer sampling pump (V31 should be open) using the start/stop button on the front of the unit. o Start transferring data from the Honeywell system to the Excel file mentioned above o Run AIR to the analyzer for 5 minutes at 60 L/h, or the total flow rate defined by the experimental plan Solid-Gas Adsorption in Column 1(DN25) or Column 2(DN40) Column To begin gas flow through one of the columns, open o V12 (Col. 1 gas feed) or V7 (Col. 2 gas feed) o V10 (Col. 1 exhaust valve) or V5 (Col. 2 exhaust valve) o V22 (exit gas to vent) **(V12+V10+V22) or (V7+V5+V22) must be opened if V17 is open** Brown, Herman, & West (edited by S. Rochelle, H.J. Toups) 2 3/28/2018
To switch the gas feed from bypassing the adsorption column to feeding the adsorption column o Open V17 (feed gas to preheater) o Close V18 (gas feed to GC analysis system) Run only air through the column for 5-10 minutes at the desired feed rate Starting up the liquid heating [IKA HBC5] o Turn on water via V29 for the heating bath o Open V27 (Col. 1) or V28 (Col.2) o Ensure the power switch on the back of the heating unit is in the on position (1) o Set the desired temperature via the left-hand knob on the unit and the proper rpm (4000 rpm) via the right-hand knob Starting up the gas heating ** Gas MUST be running through the column PRIOR to the heating cycle ** DO NOT introduce any CO2 into the system until the desired temperature is reached throughout the column (As noted by TT2 (Col. 1) or TT3 (Col. 2) and TIC1) o Select TIC1 on the control panel, ensure that it is set to MANUAL at 0% OP o Also on the control panel, tap the green box on the GAS HEATING icon to switch the power on o Select the TIC1 controller again, change the SP to the desired temperature, and switch the controller into AUTO To begin an adsorption cycle with CO2: o Open valve V13 and start CO2 feed at 0-10% of the total concentration (or other composition suitable to the experimental study objectives) and the balance air flow rate. Record time of CO2 start according to the Excel data collector s time stamp Let adsorption run until the bed is saturated (CO2 analyzer data results in a clear and constant full breakthrough) and record end time Solid-Gas Desorption in Column 1 (DN25) or Column 2 (DN40) Column Cut the CO2 feed flow rate to 0 L/h and only run air (at an appropriate rate) through the system until no more CO2 is detected at the exit of the column. Brown, Herman, & West (edited by S. Rochelle, H.J. Toups) 3 3/28/2018
Lab Equipment Shut Down Set air and CO2 flow rates to 0 L/h Record the end time of the last desorption cycle Stop transferring data from the Honeywell system to the Excel file Switch OFF the sampling pump using the Start/Stop button on the front of the CO2 analyzer. Open valve V18 and close valve V17 Close valves V10, V12, V13, V14, V15 and V22 (Col. 1) or valves V5, V7, V13, V14, V15 (Col. 2) Shutting down the gas and liquid heating units o Set TIC1 to MANUAL and reduce the OP to 0% and change the SP to 20 C o Turn off the GAS HEATER by selecting the red box under the icon o Manually set the liquid heater to 20 C and leave it circulating through the column o Once the liquid heater drops to at least 30 C, close of the water valve (V29) and then close V27 (Col. 1) or V28 (Col. 2) to stop circulation through the column Maximum Reaction Volumes Volume of empty Column 1 glass column 0.30 liters, 25 mm diameter, height 0.6 m Volume of empty Column 2 glass column 0.75 liters, 40 mm diameter, height 0.6 m Gas phase adsorption cycle: Process: continue until the adsorbent is saturated Nature of the gaseous phase: air containing roughly 0.04% or 400 ppm CO2 Maximum pressure of the gaseous phase: 1 bar Gas phase desorption cycle: Process: continue until the adsorbent is unsaturated Nature of the gaseous phase: air Maximum gas phase pressure: 1 bar Air flow rate: 60 L/h or another rate as defined by the experimental plan Brown, Herman, & West (edited by S. Rochelle, H.J. Toups) 4 3/28/2018
VALVE INDEX V1 By-pass valve on the liquid feed pump, which can also be used for taking samples V3 Valve for supplying the right-hand column (2nd column, DN40), which can also be used for venting when it is not connected to the flexible supply tube V4 Valve for sending a sample towards the GC analysis system V5 Cut-off valve for the DN40 column and/ exhaust valve for the gas phase from the 2nd column V6 Input valve for treatment of the liquid phase in the 2nd column V7 Input valve for the gas phase in the 2nd column, which can also be used as a cut-off valve V8 Valve for input to the left-hand column (1st column, DN25) which can also be used for venting when it is not connected to the flexible supply tube V9 Valve for sending a sample towards the GC analysis system V10 Cut-off valve for the DN25 column and/ exhaust valve for the gas phase from the 1st column V11 Input valve for treatment of the liquid phase in the 1st column V12 Input valve for the gas phase in the 1st column, which can also be used as a cutoff valve V13 Cut-off valve for the CO2 supply V14 CO2 supply cylinder V15 Cut-off valve for the compressed air supply V16 Air supply V17 Input valve for the feed gas in the preheating system V18 Valve for sending a gas feed sample towards the GC analysis system V19 Input valve for the feed gas in the neutralization system V20 Drainage valve for the titration cell V21 Valve to pass the feed gas from the exit of the column into the neutralization system V22 Valve sending the gas at the exit of the column to the vent V23 Drainage valve for the supply reservoir/container V24 Drainage valve the reservoir/container containing the liquid to be treated V25 Vent valve for DN25 column double jacket draining V26 Vent valve for DN40 column double jacket draining V27 Feeding valve for DN25 column double jacket oil V28 Feeding valve for DN40 column double jacket oil V29 Feeding valve for heating coil water circulation V30 Drainage valve for heating group oil circuit V31 CO2 analyzer V32 Last valve in vent line before venting to POLY vent system Brown, Herman, & West (edited by S. Rochelle, H.J. Toups) 5 3/28/2018
DESCRIPTION OF THE MEASUREMENTS 2.7.1. Temperature TIC1 temperature of the gas phase supply TI2 internal temperature of the DN25 column TIC2 temperature of the oil bath TI3 internal temperature of the DN40 column TIC3 temperature of the liquid preheating TI4 temperature at the head of the columns The sensors used are Pt 100 Ohm (3-wire) sensors. For the technical information on these temperature sensors, refer to the corresponding technical file. 2.7.2. Pressure PI1 0-1.6 bar needle pressure gauge, pressure at the foot of the columns PI2 0-1.6 bar needle pressure gauge, pressure at the head of the 1st column DN25 PI3 0-1.6 bar needle pressure gauge, pressure at the foot of the 2nd column DN40 PI4 0-4 bar needle pressure gauge, compressed air supply pressure PI5 0-8 bar needle pressure gauge, CO2 supply pressure. For the technical information on these pressure sensors, refer to the corresponding technical file. 2.7.3. Flow rate FI1 0-1200 NL/h rotameter, flow rate of the air feed FI2 0-400 NL/h rotameter, flow rate of the CO2 feed FI3 0-25 L/h rotameter, flow rate of the liquid feed For the technical information on these rotameters, refer to the corresponding technical file. SAFETY: While the unit is functioning, the protective shield/plate must be in place in front of the pilot unit. However, it is important to note that, IT IS FORBIDDEN TO: Introduce solid particles into the feed reservoir/container and thereby into the pump Use clogging solutions in the column Use the unit under vacuum or at high pressure Leave the unit while it is functioning without it being under the supervision of an operator who has been taught the risks encountered on this unit Introduce reactants incompatible with the materials used for the unit Brown, Herman, & West (edited by S. Rochelle, H.J. Toups) 6 3/28/2018