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Author Topic: Emulsion fighting  (Read 65 times)

Sydenhams chorea

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Emulsion fighting
« on: May 19, 2012, 09:57:49 AM »
I want to hear your techniques :P

Just prepared some 2C-H via electroreduction, as always basification of the washed acidic aqueous layer and subsequent extraction with toluene caused an emulsion. This time, however, it's one big ass chunky, foaming orange emulsion that hasn't cleared up at all after standing one day.

Buchner filtering over celite is not an option, as no celite is handy.

What do you do in such a situation?
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b6baddawg

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Re: Emulsion fighting
« Reply #1 on: May 19, 2012, 12:20:12 PM »
im just tossing a perhaps lame idea, would an emulsion separate through a setup similar to a chromotography column?

my only other thought, is  toluene substitutable? perhaps xylene emulsion isnt as bad to clear.

salat

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Re: Emulsion fighting
« Reply #2 on: May 19, 2012, 12:22:22 PM »
Patience, a vibrator, more patience, sometimes adjusting the ph then more patience.
Salat

fresh1

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Re: Emulsion fighting
« Reply #3 on: May 19, 2012, 02:28:20 PM »
Quote
Patience, a vibrator, more patience

lol I take it the vibrator helps with the patience and not the emulsion ::) ;)

SC what about adding NaCl to assist in the separation...just start adding salt (make SURE it's non Iodised ;)) and stir.

IDK exactly how much you will need to add to 'break' the emulsion but it will 'break' eventually.

 If it's a toluene water emulsion this should work fine. Just start adding small amounts of salt, shake and let settle. You didn't say how much you had nut start with maybe 1gm/litre and titrate up :P

You should start noticing an improvement fairly soon keep adding small amount until separation becomes evident and then wait. :D
« Last Edit: May 19, 2012, 03:27:09 PM by fresh1 »
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Enkidu

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Re: Emulsion fighting
« Reply #4 on: May 19, 2012, 02:48:49 PM »
IIRC, you can use one of those ultrasonic cleaners to break up emulsions.

lugh

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Re: Emulsion fighting
« Reply #5 on: May 19, 2012, 03:31:00 PM »
Adding finely granulated sodium chloride or a brine solution often helps break the emulsion ;)  Vibrations or ultrasonic agitation have been known to work too  :P  Filtration through diatomaceous earth, sand or fine fiberglass/cotton wool can separate the emulsion  :-X If all else fails then one can try heating the emulsion up, and if that doesn't work one can always put it in the freezer  8)
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Electro´S

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Re: Emulsion fighting
« Reply #6 on: May 19, 2012, 05:21:13 PM »
Hot water bath and vibration with a sanding machine ussually works well. Other times just adding more solvent (if you want recover organics) or water (if you need recover acid) in a hot water bath is enough.
« Last Edit: May 19, 2012, 07:30:14 PM by Electro´S »
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