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Flash Evaporation to remove methylene chloride and The recovery of the Aniline from Extraction.

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Presentation on theme: "Flash Evaporation to remove methylene chloride and The recovery of the Aniline from Extraction."— Presentation transcript:

1 Flash Evaporation to remove methylene chloride and The recovery of the Aniline from Extraction.

2 At this point, you should be able to account for the following items. If you have all three of these, you are ready for Flash Evaporation; p. 135 Zubrick If you have all three of these, you are ready for Flash Evaporation; p. 135 Zubrick. (Note: IF the methylene chloride had evaporated, you will need to add more.)

3 You have gone to a great deal of effort to DRY everything You have gone to a great deal of effort to DRY everything. Then, from this point, be sure that ALL of the glassware you use is ABSOLUTELY DRY.Then, from this point, be sure that ALL of the glassware you use is ABSOLUTELY DRY.

4 Start setting up with a good sturdy ring stand. If the rod is loose, tighten it before you begin so your set-up won’t WOBBLE

5 Place the burner on the stand. The hotplate is NOT a good option for this procedure. Be sure your burner has a needle valve to adjust gas flow, and a rotating barrel to control air- flow.

6 Now, add the iron ring Leave 2 to 3 inches for the flame.

7 The wire gauze is next. The wire gauze should have a ceramic center. Don’t worry if there is hole in it.

8 A beaker serves as a hot water bath. Select a LARGE beaker with sufficient capacity for your 50 mL RB flask.

9 Clamp your 50 mL RB flask (NO LARGER) in the water bath Place the flask as far into the water as possible Place the flask as far into the water as possible.

10 Attach the three- way adapter atop the flask Attach the three- way adapter atop the flask. (The adapter is commonly called the “still head”.)

11 CLAMP the condenser to another ring stand. Rubber bands are available to snug up the condenser. But do NOT trust a rubber band alone, to hold that $50.00 piece of glassware !

12 Arrange an Erlen- meyer flask in an ice slurry for your receiver. You may want to clamp the receiver onto another ring stand.

13 Attach water hoses to the water jacket of the condenser Water always enters at the LOWER end of the water jacket.

14 Place the sep funnel on top of the still head. No need for a stopper; but be sure the stopcock is CLOSED !

15 Remove the spent magnesium sulfate (GRAVITY FILTER) from the aniline – in - methylene chloride solution. Wash with small portions of methylene chloride; collecting all of the filtrate.

16 Make sure the stopcock is CLOSED. (Don’t be one of those who will forget!) THEN, transfer the filtrate into the sep funnel.

17 Light the burner and adjust to a good hot flame. Bring the water in the beaker to near boiling.

18 Adjust the burner to a small flame. The object is to keep the water bath hot.

19 Open the stopcock SLIGHTLY and allow slow steady drops to fall onto the hot flask. Methylene chloride boils over in an instant (in a flash?) as the high boiling aniline remains behind.

20 While the Flash Evaporation is going on, filter the magnesium sulfate from your p-dichlorobenzene. Place the filtrate on your hot plate UNDER YOUR SNORKEL, and and evaporate off the methylene chloride. When the volume reached only a few mLs, you may begin to see white vapors rising from the beaker. STOP the evaporating, and COOL the contents. The residual p-dichlorobenzene “should” solidify.

21 Finally, only aniline remains in the RB flask. Discard the methylene chloride in the waste receptacle provided for it; -- and prepare to collect the aniline.

22 Collecting the Aniline by distillation through an AIR-COOLED condenser.

23 Turn off the burner flame. Remove the ice bath and receiver. Discard the methylene chloride in the receptacle provided Remove the ice bath and receiver. Discard the methylene chloride in the receptacle provided.

24 Drain the water from the water jacket. Remove the hoses from the condenser

25 Remove the sep funnel from the “still head”. Loosen the blue retainng nut and return the sep funnel to the box from which you got it.

26 You no longer need the water bath. Remove it and return the large beaker to the cabinet from which you got it Remove it and return the large beaker to the cabinet from which you got it.

27 Lower the RB flask to sit firmly on the wire gauze. LEAVE NO AIR SPACE! Lower the condenser assembly and re- attach it firmly to the still head. NO WATER HOSES!

28 Place the thermo- meter assembly into the still head. The thermo- meter bulb should be just below the side- arm of the still head.

29 Pre- weigh and label two DRY 50- mL Erlen- meyer flasks. The first is to catch the “forerun”; the second is to catch the final product (aniline).

30 With a good, hot flame, distill the contents in the RB flask. Switch receivers as the temper- ature climbs rapidly toward 180 degrees Switch receivers as the temper- ature climbs rapidly toward 180 degrees.

31 Collect the aniline that boils at degrees. Never distill to a dry flask. When dark droplets spatter in the RB flask, you may have difficulty cleaning it!

32 Part F-neutral compound Part F- recovering the neutral compound Remove the spent MgSO 4 by gravity filtration. (You may have done this while working with the aniline.)

33 UNDER YOUR SNORKEL,evaporate to near-dryness on a hotplate. (You may have already done this too.) UNDER YOUR SNORKEL, evaporate to near-dryness on a hotplate. (You may have already done this too.)

34 steam distill Transfer the residue into a larger RB flask, and steam distill the mixture as before. Collect the distillate in an ice-cooled receiver. Recover the product on Buchner with suction.

35 THIS CONCLUDES THE EXPERIMENT ON EXTRACTIONS Complete your laboratory report form, and prepare to turn in some of your products Complete your laboratory report form, and prepare to turn in some of your products.


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