Wizzard
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T-butyl project side discovery: Wonderful Na2SO4 crystals!
Tought I'd share these. Trying to dry my Turbo108 with Sodium Sulfate, the batch was too large, and I could not extract all the drying agent.
Distillation, ahoy!
Over 4 days, I distilled at 120*C, collecting the distillate. From this, I still don't know what I'm going to do to try to get out my T-butyl. But the
goal is the adventure, not just the destination!
What was left in my distillation RBF was all the heavy stuff, and these wonderful, dense crystals of sodium sulfate. From 2 days out in the sun and
fresh air (and it's been humid here, for sure), they aren't hygroscopic. The single cluster here weighs 3.6 grams, and includes a wonderfully large
single crystal. Enjoy!
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blogfast25
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Quote: Originally posted by Wizzard  |
Over 4 days, I distilled at 120*C, collecting the distillate. From this, I still don't know what I'm going to do to try to get out my T-butyl. But the
goal is the adventure, not just the destination!
What was left in my distillation RBF was all the heavy stuff, and these wonderful, dense crystals of sodium sulfate. From 2 days out in the sun and
fresh air (and it's been humid here, for sure), they aren't hygroscopic. The single cluster here weighs 3.6 grams, and includes a wonderfully large
single crystal. Enjoy! |
Nice crystals.
What did you start off from again?
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Wizzard
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I started with Turbo 108 octane booster, to try and get it's known indredient: T-butyl alcohol.
I mixed with distilled water, let settle, and froze the mixture- I separeted the ice from the oil, and then thawed the ice.
I believe the ice contains most of the alcohols (and the water). I then tried to dry about 300mL of the liquid by mixing in copious quantities of
sodium sulfate... Let's just say I ended up worse 
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blogfast25
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Any idea what temp. the distillate come over at?
I think you’re approach should basically work. Try using less water to begin with? Of course t-butanol is somewhat soluble in alkane based oils, so
you have a distribution constant that may not be very favourable.
Separate oil from water/alcohols, then distil water/alcohol, then dry with anh. Na2SO4? Then perhaps redistill once, watching still head temp.
closely?
Diethylether could be another solvent for t-butanol extraction. Hard to get though...
[Edited on 26-7-2012 by blogfast25]
[Edited on 26-7-2012 by blogfast25]
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Twospoons
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Diethylether is one of the main components of Engine Start spray. Its meant for getting old, cold engines started, its the stuff you squirt into the
carb.
Helicopter: "helico" -> spiral, "pter" -> with wings
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blogfast25
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| Quote: Originally posted by Twospoons | | Diethylether is one of the main components of Engine Start spray. Its meant for getting old, cold engines started, its the stuff you squirt into the
carb. |
Yes, there's some thread here on how to recover it.
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SM2
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Of course, after freezing, because t-butyl would be extremely hydrophobic. I think MSD index says tert-butyl amine, is some sort of central
stimulant.
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Zan Divine
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So, you want to experience the isolation for yourself? The reason I ask is because t-butanol (unlike my favorite, Et2O) is both cheap and easy to get
here (US) and, when you weigh the considerable time you've invested against the fact that Sargent-Welsh will ship you 500 mL for $21, the per hour
value of your efforts is pretty small.
I tend to be "target" oriented having been a professional chemist. From my viewpoint anything that can be purchased easily and cheaply quickly loses
its synthetic attraction. Since t-butanol isn't your target (presumably, but I could be wrong), how much time and effort does it really warrant? You
seem to have an understanding of the techniques and concepts already.
Depending on your age, maybe time seems infinite. As one who saw a lot of potential in rediscovering the wheel as a learning experience when I was
much younger, restrospectively I see much wasted time which could have been better used.
My bottom line is this: Unless you pursue it for the joy of the experience, or it saves you appreciable money (kinda' unlikely) or unless it teaches
you important new techniques or concepts, synthesizing or isolating from other products a cheap and available chemical is like turning gold into lead.
He who makes a beast of himself gets rid of some of the pain of being a man. --HST
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blogfast25
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| Quote: Originally posted by Zan Divine |
I tend to be "target" oriented having been a professional chemist. From my viewpoint anything that can be purchased easily and cheaply quickly loses
its synthetic attraction. |
Yup. It's subjective though... and good lessons in chemistry are in those synths/isolations.
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Wizzard
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I'm 27 and work full time doing PC repair- I like to work maybe an hour or day with chemicals, especially things I can 'leave running' during work,
like distillation and evaporative crystal growth.
I now have a source for T-butyl alcohol, I'm just trying to wrap up the experiment with extraction from Turbo108. Speaking of which, after freezing
the distillation remnants (what did not distill out), I'm left with a slurry not unlike the intermediary in solgel process- A crystalline liquid,
perhaps large, thin crystals within a liquid for a soupy appearance. I've since melted (above 50*c), cooled (freezes below 0) and tried to separate
the liquid from the crystal- I have a batch now. I wonder what I've extracted.
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Zan Divine
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I understand where you're coming from. BTW, those are beautiful crystals.
When you have an organic which is soluble in water you have a couple common ways to approach it:
a) Salting out - In some cases simply saturating (don't add much more than will dissolve) the solution with common salt will cause the organic to
separate out.
b) Extraction - you could also add a solvent that doesn't mix with water and that also is a good solvent for the dissolved organic. In a lab, my first
thoughts would usually be ether or methylene chloride because of the ease of getting my product out of them. In the basement, my thoughts turn to
whatever is available, usually methtlene chloride. Look up solvent-solvent extraction for the details.
c) With a difficult to separate mixture like yours, a) and b) can be used together.
If you have a mixture such as yours, trying to remove water by sodium sulfate is futile.
He who makes a beast of himself gets rid of some of the pain of being a man. --HST
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