GROUP B 2002

FALL

DISTILLATION STARTUP
Pre-Lab:

Fill out paperwork for the lab-technicians to startup the distillation column at total reflux for the day of experimentation. Verify column is at steady state. The guidelines for steady state are listed in Determination of Steady State. Verify the reflux tank level exceeds 20 in !abview" or # of the reflux tank meter" otherwise see Reflux/Reboil Tank Level Adjustments. Verify the reboil tank level is within the designated $green% &one" otherwise see Reflux/Reboil Tank Level Adjustments. Verify the temperature profile of the column is similar to that shown in Figure '(" initial. )f the reboiler temperature exceeds *' +," )t will be necessary to reduce the temperature of the reboiler. -efer to Reboiler Temperature Reduction for instructions. .elect the *th feed tray by turning the valve on. The valve handle on the *th tray must be hori&ontal. Verify that no other feed tray is turned on" i.e. the other feed tray valve handles are vertical. Turn the feed direction valve" located above the feed tank" to $Feed%. /ote0 The feed direction valve usually set initially to $-eboiler%. (fter completion of the initial checklist proceed to the Start-up Procedure.

Initial Checkli t:

Deter!inin" Stea#$ State: T%tal Re&l'(: Tray temperatures do not change more than ' degrees in 1 minutes. -eflux tank level does not change more than ' in 1 minutes. -eboil tank level does not change more than ' in 1 minutes C%ntin'%' : ,onditions from Total Reflux must be satisfied. Feed" 2istillate" and 3ottoms streams must be balanced. Re&l'()Reb%il Tank Le*el A#+' t!ent : Re&l'( Tank Le*el ,i"h: Re&l'( Tank Le*el L%-: Reb%il Tank Le*el ,i"h: Reb%il Tank Le*el L%-: N%te : )ncrease distillate valve setting. 2ecrease distillate4reflux valve setting. )ncrease bottoms valve setting. 2ecrease bottoms4steam valve setting.

)f both tanks are low or decreasing valve settings do not significantly change the tank levels" a feed stream may be added to increase the volume of li5uid in the column. )f the reboiler needs additional li5uid 5uickly" the feed direction valve may be changed to send the feed directly into the reboiler. 6ake sure that the feed valve is turned OFF while changing the feed direction valve. Thi h%'l# %nl$ be #%ne bet-een r'n #'e t% the #ra tic chan"e that -ill take .lace in the c%l'!n/

Reb%iler Te!.erat're Re#'cti%n: 0/ 6ake sure that the feed and steam valves are set to 0. 2/ Turn the feed direction valve" located above the feed tank" to $-eboiler%. The feed will now be sent directly to the reboiler and not to the feed tray. 1/ .et the feed4bottoms valves to 10 and 21 respectively. 7ay close attention to the level in the reboiler. (d8ustments may be necessary if the level changes more than 94- 2 or approaches the limits of the $green% &one. To raise4lower the amount of li5uid in the reboiler" decrease4increase the bottoms valve setting respectively. The optimal reboiler level is approximately :* . The temperature of the reboiler will usually appear to fall below ;1 +,. This is a false reading due to insufficient mixing of the cold feed and hot reboiler li5uid. 2/ (fter a couple of minutes set the feed and bottoms valves to 21 and <'0. =atch the temperature of the reboiler closely. )f it should begin to rise above *' +," step : must be repeated. 3/ >nce the temperature of the reboiler begins to slow its approach to steady state" set the feed and bottoms valves to 0. 4/ )f the temperature begins to approach a steady state temperature lower than *' +," let the column come to steady state according to Determinin Steady State" and return to the initial checklist. Start-'. Pr%ce#'re: N%te: The specific values in this manual" used to determine times at which valve settings must be changed" pertain specifically to the steady state achieved with final valve settings of0
Stea!: 23 Fee#: 22 Re&l'(: 22 Di tillate: 12 B%tt%! : 23

0/

The column should be in total reflux at steady state with the initial valve settings of0
Stea!: 10/0 Fee#: 0 Re&l'(: 44 Di tillate: 0 B%tt%! : 0

2/ 1/

.et steam valve to '00.

Stea!: 000 Fee#: 0 Re&l'(: 44 Di tillate: 0 B%tt%! : 0

(t <*0.1-*' +, set the feed valve to ?2" <': minutes to step :.

 Stea!: 000

Fee#: 22

Re&l'(: 44

Di tillate: 0

B%tt%! : 0

2/

=ait for the temperature profile to be approximately that of the steady state position" shown in Figure '3" transition. This will occur approximately when the reboiler temperature has reached its steady state temperature" <*2.0-*:.0 +,. @owever it is necessary to make sure that the rectifying section trays have surpassed their respective steady state temperatures to create a convex curve demonstrated in Figure '3" transition. )t is also necessary to ensure that the stripping section trays have reached or are slightly elevated from their respective steady state temperatures. The Tra$ 5 te!.erat're i the #eci i*e c%n#iti%n &%r the &inal tran iti%n/ >nce the prior conditions are met" tray A will begin to increase significantly past its steady state temperature" <B;.1-B*.0 +,. DO NOT let the stripping section tray temperatures raise more than '-2 +, above their respective steady state temperatures. (t this point change the steam" reflux" distillate" and bottoms to the following" <? minutes from step : to step ?0
Stea!: 23 Fee#: 22 Re&l'(: 22 Di tillate: 11 B%tt%! : 23

3/

!et the system come to steady state" <A minutes from step ? to step 1. Verify according to Determinin Steady State.
A) Initial B) Transition C) Final

Temperature Profiles on Startup

100 Temperature ( C) 90 80 70 60 50 0 2 4 6 8 10 12
o

14

Tray Number
Fi"'re 0/ Typical temperature profiles during startup with only steam or feed4steam together. A6 )nitial profile at time 0. B6 Transition profile at a t when the final valve settings are set. C6 The final steady state profile achieved when both the profile and the reflux4reboil tank levels are constant.

Tr%'ble h%%tin"),el.&'l ,int : )f the initial reboiler temperature is above that of the steady state" and specifically *' +, in this experiment" follow the steps outlined in Reboiler Temperature Reduction.

)f the temperature profile is allowed to pass the transition profile outline in Figure '3" two possible solutions exist0 I )f the temperature profile of the rectifying section appears hori&ontal" then follow Reboiler Temperature Reduction. )nstead of aiming for a temperature lower than *' +, the target temperature will be the steady state reboiler temperature of <*2.1 +,. II )f the temperature profile is only slightly above the target transition profile" then the column can be left to arrive at steady state over a longer period or forced down by following the steps in Reboiler Temperature Reduction with a target temperature of <*2.1 +,. -eflux4-eboil tank levels must be closely watched and may be ad8usted according to Reflux/Reboil Tank Level Adjustments. B7 SUR7 TO TURN ON T,7 DATA LOGGING S8ST79. 7ay extreme attention to the profile changes early on. Cxperience in determining transition times is critical to reducing the column startup time.

G/C/ Calibrati%n

6ake up methanol4water solutions with concentrations of 1" 20" ?0" B0" ;0" and *1 mole percent methanol. -un each solution through the D.,. noting the peak areas for water and methanol Emethanol will be the first peakF. 7lot concentration versus peak area for both water and methanol. !inearly regress the data and use the resulting e5uation to accurately determine concentrations from future D.,. runs.