Getting a Pot Still to Reflux
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Getting a Pot Still to Reflux
Wow. Haven't posted in about 2 years!
My pot still consists of a 20L tea urn, with a 22mm pipe up from the lid, leading to a liebig condenser at 45 degrees.
The urn has a 2kW element, but I reduce the power to 25%-50%.
I've cut the vertical column and patched in a 1m length of 28mm diameter pipe. I've filled the pipe with ceramic raschig rings.
- Should the extra surface area and height cause any useful / measurable amount of reflux to happen?
- What will be the effect (if any) of going from 22mm above the boiler to 28mm for the column and back down to 22mm just before the condenser? (The condenser core is actually 15mm.)
- Will there be any additional (useful) effect if I add a few turns of 8mm copper pipe at the top of the column (before the vapour turns the corner into the condenser) and run cold water through that?
Comments on design would be great, please.
My pot still consists of a 20L tea urn, with a 22mm pipe up from the lid, leading to a liebig condenser at 45 degrees.
The urn has a 2kW element, but I reduce the power to 25%-50%.
I've cut the vertical column and patched in a 1m length of 28mm diameter pipe. I've filled the pipe with ceramic raschig rings.
- Should the extra surface area and height cause any useful / measurable amount of reflux to happen?
- What will be the effect (if any) of going from 22mm above the boiler to 28mm for the column and back down to 22mm just before the condenser? (The condenser core is actually 15mm.)
- Will there be any additional (useful) effect if I add a few turns of 8mm copper pipe at the top of the column (before the vapour turns the corner into the condenser) and run cold water through that?
Comments on design would be great, please.
Re: Getting a Pot Still to Reflux
With out forced reflux and a way to initiate multiple phase change cycles ( Plates. Theoretical or actual) you'll only ever get a very small amount of abv boost.
The added height will however allow you to fashion your apparatus to set up a counter top collection height.
Maybe not an issue if you're not a crusty old dude.
The added height will however allow you to fashion your apparatus to set up a counter top collection height.
Maybe not an issue if you're not a crusty old dude.
Trample the injured and hurdle the dead.
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Re: Getting a Pot Still to Reflux
This is something I am interested in. Why don't you do a series of washes - all made the same at say 10% abv then gather the output in jars and proof them individually ?eStill wrote: ↑Thu Aug 29, 2019 1:46 pm Wow. Haven't posted in about 2 years!
My pot still consists of a 20L tea urn, with a 22mm pipe up from the lid, leading to a liebig condenser at 45 degrees.
The urn has a 2kW element, but I reduce the power to 25%-50%.
I've cut the vertical column and patched in a 1m length of 28mm diameter pipe. I've filled the pipe with ceramic raschig rings.
CompleteStill.jpg
- Should the extra surface area and height cause any useful / measurable amount of reflux to happen?
- What will be the effect (if any) of going from 22mm above the boiler to 28mm for the column and back down to 22mm just before the condenser? (The condenser core is actually 15mm.)
- Will there be any additional (useful) effect if I add a few turns of 8mm copper pipe at the top of the column (before the vapour turns the corner into the condenser) and run cold water through that?
Comments on design would be great, please.
Then try your cooling coil idea and repeat the same procedure ?
Then perhaps make a Short column of 18" or so and attach your liebig to that so as to see how the 3 designs perform against each other ?
Personally I think it Will make a difference - but as to how much ? I don't know - but we do sort of argue about this a little here sometimes and a proper experiment, showing the abv contents of each jar for all 3 runs would be great !
Consider yourself delgated to increase the knowledge of the forum !
Re: Getting a Pot Still to Reflux
Cooling coil definitely works somewhat. I used to have a little outer cooling coil column I used
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Re: Getting a Pot Still to Reflux
I suppose that was part of the question. Does a column full of disruption not give me a theoretical plate? I did my cleaning run with old heads. First thing I noticed was that the top of the column was 2.5 degC cooler than the bottom. Previously, there was maybe only half a degree difference. I hoped that meant some condensation on the raschig rings.
I pinched my sciatic doing karate last month. So, feeling fairly crusty at the moment.
Re: Getting a Pot Still to Reflux
The good news is I can easily empty the column.
My Raspberry Pi will happily log the temperature with time and I use the table from the mothersite to graph ABV over the duration of the run. So, I have data. The trouble is I never took a log of what the initial ABV was, at least not for the first pass. on subsequent stripping runs, I normally dilute to 40-50% first, but it's never what you would call "exact".
Now you're making it sound like hard work. I have data from when the column was 18mm diameter and only 300mm long. Again, the asshole is I don't know what the initial ABV of the wash was. Frankly, I think this stuff had less taste than with the long column. (When using Turbo Yeast, that's a GOOD thing!!)
Dammit, now you're bribing me with kudos!! It's difficult to resist!Pikey wrote: ↑Thu Aug 29, 2019 2:45 pm Personally I think it Will make a difference - but as to how much ? I don't know - but we do sort of argue about this a little here sometimes and a proper experiment, showing the abv contents of each jar for all 3 runs would be great !
Consider yourself delgated to increase the knowledge of the forum !
Re: Getting a Pot Still to Reflux
Interesting thing: pressure. There is now pressure in my kettle. What does that mean? To me, it seems to indicate that there is too much heater power. If the vapour is under pressure, it means it's being forced up the column, rather than rising of its own accord.
Re: Getting a Pot Still to Reflux
Pressure? It may mean you have column flooding or column blockage. Not a good thing. In a well designed column the column cooler, by phase shifting gasses back to liquid, creates de facto under pressure (gasses collapsing to liquid state loose 99.9% of their volume), pulling the vapors upwards through the column. If you get pressure in your boiler, you are down the wrong path. Potentially very dangerous. You need a more free vapor path, lower power input and/or more cooling capacity.
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Regards, Odin.
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Re: Getting a Pot Still to Reflux
Sure, you'll get an improved abv. But with out a way to force reflux in conjunction with multiple phase change cycles, you'll never exceed / hold 87% for the duration.eStill wrote: ↑Fri Aug 30, 2019 10:38 amI suppose that was part of the question. Does a column full of disruption not give me a theoretical plate? I did my cleaning run with old heads. First thing I noticed was that the top of the column was 2.5 degC cooler than the bottom. Previously, there was maybe only half a degree difference. I hoped that meant some condensation on the raschig rings.
I pinched my sciatic doing karate last month. So, feeling fairly crusty at the moment.
Maybe not a big deal. Especially if you're making whiskey.
Trample the injured and hurdle the dead.
Re: Getting a Pot Still to Reflux
Hmmm. I get the phase change / volume bit. But the change from liquid to vapour is what's creating pressure.Odin wrote: ↑Fri Aug 30, 2019 12:15 pm Pressure? It may mean you have column flooding or column blockage. Not a good thing. In a well designed column the column cooler, by phase shifting gasses back to liquid, creates de facto under pressure (gasses collapsing to liquid state loose 99.9% of their volume)
The rig was fine and the condenser was adequate until I packed the column. I have a feeling there's too much input power. Will try 25%.
Re: Getting a Pot Still to Reflux
28mm might be enough for a riser on a pot still, but I reckon you are being a bit overly hopeful thinking you can use it for a tall reflux still. The vapor speed will always be a problem and will prevent the reflux from falling back down the column. If you want some speed, get yourself down to the scrap yard and find yourself a decent sized piece of copper and build something that isn't going to give you problems for the next forty or fifty years.
Re: Getting a Pot Still to Reflux
Copper must be worth very little in NZ! Scrap copper is a real struggle for me. It ain't chap. You are undoubtedly correct, though.
Re: Getting a Pot Still to Reflux
You asked for it!! OKay, 3 off 1 gallon runs, with fresh wash at 15%. Top temp is the temperature at the top of the column. Bot temp is the vapour in the kettle. ABV is calculated from the lookup table in the mothersite based on the vapour temp of the eutectic mix. Coolant temp is the temperature o the water exiting the Liebig. It continually rises because it's being recirculated. First is with the 28mm column full with about 400g raschig rings. You can see an increase in bot temp, a decrease in ABV and a more rapid rise of coolant water temp. that's because the distillate was only dripping out and I shifted the power up from 20% to 35%. (That's 20% of 2kW into 4.5 litres.) I stopped the heater when the top vapour got to 95 degC. What's interesting is that with the reduced input power, the top temp is about 5 degrees less than the bottom, but when I hike the power, the difference is only about 3 degrees. I'm not sure I trust these temperatures exactly (95 degrees seems VERY high), but I trust the difference between the top and bottom. Yielded up 1.2L at 65% (including heads - nothing discarded).
Second is with the column only half full of beads.The delta from bot temp to top temp has stayed the same: 3 degrees. Already I can see that the most influential variable there is the input power. Critically, the result was 1.2L at 65%. The quantity of beads has made no difference. Maybe it will if I chill the beads with my coil later. Third run with no beads yields exactly the same result. Same quantity, same overall ABV, same duration of run. That's just irritating. Packing the column has done nothing, but give me pressure in my kettle. Need to think about active reflux. In summary:
Re: Getting a Pot Still to Reflux
In the book "The Compleat Distiller", by Nixon, your kind of still is considered.
Nixon calls it a "fractionating still". It's a modified pot still which has a packed column, no forced reflux, and a normal liquid-cooled final condenser.
According to Nixon, such a still can actually be made to reflux quite a lot, provided that the temperature applied to the system is carefully chosen.
You find a description of such a still at pag. 37 - 38
In particular:
"In a 1 meter (just over a yard) fractionating column filled with high-efficiency packing, hundreds or
even thousands of condensation and re-evaporation cycles take place. This is equivalent to re-distilling
dozens of times with a pot still. The net result is a product with a very high percentage of volatiles
indeed, even up to 90%. The key limitation of a fractionating column is that the vapor flow must be
slow enough for the fractionating process to work efficiently. In a fractionating still, the relationship
between fractionating column capacity and boiler energy input is critical."
Pag. 53
"There is considerable leeway in the operation of a fractionating
column, but remember that the more slowly the vapor rises up
the column, the more efficient the fractionating process will be.
We have found that it works best to limit the heater element to no
more than 1 kW for a 50mm (2 inch) column."
But he also says that such for such a still "the slower, the better", which is unsurprising as you have to let air to the job which water would do much more effectively.
In your case, that would mean probably governing your still, once you reach evaporation, at less than 250 W or less
(the diameter is 1/2 of the diameter considered by Nixon, so the section is around 1/4, 250W would be the "limit" indicated by Nixon for your still I suppose, but "the slower the better", so you can use it at much less than that, very slowly!).
I hope you like Opera, especially long operas, try Wagner while you distill
Maybe you could try some wet rag on the top of the column, as a work-around, to be constantly renovated.
Ultimately it can be done, but at an excruciatingly low speed and I wonder, besides the cultural-academic interest, what's the point of such a still for normal production. After the first two runs, you'll want to add a water-cooled dephlegmator. You already have to have water for the final condenser after all.
The only practical use for such a still IMHO would be using a very long air-cooled spiral final condenser, so that the entire still can be operated without any need of water.
Nixon calls it a "fractionating still". It's a modified pot still which has a packed column, no forced reflux, and a normal liquid-cooled final condenser.
According to Nixon, such a still can actually be made to reflux quite a lot, provided that the temperature applied to the system is carefully chosen.
You find a description of such a still at pag. 37 - 38
In particular:
"In a 1 meter (just over a yard) fractionating column filled with high-efficiency packing, hundreds or
even thousands of condensation and re-evaporation cycles take place. This is equivalent to re-distilling
dozens of times with a pot still. The net result is a product with a very high percentage of volatiles
indeed, even up to 90%. The key limitation of a fractionating column is that the vapor flow must be
slow enough for the fractionating process to work efficiently. In a fractionating still, the relationship
between fractionating column capacity and boiler energy input is critical."
Pag. 53
"There is considerable leeway in the operation of a fractionating
column, but remember that the more slowly the vapor rises up
the column, the more efficient the fractionating process will be.
We have found that it works best to limit the heater element to no
more than 1 kW for a 50mm (2 inch) column."
But he also says that such for such a still "the slower, the better", which is unsurprising as you have to let air to the job which water would do much more effectively.
In your case, that would mean probably governing your still, once you reach evaporation, at less than 250 W or less
(the diameter is 1/2 of the diameter considered by Nixon, so the section is around 1/4, 250W would be the "limit" indicated by Nixon for your still I suppose, but "the slower the better", so you can use it at much less than that, very slowly!).
I hope you like Opera, especially long operas, try Wagner while you distill
Maybe you could try some wet rag on the top of the column, as a work-around, to be constantly renovated.
Ultimately it can be done, but at an excruciatingly low speed and I wonder, besides the cultural-academic interest, what's the point of such a still for normal production. After the first two runs, you'll want to add a water-cooled dephlegmator. You already have to have water for the final condenser after all.
The only practical use for such a still IMHO would be using a very long air-cooled spiral final condenser, so that the entire still can be operated without any need of water.
Re: Getting a Pot Still to Reflux
OKay. This unequivocally proves it.
OKay, so, I demonstrated what you all already told me!
The previous three experiments were about 90 minutes. How the hell is my still producing higher ABV distillate in a shorter time with a small amount of forced reflux?
I re-added about 100g Raschig rings, AND modified my column with an external cooling coil (7.5 turns of 8mm pipe, 3/4 the way up the column). I used 40% of my 2kW heater. Based on the 1.1L of distillate at 70% (SEVENTY!) ABV over a time of only 1 hour. The temperature delta from botton to top has shifted from 2 or 3 to about 6 or 7 degrees!
OKay, so, I demonstrated what you all already told me!
The previous three experiments were about 90 minutes. How the hell is my still producing higher ABV distillate in a shorter time with a small amount of forced reflux?
Last edited by eStill on Sat Sep 07, 2019 12:08 pm, edited 1 time in total.
Re: Getting a Pot Still to Reflux
Oh, here's another interesting thing. I normally kill the boiler when the top temperature hits about 95 degrees. With the coil added, once the top vapour temperature reached about 93 degrees, the reflux appears to have been significant enough that there was no distillate getting to the Liebig!
Oh, yeah: see the little rise in top vapour temperature about 18:40? that's me turning down the flow through the coil just to see what would happen.
Oh, yeah: see the little rise in top vapour temperature about 18:40? that's me turning down the flow through the coil just to see what would happen.
Re: Getting a Pot Still to Reflux
Yes, and this kind of thinking is what's taught at school in chemistry lessons and is what led me to stupidly, blindly, assume it would fractionate. Nothing I learned at school ever turned out to be the truth.
...which is the bloody important bit which is omitted!
Insight and, evidently, truth.
Gawd, no.
Precisely that! Nobody believes me, but this started out with my 15 y/o asking me if I could show him how to solder pipes. After we made an apprentice piece, I realised it was a heat exchanger. In fact, it's the one unmodified, original component of my still: the Liebig.
THAT's next!
Re: Getting a Pot Still to Reflux
This time, with only about 30grams of beads in the column. The pressure is musch less evident.
Again, 1 hour to obtain 1100ml at 70% from an initial 4.5L which had been at 15%. Again, it seems to have self-arrested at about 50% ABV. I am tempted to ramp up the heater power now that the pressure isn't building. There's still a good lot some useable alcohol in the kettle, but it tastes a bit like a wet dog.
See the little kinks at about 10:40? I can't exaplain them; it's about 20 minutes after I slid the coil down from the top of the column to the middle.
Next is to run a couple of gallons at 40%, take off some heads.
Again, 1 hour to obtain 1100ml at 70% from an initial 4.5L which had been at 15%. Again, it seems to have self-arrested at about 50% ABV. I am tempted to ramp up the heater power now that the pressure isn't building. There's still a good lot some useable alcohol in the kettle, but it tastes a bit like a wet dog.
See the little kinks at about 10:40? I can't exaplain them; it's about 20 minutes after I slid the coil down from the top of the column to the middle.
Next is to run a couple of gallons at 40%, take off some heads.
Re: Getting a Pot Still to Reflux
15% of 4.5L is 675ml raw. 70% of 1.1L is 770ml.
I suspect my calculation of the initial ABV was out. It was based on SG,but I guess if the wash wasn't completely clear, it would have appeared artificially dense.
Re: Getting a Pot Still to Reflux
Pass 2. Diluted the above first pass with tapwater, then ran it again. Produced 1.6L @ 81% from 4.5L at 45% in 90 minutes. Power set to 35%.
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Getting a Pot Still to Reflux
In a long and contentious thread about spirit runs on pot stills, I did an experiment which will help you to visualize the effects of passive reflux and compare them to the effects of active reflux with real plates.
Here is the thread: viewtopic.php?f=15&t=58627&start=330
Look for my post on Jan 30, 2016. (Comment #334?) Hope that helps.
Here is the thread: viewtopic.php?f=15&t=58627&start=330
Look for my post on Jan 30, 2016. (Comment #334?) Hope that helps.
Trying to make it real compared to what?
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Re: Getting a Pot Still to Reflux
My hunch is that this is completely accurate. I didn't harvest any data, but I spotted a funny break point in my pot still. i'd turn the power donw, down, down... all that would happen is the run took longer. Then I hit a point where the temperature at the top and bottom of the column diverged suddenly. It was a sure sign of proper reflux. My distillate went up from 70% to 80% as reflected here with the introduction of forced reflux. The problem I found was that if I went much below this sweet spot,t here wasn't quite enough power input to get the vapour to rise as far as the Liebig!!Badmotivator wrote: Ironically, it only works to the extent that your pot still is actually behaving like a reflux still.
I'm interested t learn: what was the conclusion about insulation? My kettle is insulated (I think it's efficient), but I leave the lid and the column un-insulated (I thin kit helps with reflux).
Incidentally, I love the wooden box and the fact that your still is just sitting there like it's the kind of regular white goods everyone has in their kitchen!!
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Re: Getting a Pot Still to Reflux
With a coil of water , you have a Coolant Management still .My distillate went up from 70% to 80% as reflected here with the introduction of forced reflux. The problem I found was that if I went much below this sweet spot,t here wasn't quite enough power input to get the vapour to rise as far as the Liebig!!
In these stills , the amount of cooling is balanced against the amount of heat you pit into the boiler.
Normally in a CM still you have the power fixed and adjust the coolant flow through the coil .
You are doing it the other way .... fixed cooland and adjustable power .
The result is the same either way ... reflux increases until it is at 100% and nothing comes out as product.
Sounds like its working perfectly normal to me
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Re: Getting a Pot Still to Reflux
As already said, with the addition of the water-cooled copper coil around the column you have a proper dephlegmator and you fell back into the normal reflux still case, in you case a CM still.
In a CM still, you have the dephlegmator on top of the column, just before the elbow which leads to the final condenser.
Many say you should insulate the column (and the lid of the kettle, or the entire kettle) in order to save energy, heat your room less, and avoid "channeling" along the walls of the column, which are cooler than the packing.
The price to pay is the lack of "copper porn"
If, instead, you really want to run your column as an "air-cooled" reflux column, that doesn't only mean a very small amount of heat and an extremely slow production rate, but an un-insulated column, because it's the air around the column which creates the reflux. Instead of the insulation, you should theoretically apply some fins in order to obtain a heat sink.
Again, this makes no sense unless you have the need to still in a waterless environment, or you chase academic knowledge