Chemical Engineering Experimental Design 2 / Recitation CHME 4315/4316

Module 3
Chemical Engineering Department
CHME 4315/4316: Chemical Engineering Experimental Design 2 / Recitation
Liquid – Liquid Extraction Unit

Challenge:

Your company produces vegetable oils from raw plant tissues, and in order to modify the oil for
specific purposes, mixes the oil with ethanol. This ethanol then needs to be separated from the
final oil product by extraction with liquid. You have been given a smaller-scale model of the
LLE column that your company would like to use for this process. You are tasked with
understanding the liquid-liquid extraction process well enough to be able to adapt its operation to
other situations.

Overall objective: Analyze the performance of the liquid-liquid extraction column at different
flow rates, initial concentrations and steady state or semi batch configurations. What is the
maximum extraction you can achieve? How efficient is it to achieve that level of purity. What
variables are most important? Can a high level of purity be achieved for a reasonable amount of
energy and/or solvent expenditure?

For Pre-Lab: Overall Goal: Learn your system and define a set of experiments that gives you
the most information in the time allotted.
 What is the plan for Teamwork Effectiveness? (For this, use the template provided for the
Discovery Module.)
 Define the questions that you want to explore. Indicate the specific objectives for the next
two weeks of experiments.
 Explain your experimental methods. Develop a process flow diagram and list of materials
and equipment, outline the procedure, and describe the safety risks and mitigation
approaches that will be applied to answer your questions and meet the specific objectives.
 Describe the relevant theory and mathematical/engineering equations. Describe the
relevant statistical tests.
 Set up the tables that will be used to collect data on variables that apply to the theory,
engineering equations, and statistics.
 Develop example calculations, such as material balance and include units from your
measurements (i.e. calibrate rotameter and water/IPA density curve).

Procedure:

PRECHECKS – UNIT GROUNDED TO LABORATORY GROUND – IMPORTANT SO

THAT STATIC ELECTRICITY DOES NOT ACCUMULATE

1 Check with a continuity meter, electrical continuity of stainless steel parts within unit
and to the 3rd prong (grounding prong) on the electrical cord.
2 Plug cord into a wall outlet.
3 Re-check continuity with meter leads touching a stainless steel surface of the unit and
a copper or brass surface within laboratory. 3 ohms or less should be read indicating
good grounding of the unit to the laboratory.

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Chemical Engineering Experimental Design 2 / Recitation CHME 4315/4316
Pre-Lab Guide: Liquid-Liquid Extraction

START UP PREP
4 Bring all drain lines on unit to the sewer or external collection vessels
a There are 3 or 4 lines total
b V27 (Solvent Feed Tank Drain)
c V28 (Column Drain)
d V29 (Sample Bottoms of Column)
5 Trace all lines. Recognize which is the “primary” flow path and which is the
“alternative” flow path. Recognize the two operations: Liquid-Liquid Extraction, and
Distillation of the Solvent after extraction.

FILLING OF THE TANKS

6 NOTE – MOST VALVES MAY BE OPEN DUE TO CLEAN UP AND

ALLOWING THE SYSTEM TO “DRY” DURING THE PREVIOUS USE.
7 Close all valves, insuring that this action seems to make sense. (for example V27
should be closed so that Solvent Feed Tank does not empty during filling. A partial
table of valves and their positions during filling are provided below.
8 NOTE - BEFORE BEGINNING TO THE EXPERIMENT, IT IS BETTER TO FILL
TANKS WITH WATER AND RINSE THE SYSTEM WITH WATER TO
ELIMINATE ANY REMAINING DETERGENT IN THE SYSTEM DUE TO
PREVIOUS CLEANING.

IF INTENDING TO CONDUCT A TOTAL RECYCLE RUN, NO ALCOHOL ADDED: This

run is a practice on observing the L-L system operating. Feed and Solvent are recycled through
the system back to their respective supply tanks (B1 and B5)
9 Fill tank B1 with water to about ¾ full. (~ 8L)
10 Fill Tank B5 with BioOil to about ½ full. (~12L)
11 Turn on Unit (NOTE if signs of “no power” check emergency stop, it needs to be
fully pulled out)
12 Open the correct valves to initiate a flow of feed to the column by tracing the lines
before turning feed pump on. Valves to open or switch are: V2 (controls flow thru
rotameters, set this to 90% for rapid filling), V3 Closed (this valve controls flow to
the Raffinate Tank), Two way valve V7 to Feed Tank (recycle), V4 Open (this
allows the column to “bleed” air as it is filled. Turn on feed pump. Fill the column to
about 50% of the feed (BioOil).
13 Stop filling with feed when level reaches 50%.
14 Then, to add water (solvent) from top by turning on solvent pump, Valves to open or
switch are V-1 (controls flow through the solvent rotameters), V3 Closed (we’ll open
this on the next step), V4 Open (this allows the column to bleed air at it is continued
to be filled, V8 to Solvent tank (recycle). Filling the column the rest of the way.
15 Set the feed and solvent rotameters flow rates, adjusting flows in both directions, at
about 30% to 50%.
16 Valve V3 needs to be open to allow the extract stream to flow into the solvent tank.
17 Once you are comfortable with this operation, move on to the addition of alcohol to
the BioOil

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Chemical Engineering Experimental Design 2 / Recitation CHME 4315/4316
Pre-Lab Guide: Liquid-Liquid Extraction
18 SHUT OFF PUMPS DURING THE NEXT STEP
19 CLOSE V3 SO THAT COLUMN DOES NOT EMPTY DURING THE NEXT STEP

FULL LIQUID-LIQUID EXTRACTION

20 Once column is verified working properly, Add about 10-20% by volume of IPA to
Feed Tank, B5 (the tank with the BioOil in it), and mix it with the agitator for hand
drill.
21 Continue for a few moments on recycle just to insure steady state.
22 Once a controlled interface is established, switch V7 to Raffinate Tank, and V8 to
Extract Tank.
23 Extraction will begin
24 Interface level can be controlled by adjusting valves V3 and V4. Material must be
taken off from both the top and bottom continually for column to function correctly.
25 Shut down is done by switching off both pumps and closing Valve V3. Material will
remain in the column until the column is drained manually.

DISTILLATION OF SOLVENT (WATER) WITH ETHANOL

This experiment is separate from the liquid-liquid extraction set. This can be completed as a
later experiment to determine how effectively you can recover the original amount of ethanol.

26 Start a flow of cooling water

27 Transfer material from Tank B3 into distillation pot by opening glass valve slowly on
the line from Tank B3 to the Distillation Pot
28 You may have to open Valve
29 Close Glass Valve
30 Turn on vacuum pump, vacuum should go negative rapidly, otherwise there is an
open valve or system leak. One leaking spot discovered included a plastic
relief/fill/plug valve. Turn slightly to get a seal.
31 Switch heater to “2”
32 Turn on heater at control panel
33 Temperature reading will be on K3
34 We used an initial set point of 80 C because we had -0.8 bar

SHUT DOWN DISTILLATION UNIT

35 Turn heater dial selector to 0

36 Turn off distillation heater at control panel.
37 Let everything return to a non-boiling state – the temperature for example should
begin to drop (the boiling process is removing heat from the heating tape, cooling it,
by boiling)
38 Shut off the vacuum pump
39 Open V11, air bleed very slowly, the system will return to normal pressure
40 Leave this valve open
41 Open V22 to drain the distillate tank,

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Chemical Engineering Experimental Design 2 / Recitation CHME 4315/4316
Pre-Lab Guide: Liquid-Liquid Extraction
42 After draining, shut down the water flow to the condenser

TO DRAIN COLUMN

43 Open V28 and drain water to drain

44 Open V30 slightly to allow air into system

TO DRAIN SUPPLY TANKS

45 The solvent tank, B1, can be dumped directly to the sewer, V21
46 Recollect the BioOil into jugs by opening V25 and V24 and filling the jugs slowly.

TO CLEAN UNIT

47 Add water to tanks B1, B4, and B5, and rinse once with water.
48 Add a small amount of Dawn Dish Liquid to Tanks B4 and B5
49 Continually rinse with a small amount of water in each tank, gradually decreasing the
soap bubbles within and in the column is minimize
50 Towel dry all tanks (B1, B4, and B5), leave lids off, and all valves open so that unit
can air dry and leave no water behind within the tanks.

Valve listing for start up

V1 Control Valve for solvent flow to unit
V2 Control Valve for Feed Flow to Unit
V3 Control Valve Extract from Unit (helps balance the interface)
V4 Control Valve for Raffinate from Unit (helps balance the interface)
V5 Relief Valve solvent pump line (back to tank B1)
V6 Relief Valve feed pump line (back to tank B5)
V7 Two way valve (Raffinate) (to B4 Raffinate or B5 Feed Tank)
V8 Two way valve (Extract) (to B1 Solvent or B3 Extract Tank)
…..
V12 Closed (from Distillate Collection Tank to Solvent Tank)
…..
V21 Closed Front Drain for Solvent Feed Tank
V22 Drain from Distillate Collect Tank B2 Open for continuous sampling into a collection
receiver if ethanol distillation
V23 Closed Drain Valve for Extraction Tank.
V24 Closed Front Drain for Feed Tank B5
V25 Closed Front Drain for Raffinate Collection Tank B4
V27 Closed (from Solvent Feed Tank B2)
V28 Closed (empty Column)
V29 Closed (to obtain sample or to empty lines)
V30 Closed (top of column for Sampling)

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