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EF2000
Hazard to Others
Posts: 147
Registered: 10-5-2023
Location: The Steppes
Member Is Offline
Mood: Taste testing the Tonka fuel
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Like that: https://www.orgsyn.org/demo.aspx?prep=CV1P0199
Synthesis of diacetone alcohol. They use Soxhlet extractor with thimbles filled with Ba(OH)2.
Wroom wroom
"The practice of pouring yourself alcohol from a rocket fuel tank is to be strongly condemned encouraged"
-R-1 User's Guide
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Organikum
resurrected
Posts: 2336
Registered: 12-10-2002
Location: Europe
Member Is Offline
Mood: frustrated
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Bisulfite did not work for anybody in a meaningful way, why do you not just follow your own advice? And try it out before repeating the old "should,
would, might" mantra?
The H2SO4 pumice works I can vouch for it. And it is much safer for having a very small actual reaction volume. Not to talk of the excellent TOF if
good quality alcohol is used.
Why is this, people always sending others on hopeless quests like this bisulfite crap?
"If in doubt, try it out!"
Absolutely.
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macckone
International Hazard
Posts: 2165
Registered: 1-3-2013
Location: Over a mile high
Member Is Offline
Mood: Electrical
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I have done the bisulfate method and produced ethyl ether.
You need DRY sodium bisulfate which is an added prep step. Out of the bag it contains more water than the monohydrate.
You do not dissolve the sodium bisulfate, you make a slush of ethanol and the powder.
Then you heat under heavy reflux until the slush is 140C.
Next you drip in additional ethanol. It is much slower than the sulfuric acid method.
I am uncertain as to the exact mechanism since this not been studied since sulfuric acid is readily available for most people outside of the EU and
that is recent.
My guess is that it is producing sulfuric acid in situ.
It is not as easy or fool proof as the sulfuric acid method.
It also builds up water quickly and the reaction ceases when it gets too 'wet'.
Doing this on a 10ml scale and expecting results is insane. I used a 1L RBF with about half filled with sodium bisulfate before adding ethanol.
I was on the verge of screaming at the number of times people said bisulfite in this thread. That is NOT what you need.
As for references, I originally got the idea from Mellor's.
It was mentioned that it produced less tar which was my primary interest in it.
The tar clean up is the worst. It requires piranha solution.
From a practical perspective, boiling down dilute acid is easier and will yield better results. Extracting the sulfuric acid from the sodium
bisulfate would be more reliable.
While this does work it is neither practical nor preferable if you have access to sulfuric acid. And given that you can extract sulfuric acid from
sodium bisulfate, you basically have access to sulfuric acid. You can also boil down 15% acid to get concentrated acid, which my understanding is
that 15% is available in the EU.
When I get time I need to do a proper write up so it is reproducible.
A few other notes about ethyl ether formation:
the diethyl sulfate decomposes to diethyl ether and sulfur trioxide when heated. So the ester formation is at least one pathway in the traditional
sulfuric acid method.
The ethyl hydrogen sulfate reacts with sodium sulfate to produce diethyl sulfate and sodium bisulfate.
oleum and ethyl ether produce significant tar when heated together.
Sodium sulfate can sequester a substantial amount of water. The commercial technical grade sodium bisulfate probably contains significant amounts of
sodium sulfate decahydrate out of the bag explaining the need to dry it.
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