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aga
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Spain.
I'm sure that a much larger boiling volume of 'mash' would NOT exhibit rapid temperature changes, and so the Real distilleries using Thumpers would
see little or no suck-back at all.
Their boiling pot Output would always be more than sufficient to overpower any pressure the Thumper could exert.
[Edited on 19-3-2015 by aga]
[Edited on 19-3-2015 by aga]
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Zombie
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You fought thru a series of hurdles to do all this. Kudos for all your efforts.
Your findings are in line with what I expected, and could not have been achieved if you did not apply such a valiant effort.
I also believe you numbers are correct. I have hit 99% Many times in column distillations, and several more times in "Triple distillations" using
nothing but a pot, and thumper. That level never holds due to the hygroscopic nature of EtOH but the numbers can be reached.
The action(s) explained are also to be expected. Distillation will stop as molar fractions change. More heat/power is required as the EtOH is
vaporized out. Generally there will be 3% EtOH in a "spent" boiler. Beyond that you are recovering more water than EtOH so distillation is impractical
at this level.
At this point I would suggest getting a 10Ml beaker, and some teeny/tiny ice cubes... nEnjoy!
They tried to have me "put to sleep" so I came back to return the favor.
Zom.
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aga
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Ah Crap.
What now ?
Edit:
99% would be an error.
Break the aeotrope with say CaCl2 and maybe.
[Edited on 19-3-2015 by aga]
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Magpie
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I agree that both the pot and the thumper are acting as distillation stages. I don't think, however, that condensation is a necessary part of this.
I would insulate all the way from the top of the pot, over to the thumper, and the thumper itself. The vapor coming off the pot is just at saturation
temperature and carries no superheat. It's on the verge of condensing from the git-go. So it needs a lot of insulation so that the heat can be
carried into the thumper instead of being lost to the environment.
The single most important condition for a successful synthesis is good mixing - Nicodem
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Zombie
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Unless you run thousands of distillations you would never believe 99% is real.
Fact is when a 100 gallon boiler is running for 7-8 hours, and has 9) 4" bubble plates, the combination of the heat in the system, and the purity at
the top can break the azeotrope.
Like I said... Iv'e done it with a simple pot / thumper. For fuel use we use Benzene to break the azeotrope. It's cheap, and readily available here.
If I were you I'd get the "I Broke Azeo" badge, and wear it proudly!
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aga
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I'll do a potassium iodide/sodium thiosulphate/potassium dichromate back-titration and find out for myself, and for sure.
That's the wonderful thing about Science : there's no need for speculation or argument where a proven experimental procedure is available.
Edit:
Breaking this particular azeotrope isn't simply a matter of how many TEPs there are or what fuel you use.
[Edited on 19-3-2015 by aga]
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aga
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By what measuring device are you claiming 99 w% ?
Edit :
Pardon me.
I forgot that shaking a bottle and looking at the bead size was the most accurate EtOH w% measuring method ever devised.
[Edited on 20-3-2015 by aga]
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Zombie
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Two floating Nova Tech.Alch meters, calibrated at 60*f.
The first is a general test, and the second is exact. I send them both in once a year to be calibrated.
I believe it is a matter of heat at the top of the column, and the near perfect separation at the 7th stage. Taking off product from the 7th stage is
azeotrope. Actually with a higher reflux ratio I can pull azeo. off of the 5th stage but I run at a faster rate, and add the extra plates.
At nine plates, and 182*f vapor temp. at the top of the column it is 99% consistently. It will not hold tho unless treated immediately w/ Benzine, and
sealed. I store EtOH in 15 gallon Polypropylene drums for fuel use.
http://www.novatech-usa.com/Products/Alcohol-Hydrometers/B61...
http://www.novatech-usa.com/Products/Alcohol-Hydrometers/661...
Left open to air it will return to Azeo usually within two hours in Florida. Depending on how fast you work at the titration you will see the
percentage drop on successive tests.
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aga
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7th stage ?
You have 7 Thumpers in your rig ?
[Edited on 20-3-2015 by aga]
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Zombie
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Nooooooo. I'm talking about a plated column in this case. One run beginning at 40% concentration. This is strictly a fuel still.
I have hit 99% on three successive runs thru a thumper tho, and there are several people I know that run 2 or three thumpers in line. Three is the MAX
you can run due to heat transfer losses.
They tried to have me "put to sleep" so I came back to return the favor.
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blogfast25
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I want to thank aga for the tremendous effort and time he's put into running this experiment.
But I cannot say I'm remotely satisfied with the results so far.
The aim was to compare distillate compositions using a thumper and without a thumper, in as near identical conditions as such a
comparison allows. Instead technical problems were encountered from the get go: unexpected suckback. To claim the comparison has been carried out is
like claiming the LHC found the Higgs Boson but with a seriously limping detector. No, first you repair the detector to how it's supposed to work,
then you carry on. Anything else gets you laughed out of court and rightly so.
I had also hoped the experiment would shed light on how the EtOH concentration of the distillate evolves during the run, and not yield a mere
single datapoint. This should have been fairly easy to achieve considering how well the refractometer performed and how little sample volume it
requires per analysis.
There are in the immediate responses above a number of things I strongly object to (not in the least Zombie's phantasmagorical "I broke the
azeotrope") but current poor health and other priorities prevent me from spending much time on them. Maybe later.
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aga
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Sorry, my mistake.
I thought you were referring to the OP's question.
Using a Standard Plate Equivalent distillation model is not thumper-related.
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blogfast25
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Quote: Originally posted by aga  | Sorry, my mistake.
I thought you were referring to the OP's question.
Using a Standard Plate Equivalent distillation model is not thumper-related. |
Sorry, but I really do not know what you mean, or even who you are addressing.
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Zombie
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| Quote: Originally posted by aga | Sorry, my mistake.
I thought you were referring to the OP's question.
Using a Standard Plate Equivalent distillation model is not thumper-related. |
Just answering the questions.
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aga
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As to Blogfast25's comments, all i can say is Humbled.
In the light of those comments, it is now Obvious that i've just heated stuff up and written stuff down, then thought i Knew something.
Feck.
More Thinking required before randomly doing stuff and thinking i've somehow done anything significant.
Further experimentation to follow, hopefully with more robust data.
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Zombie
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| Quote: Originally posted by blogfast25 |
There are in the immediate responses above a number of things I strongly object to (not in the least Zombie's phantasmagorical "I broke the
azeotrope") but current poor health and other priorities prevent me from spending much time on them. Maybe later. |
With all due respect, I'm not here posting B.S. just for the sake of having something to type.
If you want to debate theory, you win!
If you want to debate what "actually" happens in a distillation run, I have explained it all the best I can. Breaking Azeo is not anti gravity. It
happens.
I'm glad you saw the results, and hope you fell better soon.
They tried to have me "put to sleep" so I came back to return the favor.
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aga
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It'd be helpful if you did answer the more specific ones.
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Zombie
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Like?
They tried to have me "put to sleep" so I came back to return the favor.
Zom.
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aga
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I clicked it endless times, but this doesn't work like facebook.
Ah well, so the Thumper distillation Profile needs Properly comparing to a Standard distillation profile.
A new Project ! WooHoo !
This Learning thing is wonderful. Love it.
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blogfast25
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aga:
I would be happy, if the suckback problem cannot be overcome, with an experiment with an initially empty thumper, if possible using multiple EtOH
measurements over about 50 - 100 ml of distillate.
Zombie:
The claim that you broke the azeotrope is simply anti-scientific misinformation that should have no place on a science forum. I know
in your mind there's the 'world of booklearnin' folk and theory' and the 'real world of billies' but in reality, there is only one
world: one in which azeotropes cannot be broken the way you claim they can.
[Edited on 20-3-2015 by blogfast25]
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Magpie
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Zombie I'm trying to respect your skills and your extensive experience but telling me you broke the azeotrope with plates and heat is straining my
nerves. If you are correct you had better take out a patent quickly. Those industrial fuel manufacturers like Archer Daniels Midland are going to
want that technology bad. Then they won't have to waste all that money on running their mole sieve columns. 
The single most important condition for a successful synthesis is good mixing - Nicodem
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blogfast25
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| Quote: Originally posted by aga | In the light of those comments, it is now Obvious that i've just heated stuff up and written stuff down, then thought i Knew something.
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I think you may be a bit too hard on yourself but the difference between Good Science and Faulty Science is only a cigarette paper wide.
You're very close to solving this 'controversy' for once and for all. So lets try and do this.
Good luck: Good Science is seriously hard.
[Edited on 20-3-2015 by blogfast25]
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Zombie
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I won't beat this into the ground but I will say this.
In pressure swing distillation (which it appears Mr Aga, inadvertently achieved) you get different behaviors from azeotrope.
Even tho AT azeotrpe the mixture is basically at one boiling point the mole fraction can be shifted by varring the pressure.
These shifts in mole fractions show that the azeotrope can be broken.
Quote:
Pressure swing distillation[edit]
Azeotrope composition shift due to pressure swing.
A hypothetical azeotrope of constituents X and Y is shown in the diagram to the right. Two plots are shown, one at an arbitrary low pressure and
another at an equally arbitrary, but higher, pressure. The composition of the azeotrope is substantially different between the high- and low-pressure
plots – higher in X for the high-pressure system. The goal is to separate X in as high a concentration as possible starting from point A. At the low
pressure, it is possible by progressive distillation to reach a distillate at the point, B, which is on the same side of the azeotrope as A. Note that
successive distillation steps near the azeotropic composition exhibit very little difference in boiling temperature. If this distillate is now exposed
to the high pressure, it boils at point C. From C, by progressive distillation it is possible to reach a distillate at the point D, which is on the
same side of the high-pressure azeotrope as C. If that distillate is then exposed again to the low pressure, it boils at point E, which is on the
opposite side of the low-pressure azeotrope to A. So, by means of the pressure swing, it was possible to cross over the low-pressure azeotrope.
When the solution is boiled at point E, the distillate is poorer in X than point E. This means that the residue is made richer in X than point E.
Indeed, progressive distillation can result in a residue that is as rich in X as is required.
http://en.wikipedia.org/wiki/Azeotrope
I know my instruments are accurate I pay for them to be, and I can watch the gauge float back up to azeo.
They tried to have me "put to sleep" so I came back to return the favor.
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deltaH
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Zombie, even if you crossed the azeotropic point, you forget that the phase diagram flips at that stage and that vapour coming off
thereafter is, in fact, enriching in water, so it can't happen without a separate column or stage and collecting the bottoms as product.
Pressure swing distillation is conducted using two separate columns. First column brings it near the azeotrope, then the distillate is flashed into a
second column operating at very low pressure and the very concentrated ethanol is taken from the bottoms of the second column.
Distilling in the phase diagram region past the azeotropic point is also really difficult, because you will notice on the phase diagram that the curve
lies very close to the x=y line. That means a great many EXTRA stages are required to enrich those few extra percent in that region.
I believe that you got false readings because of the presence of contaminants (e.g ketones, other alcohols, whatever) that skew the result, so-called
matrix effects in analytical chemistry. You would need to calibrate with those contaminants present in order to get accurate readings, but that is off
course not practical, but just saying.
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aga
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| Quote: Originally posted by Zombie | | I know my instruments are accurate I pay for them to be, and I can watch the gauge float back up to azeo. |
It'd be more convincing if you could show us the test certs from the calibration people.
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