Glass Marbles for Reflux Column Structured Packing

Distillation methods and improvements.

Moderator: Site Moderator

woodshed
Master of Distillation
Posts: 2970
Joined: Tue Aug 27, 2013 5:21 pm
Location: Pagosa Springs,CO

Re: Glass Marbles for Reflux Column Structured Packing

Post by woodshed »

Great thread rad. Thx
Lester
Swill Maker
Posts: 250
Joined: Wed Sep 11, 2013 9:23 pm
Location: Cavite, Philippines

Re: Glass Marbles for Reflux Column Structured Packing

Post by Lester »

I mentioned in another topic about how I have used marbles for several years in my short stripping column... I've used as few as a dozen with no extension up to a jar full in a 6" stripper column...
Rad, pardon my ignorance. What did the marbles do for you in a stripping column?
Life is not about waiting for the storm to pass, it's about learning how to dance in the rain.
Reboiler: http://homedistiller.org/forum/viewtopi ... =1&t=43653
Thermometer: http://homedistiller.org/forum/viewtopi ... =2&t=43379
rad14701
retired
Posts: 20865
Joined: Wed Dec 19, 2007 4:46 pm
Location: New York, USA

Re: Glass Marbles for Reflux Column Structured Packing

Post by rad14701 »

Lester wrote:
I mentioned in another topic about how I have used marbles for several years in my short stripping column... I've used as few as a dozen with no extension up to a jar full in a 6" stripper column...
Rad, pardon my ignorance. What did the marbles do for you in a stripping column?
When I stripped with the needle valve in place I had unwanted reflux and those few marbles bumped and stabilized the %ABV of the spirits compared to running without... More of a hybrid run than reflux or pot...
User avatar
Red Rim
Trainee
Posts: 806
Joined: Sun Apr 06, 2014 3:14 am
Location: Orygun

Re: Glass Marbles for Reflux Column Structured Packing

Post by Red Rim »

Now damn it Rad!

After seeing your still you are going to force me to fiddle with mine. It is a 4 foot tall column with one inch pipe. I think I could stuff a reflux extension on the top of it and I may as well stuff it full of marbles and try it your way. Instead of stainless steel scrubbies, I have fine copper wire like Bushman uses in his, that I may place in the top and bottom.

Everything else you have been preaching to us is correct, I may as well try this too.
There is no such thing as a stupid question....... Unless you didn't research it first.
TheBackYarder
Novice
Posts: 20
Joined: Thu Jun 26, 2014 2:10 am
Location: AUSTRALIA

Re: Glass Marbles for Reflux Column Structured Packing

Post by TheBackYarder »

interesting shit Rad ...........now i want to fill my 3 inch boka up with marbles now hahaha
rad14701
retired
Posts: 20865
Joined: Wed Dec 19, 2007 4:46 pm
Location: New York, USA

Re: Glass Marbles for Reflux Column Structured Packing

Post by rad14701 »

I'll be interested in hearing any results that others experience... This has been on my list of things to try and I've had the marbles for at least six months... I did one run a while ago with a shorter column but the wash I tried running was the problematic component of that attempt...
User avatar
wv_cooker
Trainee
Posts: 933
Joined: Fri Feb 22, 2013 11:48 am

Re: Glass Marbles for Reflux Column Structured Packing

Post by wv_cooker »

Ok Rad stopped by the dollar tree this am while transporting the wife to work and here is the results LOL.
IMG_20140702_112017_0.jpg
IMG_20140702_112017_0.jpg (28.68 KiB) Viewed 4701 times
These are the little decorations for filling vases and glasses and such. They are about the size of a dime which should be good for my 3". They are also concave on one side and convex on the other. I am thinking as GA stated lot's of good surface area for liquid and vapor to react with each other. Holding a bag up and looking it seems they compact really well. The area between them looks like an excellent vapor and liquid path.

So off to boiling them to crack the surface a bit which should be as good as etching and hopefully create a nice scrubbing action between liquid and vapor. I am assuming my 2 - 30 gallon ferments will complete by next week so I should be able to do at least 4 runs, 2 of BW for neutral and 2 of UJ for some flavor. Will keep ya posted.

@ gaflatwoods

I don't know how I could have built something like this lol. Must have been Rad's teachings. Of course the other 3 I am finishing aren't much either lol. Pics to follow soon.
User avatar
ga flatwoods
Master of Distillation
Posts: 3192
Joined: Tue Feb 19, 2013 6:40 pm
Location: SE GA Flatwoods

Re: Glass Marbles for Reflux Column Structured Packing

Post by ga flatwoods »

Those are exactly what I was talking about! Forgot about the dempled side. Hope they work well. Before this thread I just bought a bag of lava rock for $4.50 at HD. Havent cracked them yet. May wait now on you guys results. My boka is only 2" but I bet they will work well. Let us know how the "etching " goes.
Ga Flatwoods
The hardest item to add to a bottle of shine is patience!
I am still kicking.
Ga Flatwoods
User avatar
MichiganCornhusker
retired
Posts: 4528
Joined: Mon Jun 23, 2014 9:24 am

Re: Glass Marbles for Reflux Column Structured Packing

Post by MichiganCornhusker »

A reflux column still is way beyond my skill level right now, but this is a great example of what is so great about this site: restless, relentless experimentation and shared results! Thanks for your curiosity and efforts.
Reminds me of Jimbo's tag: In theory there's no difference between theory and practice. But in practice there is.
Shouting and shooting, I can't let them catch me...
woodshed
Master of Distillation
Posts: 2970
Joined: Tue Aug 27, 2013 5:21 pm
Location: Pagosa Springs,CO

Re: Glass Marbles for Reflux Column Structured Packing

Post by woodshed »

Really curious about this and I never get excited about packing. Like the squished marbles. Keep us up on it WV.
User avatar
wv_cooker
Trainee
Posts: 933
Joined: Fri Feb 22, 2013 11:48 am

Re: Glass Marbles for Reflux Column Structured Packing

Post by wv_cooker »

woodshed wrote:Really curious about this and I never get excited about packing. Like the squished marbles. Keep us up on it WV.
Probably like most when I started 2 years ago I found the parent site and read it all LOL. Then moved on to studying everything I could find, and like most I am sure marbles were just old technology and the parent site numbers just weren't good for marbles. Now after a couple years and many types of packing and and plates all of a sudden Rad post's this LOL.

Ga mentioned the Accent Gems as they are called on the bag and the light bulb just went off LOL. Surface area, and these things have plenty of it. Then I got to thinking of the bags of marbles we bought as a kids and I remembered we use to boil them to crack them for gluing on different projects a give them different appearances. I thought geez how simple you don't need chemical etching just boiled water to crack the surface LOL.

The shape of these things have massive surface area and they will pack much tighter than round marbles how much simpler could it be. I just finished this 3" CM and was going to use Lava Rock as I really like it, but I thought why not. So here we are waiting for the holiday to be over and my 2 ferments to finish and I am really excited as I can be to try this LOL. Hopefully will have some results next week and will keep you posted. Who would have thunk it LOL.
Lester
Swill Maker
Posts: 250
Joined: Wed Sep 11, 2013 9:23 pm
Location: Cavite, Philippines

Re: Glass Marbles for Reflux Column Structured Packing

Post by Lester »

I bought 3 liters of marbles (about 3,000 pieces) for my 2" VM column. Size = 11.2mm. These came off used brandy bottles where they were used as pour regulators. Got them from a junk shop for about US$16 total.

Will tell you how it goes. :)
IMG_1189.JPG
Life is not about waiting for the storm to pass, it's about learning how to dance in the rain.
Reboiler: http://homedistiller.org/forum/viewtopi ... =1&t=43653
Thermometer: http://homedistiller.org/forum/viewtopi ... =2&t=43379
Jacksonbrown
Swill Maker
Posts: 315
Joined: Fri Sep 20, 2013 3:00 pm

Re: Glass Marbles for Reflux Column Structured Packing

Post by Jacksonbrown »

wv_cooker wrote:
woodshed wrote:Really curious about this and I never get excited about packing. Like the squished marbles. Keep us up on it WV.
The shape of these things have massive surface area and they will pack much tighter than round marbles how much simpler could it be.
A sphere is actually the smallest possible surface area for a given volume. A squashed sphere is only marginally better.
Marbles were never bad I don't think, it's just that there are much better alternatives.
googe
retired
Posts: 3877
Joined: Wed Jun 20, 2012 6:53 pm
Location: awwstralian in new zealund

Re: Glass Marbles for Reflux Column Structured Packing

Post by googe »

You gunna do a straight wash or low wines cookey?, I think low wines doesn't give a good enough result of if it's good or not. Do you do straight washes using lava?. I don't reckon marbles will be as good as lava with a straight wash, your thenman to try it though as you've used lava. Good luck, don't loose your marbles :lol:
Here's to alcohol, the cause of, and solution to, all life's problems.
"Homer J Simpson"
User avatar
wv_cooker
Trainee
Posts: 933
Joined: Fri Feb 22, 2013 11:48 am

Re: Glass Marbles for Reflux Column Structured Packing

Post by wv_cooker »

googe wrote:You gunna do a straight wash or low wines cookey?, I think low wines doesn't give a good enough result of if it's good or not. Do you do straight washes using lava?. I don't reckon marbles will be as good as lava with a straight wash, your thenman to try it though as you've used lava. Good luck, don't loose your marbles :lol:
I have never done strips googe, always done single runs as all my rigs have been reflux in one sort or another.
User avatar
FreeMountainHermit
Distiller
Posts: 1769
Joined: Thu May 12, 2011 6:45 pm
Location: Two Dogs Holler, West Virginia

Re: Glass Marbles for Reflux Column Structured Packing

Post by FreeMountainHermit »

A friend swears by his marbles, having used them for many years, but given the other packing choices out there I just assumed he was old school.

Guess I'm wrong in that assumption.

FMH.
Last edited by FreeMountainHermit on Fri Jul 04, 2014 5:30 am, edited 2 times in total.
Blah, blah, blah,........
User avatar
bearriver
Master of Distillation
Posts: 4442
Joined: Fri Nov 22, 2013 10:17 pm
Location: Western Washington

Re: Glass Marbles for Reflux Column Structured Packing

Post by bearriver »

I'll be testing my current ferment with 12 inch packing arrangements of marbles, scrubbers, and lava rock.

Might reach azeotrope with either of them if I fill the column all the way. So I am hoping that testing 12" would give more defined results.
rad14701
retired
Posts: 20865
Joined: Wed Dec 19, 2007 4:46 pm
Location: New York, USA

Re: Glass Marbles for Reflux Column Structured Packing

Post by rad14701 »

I just spent some time trying to determine whether the HETP calculator is accurate, considering how Tony Akland stated the numbers used were "approximate guesses", but need more time to concentrate on the theory behind HETP calculation... I'm not sure the numbers used are accurate and I also have a gut feeling that there is a mystery component that needs to be taken into account, at least with regard to marbles...

One aspect that contributes to the mystery is the percentage of voidage in relation to the diameter of the marbles in comparison to the diameter of the column... For example, the same 5/8" marbles in a 4" column should have less voidage than for a 1.25" column...

I've been debating ordering some 12mm(.47") marbles to see if they perform better than the 16mm(.625") marbles I am currently using...
User avatar
DAD300
Master of Distillation
Posts: 2842
Joined: Wed Mar 02, 2011 11:46 am
Location: Southern U.S.

Re: Glass Marbles for Reflux Column Structured Packing

Post by DAD300 »

I think this is a reverse TROLL.

So, this morning I bought 100 shares of Glass Globe & Marble works.
CCVM http://homedistiller.org/forum/viewtopi ... d#p7104768" onclick="window.open(this.href);return false;" rel="nofollow
Ethyl Carbamate Docs viewtopic.php?f=6&t=55219&p=7309262&hil ... e#p7309262
DSP-AR-20005
rad14701
retired
Posts: 20865
Joined: Wed Dec 19, 2007 4:46 pm
Location: New York, USA

Re: Glass Marbles for Reflux Column Structured Packing

Post by rad14701 »

I just did another run of 3 gallons of ~13% wine that was gifted to me because it wasn't worthy of drinking, and have 4 more gallons to run... Column temperature remained rock steady all the way through to the beginning of the tails, collecting at ~1oz per minute, yielding 1 liter of 95%+, 250ml of foreshots and heads, and 375ml of stinky tails...

The run took less than 2 hours from flame on to flame off, including two shutdowns to address very rare leaks due to small strands of SS scrubber hanging out of a slip joint that caused reflux to creep past the flour paste seal... This will be a non-issue in the future because I won't use scrubber at the bottom of the column as it creates a choke point at high heat input settings... Without the shutdowns I could have trimmed about a half hour off the total run time...

Will everyone who tries marbles have the same level of success as I have been having with my small scale LM rig...??? Only time will tell... Am I sold on the under-rated marble...??? You bet...!!! Now to tackle the other 4 gallons of nasty wine and 6 gallons of modified Birdwatchers...
Lester
Swill Maker
Posts: 250
Joined: Wed Sep 11, 2013 9:23 pm
Location: Cavite, Philippines

Re: Glass Marbles for Reflux Column Structured Packing

Post by Lester »

Besides the height of the column, perhaps we should also mention reflux ratios. A short column and a tall column can both attain azeo as long as the RR is sufficient, regardless of the packing. But the RR for a short column compared to a tall one will be significantly different.

Since I will be using the same height column which was previously packed with scrubbies, any improvement with marble packing should show up as reduced RR to maintain azeo. If marbles are worse then more reflux will be needed.
Life is not about waiting for the storm to pass, it's about learning how to dance in the rain.
Reboiler: http://homedistiller.org/forum/viewtopi ... =1&t=43653
Thermometer: http://homedistiller.org/forum/viewtopi ... =2&t=43379
rad14701
retired
Posts: 20865
Joined: Wed Dec 19, 2007 4:46 pm
Location: New York, USA

Re: Glass Marbles for Reflux Column Structured Packing

Post by rad14701 »

True, Lester...

Another consideration is the density of the structured packing... I just did some calculations to determine the amount of voidage within my packed column... For my small column and comparatively large marbles the voidage is in the mid-40% range... This ratio also has a direct influence on vapor speed increase which is the exact problem I was encountering with SS scrubbers... In my case this would correlate to a roughly just over double the vapor speed, without factoring in the liquid reflux which further fills the remaining voidage and subsequently further increases the vapor speed... The vapor speed is essentially more than doubled because there is roughly a 50%+ reduction in column volume... A larger column with smaller marbles would have less voidage and further increased vapor speed...

So, why do marbles work better than SS scrubber in my column...??? Several reasons... Increased voidage and increased reflux, combined with reduced vapor speed, mainly... How much the thermal mass contributes or detracts from functionality is currently an unknown...
Lester
Swill Maker
Posts: 250
Joined: Wed Sep 11, 2013 9:23 pm
Location: Cavite, Philippines

Re: Glass Marbles for Reflux Column Structured Packing

Post by Lester »

This is the cleaning run.

Loaded the boiler with 1.5 liters of Heads and Foreshots plus 3 liters of water, roughly 30% ABV.

Stabilized the column for 10 mins and proceeded to collect the alcohol. I seem to get good separation of the fractions. Boiler temp at this time is 86 deg C and is climbing as I proceed to take out product. RR = 3:1

When I got to 80-deg C head temperature (this is the temp on MY thermometer where I always take out hearts) I reduced reflux to 1:1 RR. The temp held steady at 80-deg C. With scrubbies I needed a RR of 2:1 so this is a big improvement already.

When boiler temp reached 91-deg C (~13.5% ABV) I timed my take off rate. RR is still at 1:1 and I got 300ml in 5mins & 8secs (about 3.5LPH of 95.6% ABV). The boiler temp was at 94-deg C (~8% ABV) when this was completed. I proceeded to take out the remaining alcohol then shut it down when the boiler reached 97-deg C.

First impressions:
I was very pleased to be able to take product out at 1:1 RR and the head temperature would still hold steady. This is a big improvement from the 2:1 RR I needed with the scrubbies.

From boiling to flame off it took me 35 minutes to go through 4.5 liters of ~30% ABV low wines. I think this is fast.

Output rate at middle of the run = 3.5 LPH of 95.6% ABV

Column Type: VM
Column Diameter: 2"
Column packed height = 45"
Packing: Round glass marbles 11.2mm in diameter

Will continue with more trials over the next few days using actual low wines that I will be able to taste.

So far I am very pleased with the results. Less RR and the column temperature is very steady. The marbles seem to perform better than scrubbies. :)
Last edited by Lester on Thu Jul 03, 2014 5:58 pm, edited 1 time in total.
Life is not about waiting for the storm to pass, it's about learning how to dance in the rain.
Reboiler: http://homedistiller.org/forum/viewtopi ... =1&t=43653
Thermometer: http://homedistiller.org/forum/viewtopi ... =2&t=43379
Lester
Swill Maker
Posts: 250
Joined: Wed Sep 11, 2013 9:23 pm
Location: Cavite, Philippines

Re: Glass Marbles for Reflux Column Structured Packing

Post by Lester »

If I may add........

Gas flow over the marbles is less turbulent and therefore more predictable. The boundary layers on the marbles are evenly exposed to the gasses and I think that is a good thing.

Not so sure about flattened spheres though I think they will be inferior to a perfectly-round shape. On flattened spheres, the surface is not evenly-exposed to the flowing gases. And it will hold more liquid (not necessarily a good thing) at the point where the marbles touch one another due to capillary action.
Life is not about waiting for the storm to pass, it's about learning how to dance in the rain.
Reboiler: http://homedistiller.org/forum/viewtopi ... =1&t=43653
Thermometer: http://homedistiller.org/forum/viewtopi ... =2&t=43379
User avatar
Brutal
Distiller
Posts: 1352
Joined: Sat May 18, 2013 6:02 pm

Re: Glass Marbles for Reflux Column Structured Packing

Post by Brutal »

@Rad. The stainless scrubbie at the bottom of your column must be pretty tight. Do you think liquid could be flooded on top of it during a run? That would cause all the vapor to bubble through it before proceeding up the marble section of the column. Sort of a faux bubble plate?
Steam injection rig http://tinyurl.com/kxmz8hy
All grain corn mash with steam injection and enzymes http://tinyurl.com/mp6zdt5
Inner tube condenser http://tinyurl.com/zkp3ps6
User avatar
wv_cooker
Trainee
Posts: 933
Joined: Fri Feb 22, 2013 11:48 am

Re: Glass Marbles for Reflux Column Structured Packing

Post by wv_cooker »

Lester wrote:If I may add........

Gas flow over the marbles is less turbulent and therefore more predictable. The boundary layers on the marbles are evenly exposed to the gasses and I think that is a good thing.

Not so sure about flattened spheres though I think they will be inferior to a perfectly-round shape. On flattened spheres, the surface is not evenly-exposed to the flowing gases. And it will hold more liquid (not necessarily a good thing) at the point where the marbles touch one another due to capillary action.
Not so sure this is going to be true. The spheres are half round on one side and concave or Dimpled on the other they seem to pack maybe a little tighter than the round ones and they don't necessarily lay flat as you would think. They also have a lot of surface area for liquid and vapor to react with each other. I have some glass I will pack a piece and try to get a pic and show what I mean. My initial thought was channeling would be a big issue, but what I am seeing in playing with them it won't be a problem at all I don't think.

It makes sense once you think of the areas between the marbles and how tightly you have to pack copper or stainless scrubbies to make them work properly. Lava rock works in a similar way as you have to get the size right for your column and get it packed tightly. Really if you think of it spp also has to be the same way. In our quest to find the greatest packing material we may have just bypassed a good cheap method LOL.

Can't run them till next week when the ferments finish but I can see possibilities. If the decorative ones don't work I'll get a bag of round ones and try them too LOL. I think the decorative ones will do just fine.
Jacksonbrown
Swill Maker
Posts: 315
Joined: Fri Sep 20, 2013 3:00 pm

Re: Glass Marbles for Reflux Column Structured Packing

Post by Jacksonbrown »

How many grams per meter of copper or SS are your guys cramming into your columns?
Has anyone even checked?
Boda Getta
Distiller
Posts: 1279
Joined: Wed Apr 20, 2011 12:39 pm

Re: Glass Marbles for Reflux Column Structured Packing

Post by Boda Getta »

Rad:
I sure hope you don't have a cat.

Image
User avatar
Red Rim
Trainee
Posts: 806
Joined: Sun Apr 06, 2014 3:14 am
Location: Orygun

Re: Glass Marbles for Reflux Column Structured Packing

Post by Red Rim »

One of my favorite parts of this pic is, that Dr. Rad, uses whatever is on hand to make his still work. Carbage cans, twine, whatever it takes to make it happen. Not what I would expect, however, a better glimpse into a creative mind at work. Looks like something I would do!
There is no such thing as a stupid question....... Unless you didn't research it first.
Lester
Swill Maker
Posts: 250
Joined: Wed Sep 11, 2013 9:23 pm
Location: Cavite, Philippines

Re: Glass Marbles for Reflux Column Structured Packing

Post by Lester »

wv_cooker wrote:
Lester wrote:If I may add........

Gas flow over the marbles is less turbulent and therefore more predictable. The boundary layers on the marbles are evenly exposed to the gasses and I think that is a good thing.

Not so sure about flattened spheres though I think they will be inferior to a perfectly-round shape. On flattened spheres, the surface is not evenly-exposed to the flowing gases. And it will hold more liquid (not necessarily a good thing) at the point where the marbles touch one another due to capillary action.
Not so sure this is going to be true. The spheres are half round on one side and concave or Dimpled on the other they seem to pack maybe a little tighter than the round ones and they don't necessarily lay flat as you would think. They also have a lot of surface area for liquid and vapor to react with each other. I have some glass I will pack a piece and try to get a pic and show what I mean. My initial thought was channeling would be a big issue, but what I am seeing in playing with them it won't be a problem at all I don't think.

It makes sense once you think of the areas between the marbles and how tightly you have to pack copper or stainless scrubbies to make them work properly. Lava rock works in a similar way as you have to get the size right for your column and get it packed tightly. Really if you think of it spp also has to be the same way. In our quest to find the greatest packing material we may have just bypassed a good cheap method LOL.

Can't run them till next week when the ferments finish but I can see possibilities. If the decorative ones don't work I'll get a bag of round ones and try them too LOL. I think the decorative ones will do just fine.
I don't think you will be able to place each squashed marble in a favorable orientation to take advantage of its shape, unless you laboriously drop the marble inside the column one piece at a time. If it moves out of line then you lose the benefit.

Anyway, good luck with your trials and I hope you come come up with something conclusive. Hard data is always good to have. :thumbup:
Life is not about waiting for the storm to pass, it's about learning how to dance in the rain.
Reboiler: http://homedistiller.org/forum/viewtopi ... =1&t=43653
Thermometer: http://homedistiller.org/forum/viewtopi ... =2&t=43379
Post Reply