| Pages:
1
2 |
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
Perhaps he wanted to point out that neutralizing sulfuric acid with sodium carbonate does not produce sodium bicarbonate, and denatured alcohol is not
just fine, and neither is refluxing.
Maybe he was going to say that 1-posters are full of shit but decided not to be so negative and obvious.
Better an old garbage thread than a brand new garbage thread.
I wonder how many people have died from heating this with nitrite without ventilation.
|
|
|
Fantasma4500
International Hazard
Posts: 1681
Registered: 12-12-2012
Location: Dysrope (aka europe)
Member Is Offline
Mood: dangerously practical
|
|
yes texium, the writing puzzled me for about half an hour, my brain just went on a standby and i knew my duty was to write it up in a proper way so
that others, if they realized what i had down one post further down wouldnt have to go through that, and i even ended up learning something that was
before incomphrehensive to me from my own corrections, it was very much a challenge that left my mind sore for a bit after. i see you also gave up on
the "projecting drips of the solution" bit, unless its just me that doesnt understand it- yet.
it is a very neat input he produced however, and as its his only post it would seem that he was either disgruntled that it left the thread dead
afterwards or simply died, it could be his dying breath and his last gift to this world.
i believe also the reaction of alcohol with NaHSO4 will become increasingly interesting as freedom is sodomized, one day at a time.
SC Wack, you mean to say that there must be some risidual acidic remains that generates some NOx? as for the credibility, the jumbled wordsalad would
entail that he might have had success with- whatever he was attempting.
|
|
|
S.C. Wack
bibliomaster
Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline
Mood: Enhanced
|
|
The reaction with nitrite generates more volatiles than the nitroalkane regardless, which is generally not mentioned.
It's hard to get past the whole dumbing down thing...there's a certain level that should not be crossed, and it's society in general. That something
may have been obtained is immaterial...Claesson mixed equimolar amts. acid and alcohol and heated to an unspecified point on a water bath for 15 min.,
diluted with water, neutralized with KOH, evaporated, extracted with boiling alcohol, obtained 52% yield of the salt...in 1879. (BTW he also extracted
a little ethyl sulfate with chloroform from such a diluted mixture, cooled with ice first)
|
|
|
Fantasma4500
International Hazard
Posts: 1681
Registered: 12-12-2012
Location: Dysrope (aka europe)
Member Is Offline
Mood: dangerously practical
|
|
i wanna chime in on this normally thought difficult process, typically 80mL H2SO4 is used with 180mL EtOH
-- why?
80mL H2SO4- 78g reacts with 36g EtOH?
one annoying step that really messes up this process is using Na2CO3. also long reflux time- 3H is normally advocated for
i found one youtube video that explains only refluxing for 30 minutes, and with my vague reflux lets call that an hour at just barely EtOH's BP, done
as simple as 500mL RBF with a 25mL erlenmeyer flask fitted upside down on the top and with a small container with water ontop of the flask
NaOH can be used just fine and prevents excessive foaming as with Na2CO3- and now comes the scientific part. when a liquid evaporates it cools down,
evaporative cooling. so having a bit of extra ethanol in will explain you when the neutralization is done, so you wanna add in NaOH solution rapidly,
the EtOH will do the cooling. once you add in NaOH solution and the EtOH doesnt shockboil out- then its neutralized, this easily cuts time spent on
this step to maybe 1/5 maybe even further
then the solution is cooled down as far as possible and filtered, the solution now is NaEtSO4 + Na2SO4 - at 0*C Na2SO4 is 4.9g/100mL - it seems
redundant to do EtOH extraction though thats easily done by heating up EtOH with the dried out solid and thereafter decanting and putting that in
freezer, a slushy crystal mass will be attained which can then easily be vacuum filtered- and then subjected to drying out once again- but as
practically all solids dissolved in the EtOH i wager this step as waste of time and resources
i found another user stating that alkaline pH causes NaEtSO4 to degrade, not even with NaOH this seems to be the case
care must also be taken to not excessively heat the NaEtSO4 as i found about 31% drop in weight after subjecting 0.81g of it in oven at 180*C for a
few hours
in short: 1:1 H2SO4:EtOH
reflux 1H 50*C
neutralize NaOH solution until EtOH doesnt boil up anymore
cool down
filter
boil dry
|
|
|
| Pages:
1
2 |
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
