Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by kimbodious »

Saltbush Bill wrote: Sun Jun 12, 2022 2:48 pm
kimbodious wrote: Sun Jun 12, 2022 1:12 pm I get greatest efficiency and highest purity when I run my CCVM with a stable level of bubbling condensate on top of the packing
Kimbo to get things perfectly clear, does that mean that you choose to run that still that way all of the time.....or just that you can if you want?
kimbodious wrote: Sun Jun 12, 2022 1:12 pm this and minimise the risk of flooding.
Does "minimise the risk of flooding" mean that it is still tricky to run that way and needs constant supervision or it can still easily flood?
I haven’t been lately but I can if I want. Yes it is tricky to run it right at the limits which is why I don’t usually. When I see liquid starting to pool I usually wind back the heating energy just until I see the odd bubble on top of the packing. There’d be an 8” gap between the top of the packing and the bottom of the offtake, It is a good idea to have that sized gap if you are going to run the column hard.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by kimbodious »

shadylane wrote: Sun Jun 12, 2022 8:33 pm And watch really close for the tails cut on a sugar wash run for neutral.
When the compressed tails finally gets out of a packed column it happens fast.
Towards the end of the run, Ya better be using small jars and changing them often. :ewink:
So true!
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by Saltbush Bill »

kimbodious wrote: Mon Jun 13, 2022 2:45 am Yes it is tricky to run it right at the limits which is why I don’t usually.
:thumbup: Thanks , thats all that I wanted to know.
So in short much less hassle to just take a more relaxed approach and take a little more time to make the run.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by cranky »

Saltbush Bill wrote: Mon Jun 13, 2022 3:58 am
kimbodious wrote: Mon Jun 13, 2022 2:45 am Yes it is tricky to run it right at the limits which is why I don’t usually.
:thumbup: Thanks , thats all that I wanted to know.
So in short much less hassle to just take a more relaxed approach and take a little more time to make the run.
Isn't that usually the best answer while distilling?
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by cranky »

shadylane wrote: Sun Jun 12, 2022 8:33 pm It sounds counter intuitive that a restriction might help.
I'm thinking the difference may be due to the size of the boiler to column fittings.
My 18ish gallon boiler has 4" tri-clamp outlet connecting the 4" packed glass column and I can't get the column to flood uniformly like your 2" boiler outlet adapted to a 4" glass column.

On my column any signs of flooding is detrimental to making neutral spirits.
The column works best when the packing looks wet, due to the reflux draining down and the rising vapor is invisible except for blowing a few bubbles in the reflux.

The way I run my column for neutral.
The foreshots/heads cut is easy, run max possible boiler power and reflux, while slowly dripping off the nasties. Then go, slow and steady for the hearts.
As the run progresses, the output will slowly decrease.
That makes timing the tails cut easier, due to the slower output.
And watch really close for the tails cut on a sugar wash run for neutral.
When the compressed tails finally gets out of a packed column it happens fast.
Towards the end of the run, Ya better be using small jars and changing them often. :ewink:
I think that everybody's still is different so we can't really make blanket statements about what can and can't be accomplished. Maybe it's the 2" connection, maybe it's the specific rocks I use, maybe their size or how they are packed or any number of factors. Also I've seen people state that they have to run a lot of power to maintain the "flood" but after initialy getting it up and ready to start taking off I can usually dial the power quite far back and still maintain everything where it needs to be. That is to say with the flood slowly dropping throughout the run.

I do tend to do a little bit of tweaking during the run, mostly because I use a reservoir and as the run progresses the reservoir starts to warm up so I watch the thermometer (I only need one) and when it increases only a slight amount, less than .5 degree f I adjust the water flow to bring the temp back down. When I can't maintain that temp any longer I switch to a tails jar.

Last night I read through some of my old posts. I have a photographic memory so I don't take notes but on the first product run on my packed column I posted about it and I think it's worth re-posting here.
cranky wrote: Tue Nov 03, 2015 7:52 pm The run went pretty good. No issues, no leaks, just a nice steady flow of 94% alcohol (this actually temperature corrected to over 95%) for the next 5 hours(I note that takeoff rate was a quart every 15 minutes) then the temp jumped up from 172.9 to 173.3 and I started collecting tails. Total tails collected was only about a half jar before there just wasn't anything left to collect and I shut it all down.

...the video is actually 2 combined into one. The first half is during equalization before I began taking off product, with the column almost completely flooded. I had to back off the heat considerably to keep it from flooding and get it to where it wanted to be...any higher than 3.8 (on the dial) and the column would start to fill up. Interestingly enough the difference in purity between a fully flooded column and one that only had a quarter or less fluid bed was about 2-4% ABV. So more power input actually resulted in slightly lower ABV but once the sweet spot was found it ran itself right to the end.
The details of what those numbers mean are,SSR controller, power is 238-240V, my V gauge is digital and wired to give input volts, not volts after the SSR so the voltage reading never changes more than minor fluctuations. Dial numbers go from 0 to 8.3, at 0 the Amp gauge reads .5A, at 8.3 it reads 20.5ish amps. At the referenced 3.8 on the dial the gauge reads 7.5-7.8A. Gauge accuracy is probably questionable but that doesn't matter because it's just a reference point.

I noted that there was a 2-4% ABV difference depending on flooding but that was really based on power input and dephlrg settings, not the actual state of what was in the column. After that first run the way I run the column is the column begins "flooded" and when I dial the dephleg in takeoff is 95+ and stays there as the flood slowly drops throughout the run but as noted pushing too hard resulted in the flood increasing which would eventually result in overflowing if left unchecked.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by MereCashmere »

drmiller100 wrote: Sun Jun 12, 2022 6:54 pm [
>>>>>>Better than 95 by a bit.

That is MIRACULOUS!!!!!!

And an indication you are pretty ignorant about distillation
If you think 95% is Azeo then I feel embarrassed for you after you made this comment. :oops:

Who’s gonna tell Dr Miller what the true measurement of Azeo is? It’s gonna break the poor guy….

Okay for the sake of the rest of the thread and cause I’m sick of people saying 95 all the time; after temp correction if your Proof and Tralles meter isn’t saying 97.2% then it’s NOT azeo. I’m sorry to burst your bubble.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by bunny »

So, are we finally getting down to the relationship between the number of theoretical plates in our columns and the calculated reflux ratio?

It seems to me there should be a formula (maybe not quite this simple) like TP x RR = XYZ where XYZ can now be compared to a numerical range similar to the formerly accepted vapor speed range (which I can't remember exactly) of 12 - 20 IPS.

I am very disappointed that so few have actually measured and determined the HETP of the exact packing they are using in their columns.

The first time I hit 97+ I could only curse the darkness. I ordered a new P&T to only find out it was 97++.
I felt pretty stupid and kept quiet. Then someone said it's not 95+, but 97+. As Murphy would have it, I have not broken a P&T, ever.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by bitter »

Azero is 95.6 ABW and that is 97.2 ABV I think thats what confusing people.

I need a taller glass cylinder as can't measure past 95.5% Now my runs are over that and in gallon jug with some tails tossed in that was lower ABV still showing 96.5% (was a stripping run.. just playing and learning to drive) And I can do that from 10-11% wash @ 3.2 LPH with SPP and by temp etc I believe getting 97.2% ABV but need glass to confirm :)

Also keep in mind temperature corection.

B
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by elbono »

I've been considering trying to measure my HETP.

I thought I would use the method Odin proposed when I find time. Do you have any alternatives?

Another data point I would like to know is my actual reflux ratio which maritimer posted a method to find.

I totally understand people not caring about these numbers but MY learning process works better with data I can digest.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by Mr Sippy »

elbono wrote: Mon Jun 13, 2022 9:48 am I thought I would use the method Odin proposed when I find time. Do you have any alternatives?
Read up on McCabe-Thiele method to get some background.

Maritimer posted some interesting analyses. I think a bit of it was flawed by relying on pure physics and not considering vapor liquid equilibria behavior. Not sure about his RR method though.

Also have a look at the hobbybrennan calculators for comparison.

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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by bunny »

elbono wrote: Mon Jun 13, 2022 9:48 am I've been considering trying to measure my HETP.

I thought I would use the method Odin proposed when I find time. Do you have any alternatives?

Another data point I would like to know is my actual reflux ratio which maritimer posted a method to find.

I totally understand people not caring about these numbers but MY learning process works better with data I can digest.
I like Odin's method. It seems a little difficult until you actually try it.

Bite the bullet and make several gallons ( I make 4) of a 10% ABV boiler charge from hearts, no heads, no tails. Don't use a wash or mash. This should give you a fairly clean and accurate azeo temp on 100% reflux (if you can reach it with your packing).

Now the idea is to remove as much packing as possible until you can no longer take off any azeo without regard to wattage.
Odin stresses to due a P&T temp corrected. I usually do that the next morning and adjust the temp of the sample to 60*
When you have done this accurately and indeed did take off azeo, measure the depth in cm of the remaining packing and divide by 15.

150cm = HETP of 10cm (typical scrubby HETP)
60cm = HETP of 4cm
45cm = HETP of 3cm
30cm = HETP of 2cm
22.5cm = HETP of 1.5cm


Some have tried to determine RR in VM by blocking off all of the reflux condenser area and the top opening.
They push all the vapor off through the product condenser and what they collect is their gross volume number to be compared to the take off number. I think this should be pretty close and more than likely, good enough.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by cranky »

MereCashmere wrote: Mon Jun 13, 2022 7:38 am
drmiller100 wrote: Sun Jun 12, 2022 6:54 pm [
>>>>>>Better than 95 by a bit.

That is MIRACULOUS!!!!!!

And an indication you are pretty ignorant about distillation
If you think 95% is Azeo then I feel embarrassed for you after you made this comment. :oops:

Who’s gonna tell Dr Miller what the true measurement of Azeo is? It’s gonna break the poor guy….

Okay for the sake of the rest of the thread and cause I’m sick of people saying 95 all the time; after temp correction if your Proof and Tralles meter isn’t saying 97.2% then it’s NOT azeo. I’m sorry to burst your bubble.
How about the definition of neutral spirit which is actually what matters even though everybody loves to talk about "azeotrope"

"Neutral spirits, also known as neutral alcohol, rectified spirits, rectified alcohol or ethyl alcohol is highly concentrated ethanol distilled until it reaches a min. ABV of 95% (190 proof). Neutral spirits can be made from grains, grapes, molasses, potatoes, and other agricultural origins. As the name suggests, neutral spirits are considered neutral in flavor, odor and are colorless."

azeotrope is nothing more than a bragging point that unless your making fuel doesn't really matter. What really matters is Neutral and thus 95+%.

Since this thread has gotten so far off the original stated reason for it's existence and no longer serves any real purpose I think I'm going to just stop reading it before it degrades even more.
Last edited by cranky on Mon Jun 13, 2022 1:01 pm, edited 1 time in total.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by kimbodious »

Saltbush Bill wrote: Mon Jun 13, 2022 3:58 am
kimbodious wrote: Mon Jun 13, 2022 2:45 am Yes it is tricky to run it right at the limits which is why I don’t usually.
:thumbup: Thanks , thats all that I wanted to know.
So in short much less hassle to just take a more relaxed approach and take a little more time to make the run.
Yeah I even detuned the column by removing some of the packing. That means I can increase the heating energy even a bit further with less risk.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by drmiller100 »

I ran the numbers a couple of months ago.

Theoretical Reflux ratio depends on. A few factors

Assume you want azeo out th top.
10 percent beer will have a lower reflux ratio than 5 percent.

From memory, if you have perfect packing (any packing can be perfect if you have enough of it) and 10 percent beer you will reflux a minimum of 70 percent.

There is no way around this except continuous or making stripper runs.
Now I know how you claim azeo so easy, it's based on a meat thermometer. :lol:
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by elbono »

bunny wrote: Mon Jun 13, 2022 12:01 pm I like Odin's method. It seems a little difficult until you actually try it.

Bite the bullet and make several gallons ( I make 4) of a 10%
The biting of the bullet is my issue, I have honed my skills of procrastination to the point it is an art. My last sugar wash was intended to be used for this, I've consumed too much of it now.

The method didn't strike me as difficult more like tedious. It's been a while I studied that thread I'll give it a fresh read.

I'm using Piotr's spp. The first time I used it I got product I judged as azeo but that was a practical judgement not analytical. I read it at 97 abv that day, later did a more controlled measurement with temp correction and called it 97.2 abv. I bought a liter but got more like 1.2 liters that stacks up to about 58 cm in my 2" type m column.

Here's a snip from his website:
Sprężynki pryzmatyczne
Below we present the technical characteristic of the rings:

material – acid-resistant stainless steel AISI 304
specific weight – 880 g/dm3
dimensions – 4,4 x 5,5 x 0,24 mm
specific surface (p/v) – 1900 dm2/dm3
free volume – 0,89
maximumheat load – 115 W/cm2
HETP – 1,6 mm

According to that I should have around 36-37 theoretical plates. Plenty to get azeotrope. I still want to measure.

I've seen some posts from the early days of spp that said more power (to a point) means shorter HETP with spp. I need to search those out again. That could lead to another experiment find a HETP vs power density relationship.
Mr Sippy wrote: Mon Jun 13, 2022 11:43 am Read up on McCabe-Thiele method to get some background.
I took a quick skim of Wikipedia's entry. I should have expected chemical engineers to have something like this but never thought to look. My chem e college roommate (long ago) was suitably impressed when I sent him pics of my "fractional distillation plant". I'll study this in detail soon. Another rabbit hole to explore!
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by MereCashmere »

cranky wrote: Mon Jun 13, 2022 12:54 pm
MereCashmere wrote: Mon Jun 13, 2022 7:38 am
drmiller100 wrote: Sun Jun 12, 2022 6:54 pm [
>>>>>>Better than 95 by a bit.

That is MIRACULOUS!!!!!!

And an indication you are pretty ignorant about distillation
If you think 95% is Azeo then I feel embarrassed for you after you made this comment. :oops:

Who’s gonna tell Dr Miller what the true measurement of Azeo is? It’s gonna break the poor guy….

Okay for the sake of the rest of the thread and cause I’m sick of people saying 95 all the time; after temp correction if your Proof and Tralles meter isn’t saying 97.2% then it’s NOT azeo. I’m sorry to burst your bubble.
How about the definition of neutral spirit which is actually what matters even though everybody loves to talk about "azeotrope"

"Neutral spirits, also known as neutral alcohol, rectified spirits, rectified alcohol or ethyl alcohol is highly concentrated ethanol distilled until it reaches a min. ABV of 95% (190 proof). Neutral spirits can be made from grains, grapes, molasses, potatoes, and other agricultural origins. As the name suggests, neutral spirits are considered neutral in flavor, odor and are colorless."

azeotrope is nothing more than a bragging point that unless your making fuel doesn't really matter. What really matters is Neutral and thus 95+%.

Since this thread has gotten so far off the original stated reason for it's existence and no longer serves any real purpose I think I'm going to just stop reading it before it degrades even more.

Lol this is the second time you’ve said that within 24 hours; instead of clogging this thread up with whining just leave already :mrgreen:

Also, let’s have some respect for our non American members, where Neutral alcohol isn’t always 95%. In Russia it’s actually 96% and above.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by cranky »

MereCashmere wrote: Mon Jun 13, 2022 2:49 pm Lol this is the second time you’ve said that within 24 hours; instead of clogging this thread up with whining just leave already :mrgreen:
The petty insults are why I said it a second time and partially why this thread has become useless. Scow's original thread on this subject was far more informative.

You drew me in one more time, there won't be another, Y'all should learn to be respectful and try to keep threads on topic.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by shadylane »

cranky wrote: Mon Jun 13, 2022 12:54 pm
...How about the definition of neutral spirit which is actually what matters even though everybody loves to talk about "azeotrope"

"Neutral spirits, also known as neutral alcohol, rectified spirits, rectified alcohol or ethyl alcohol is highly concentrated ethanol distilled until it reaches a min. ABV of 95% (190 proof).... As the name suggests, neutral spirits are considered neutral in flavor, odor and are colorless."

azeotrope is nothing more than a bragging point that unless your making fuel doesn't really matter. What really matters is Neutral and thus 95+%.
Don't run off yet Cranky your experience, opinions and knowledge is valuable. :lol:

I agree trying for azeotrope is nothing more than a bragging right.
But I disagree that neutral spirits needs to be 95% plus.
Even if a column can make 95% that doesn't mean the alcohol is neutral.
I can make neutral spirits with a column that isn't capable of high ABV.
All that's needed is to do a fast reflux stripping run, dilute then redistill again with reflux.

I could do a one run and done trying for azeo at a slow drip with the column semi flooded.
Or I can distill twice at a much faster takeoff rates and get a better neutral. :ewink:
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by Yummyrum »

I would agree that the number is not as important as the purity of the desired spirit .
I’d rather drink some hearts that come off at 95% than the heads that dripped out at 97% .

I applaud those that have the time and patients to pull off Azeo for the full run .I respect those that like me , have neither the time ( or money to invest in expensive packings) and are still able to produce a clean tasting neutral .
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by bitter »

Honestly pure neutral I find boring.. but great as a base for gin.

I have had some wheat pot still whiskeys and there were amazing. lots of runs to get there but guy only had a pot setup. Run cuts dilute and run a few times. Feints we put in a wheat whiskey run as were larger percentage. It can be done in different ways.

My 2" would azero.. but 3" till went SPP was harder to get there. Now with SPP its easy. No need for 40% in boiler..

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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by DAD300 »

Lot went on while I wasn't listening...

I can get a very neutral (flavorless) spirit at 85% or better ABV. neutral depends more on the wash and how many times it has been rerun, not how many plate it has passed, but run, diluted, run again. Every rerun, diluted with water and rerun removes more and more of the pollutants (especially the yeast).

Running packing flooded or more wet, passes more flavor toward the top. Slower, drier packing refluxes more pure alcohol, less water and it's the water carries the flavors.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by DAD300 »

flooding vs diameter...

With enough power I can flood a 4" x four foot column packed with SPP, to any level desired.

But this has a lot to do with column dia, size of SPP and power available.

Tiny SPP in a larger column is easier, takes less power, to flood than properly sized SPP.

A 2" column with 800watts should have smaller SPP than a 3" with 1,500watts or 4" with 4,500watts.

Same can be a fact with SS Scrubbies packed looser or tighter. Denser/tighter packing will transfer more heat and slow downward reflux, thus flooding easier!
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by cmac62 »

Thanks for sharing and replying everyone.
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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by StillerBoy »

DAD300 wrote: Thu Jun 23, 2022 7:03 pm Running packing flooded or more wet, passes more flavor toward the top. Slower, drier packing refluxes more pure alcohol, less water and it's the water carries the flavors.
I'm not in agreement with the above, as experiment done with my setup, indicates differently, as purity is higher with a semi flood state, but it has to be within reason like 1/2 - 3/4" otherwise yes water will be carried and done with the right setup/unit.. again the experiments I've done were using an concentric LM mainly, and I know that an VM is very touchy in semi flooded.. but there are many factors that come into play, and that most, either don't realize what is happening within there setup, or have not develop understanding of how to work their unit, which takes more than a few runs..

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Re: Semi- fluidized bed/ semi- aquatic state/ semi- flooded Etc.

Post by zukram »

Old thread, but you can check out this:
viewtopic.php?p=7779402#p7779402

About controlling the flooding level.
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