ceramic rings meant for using in an aquarium

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Re: ceramic rings meant for using in an aquarium

Post by zapata » Sun Sep 27, 2020 2:50 am

Interesting results NIN. Hey, if you get a chance, can you measure the holdup of the packing? You mentioned it seems like a lot, but quantification would be interesting to me because I'm a nerd and don't really know exactly how or when it might matter much, but think it may be relevant. It's not a particularly convenient measurement to ask someone else to make for no explicitly good reason, so just if you have the chance. When I've wanted an easy way to measure holdup, I just weigh a column section packed and DRY. Then pour water through it and reweigh after anything that can drip freely has done so. I use weight of liquid / volume of packing to compare.

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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Sun Sep 27, 2020 8:10 am

zapata wrote:
Sun Sep 27, 2020 2:50 am
Interesting results NIN. Hey, if you get a chance, can you measure the holdup of the packing? You mentioned it seems like a lot, but quantification would be interesting to me because I'm a nerd and don't really know exactly how or when it might matter much, but think it may be relevant. It's not a particularly convenient measurement to ask someone else to make for no explicitly good reason, so just if you have the chance. When I've wanted an easy way to measure holdup, I just weigh a column section packed and DRY. Then pour water through it and reweigh after anything that can drip freely has done so. I use weight of liquid / volume of packing to compare.
Yeah I can do that. That's easy enough to do.

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Re: ceramic rings meant for using in an aquarium

Post by Windy City » Mon Sep 28, 2020 9:37 am

This has been a great read. Thanks to all that have contributed to it.
I am curious how this compares to spp especially in large format (4").
Reading the link below they talk about sizing spp to column diameter as 1/10th of column diameter for packing/spp diameter and 15% of column diameter for packing/spp length.
https://homedistiller.org/forum/viewtop ... =2&t=71777
So that being said a 4" column would use 10mm diameter x 15mm length spp.
Do you think that this product should be sized the same.
I have understood that people running large format (4") spp are throwing a ton of power i.e.: 12KW (approx) into the boiler and are getting azeo (or very close to) take-off rates in the 3 to 4 gal per hour rates.
Any thoughts on how this would compare?
This product ZED255 posted seemed interesting for a 4" even though it is slightly larger in diameter.

I am wanting to build a 4" x 60" column. I have priced out large format spp and it is quite expensive. I would be willing to make the one time investment, but it would be phenomenal to find something that is close and a ton cheaper.
Thanks
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Re: ceramic rings meant for using in an aquarium

Post by zed255 » Mon Sep 28, 2020 10:05 am

I have the Siporax product but have been pot stilling lately. I am going to do a sugar neutral again soon and reflux a carboy on mixed feints. Will report when I've tried it.
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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Mon Sep 28, 2020 12:02 pm

Windy City wrote:
Mon Sep 28, 2020 9:37 am
This has been a great read. Thanks to all that have contributed to it.
I am curious how this compares to spp especially in large format (4").
Reading the link below they talk about sizing spp to column diameter as 1/10th of column diameter for packing/spp diameter and 15% of column diameter for packing/spp length.
https://homedistiller.org/forum/viewtop ... =2&t=71777
So that being said a 4" column would use 10mm diameter x 15mm length spp.
Do you think that this product should be sized the same.
I have understood that people running large format (4") spp are throwing a ton of power i.e.: 12KW (approx) into the boiler and are getting azeo (or very close to) take-off rates in the 3 to 4 gal per hour rates.
Any thoughts on how this would compare?
This product ZED255 posted seemed interesting for a 4" even though it is slightly larger in diameter.

I am wanting to build a 4" x 60" column. I have priced out large format spp and it is quite expensive. I would be willing to make the one time investment, but it would be phenomenal to find something that is close and a ton cheaper.
Thanks
This stuff isn't really expensive at all. I'd recommend anyone who's interested to give it a try. It's possible smaller rings could work better for my 3", but no telling if it would flood the column without trying it first. Larger perhaps for your bigger still. I listed a couple links in this thread for some larger rings. If I can find some smaller Ceramic Rings I might be willing to give them a shot.

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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Tue Sep 29, 2020 12:00 pm

zapata wrote:
Sun Sep 27, 2020 2:50 am
Interesting results NIN. Hey, if you get a chance, can you measure the holdup of the packing? You mentioned it seems like a lot, but quantification would be interesting to me because I'm a nerd and don't really know exactly how or when it might matter much, but think it may be relevant. It's not a particularly convenient measurement to ask someone else to make for no explicitly good reason, so just if you have the chance. When I've wanted an easy way to measure holdup, I just weigh a column section packed and DRY. Then pour water through it and reweigh after anything that can drip freely has done so. I use weight of liquid / volume of packing to compare.
1 gal wet weighs 7 lbs 11.3 oz
1 gal dry weighs 6 lbs 12 oz

Approx 0.9375 lb difference.

I spread it out to dry for a couple days, but then baked it at 350F for approx 1 hr or less. I don't think it was 100% dry because it was still steaming a bit when I removed it. I'll leave it to dry for a few more days and see what it weighs again.

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Re: ceramic rings meant for using in an aquarium

Post by zapata » Tue Sep 29, 2020 12:52 pm

Interesting, thanks. That's already over 11% by volume. If it dries a bit more, it'd be about a cup of liquid in a typical 2"x3' column.

I'm really not sure exactly where I'm gong with this tbh though. But I've just had a nagging suspicion there is something to it. Maybe, it's just that let's compare it to an otherwise identical imaginary 2'x3' packed column with zero holdup. Assuming perfect transfer of energy from liquid to vapor, the column with a cup of extra liquid in it has about... 100 watt hours extra "buffer" or "rectification" or, not sure the right term. But roughly, that's the energy to vaporize that extra cup of liquid if it's an average of 50% alcohol/water (about 366 kJ). 100 watt hours doesn't sound like a lot, but the "hour" is arbitrary just to put it in common terms. People say SPP works better flooded, which is one of the things that has made me wonder why, exactly, and if it's a more general aspect of packing that we can pay attention to.

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Re: ceramic rings meant for using in an aquarium

Post by Windy City » Tue Sep 29, 2020 1:06 pm

zapata wrote:
Tue Sep 29, 2020 12:52 pm
people say SPP works better flooded, which is one of the things that has made me wonder why, exactly, and if it's a more general aspect of packing that we can pay attention to.
This is partially what I am curious about.
What would happen if you ran this like spp being flooded with big power and reflux.
I am curious if it would run similar to the spp
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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Tue Sep 29, 2020 1:33 pm

Windy City wrote:
Tue Sep 29, 2020 1:06 pm
zapata wrote:
Tue Sep 29, 2020 12:52 pm
people say SPP works better flooded, which is one of the things that has made me wonder why, exactly, and if it's a more general aspect of packing that we can pay attention to.
This is partially what I am curious about.
What would happen if you ran this like spp being flooded with big power and reflux.
I am curious if it would run similar to the spp
Next time I run it, I'll try to flood the column, but it would take a lot of power I suspect. I forget what power I was running, but I was at the upper end of the maximum power recommended based on what the vapor speed calculator says and it didn't want to flood.

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Re: ceramic rings meant for using in an aquarium

Post by WithOrWithoutU2 » Tue Sep 29, 2020 3:44 pm

Windy City wrote:
Tue Sep 29, 2020 1:06 pm
zapata wrote:
Tue Sep 29, 2020 12:52 pm
people say SPP works better flooded, which is one of the things that has made me wonder why, exactly, and if it's a more general aspect of packing that we can pay attention to.
This is partially what I am curious about.
What would happen if you ran this like spp being flooded with big power and reflux.
I am curious if it would run similar to the spp
I am no expert and still learning about SPP, but my understanding is you want a Semi-Flooded state, or also called Semi Aquatic. I do not believe you want an actual flooded column. Again, I am not an expert and still learning about SPP. The difference is semi-flooded is pockets of puddles or pools up and down the column (although the bottom portion can get 100% flooded). The SPP allows for this and it is desirable because these little puddles act as little bubble plates. This is what gives SPP it ability to have such a low HETP. I do not believe you want to actually flood the column. This is why it is important to have SPP that has 10% width and 15% length of the column circumference. This size ratio is needed to protect against flooding. Otherwise you have to run at lower power which would negate one of the advantages of pushing the take of rate with higher power/reflux.

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Re: ceramic rings meant for using in an aquarium

Post by zapata » Wed Sep 30, 2020 10:49 am

WithOrWithoutU2 wrote:
Tue Sep 29, 2020 3:44 pm
This is why it is important to have SPP that has 10% width and 15% length of the column circumference. This size ratio is needed to protect against flooding. Otherwise you have to run at lower power which would negate one of the advantages of pushing the take of rate with higher power/reflux.
I know we are getting off topic here, but it may come back around? Anyway, does anybody have a reference to the size spec? Not that it exists, I've seen it in many places since the rediscovery of SPP, but why it is what it is? If I ever saw it I've forgotten it, but my initial guess would be that it is an arcane simplification of packing geometry, as in "how many of these thingies will fit in the this box here?", which is astoundingly complicated math. Which of course would affect flooding by affecting fill density, % void etc. But when it's phased simply as "this size is needed to protect against flooding" it occurs to me that perhaps there are specific foundations for that size based more specifically on hydraulics or something.

Or maybe / probably it was just derived experimentally and those ratios had the best performance, with no underlying mechanism understood or theorized.

1 could give insight to optimum sizing of ceramic packing, the other would simply provide a method for determining optimum sizing (test a bunch of different ones). I knew I could get back on topic somehow. So yeah, anybody know how the 10%C x 15%C was determined or if it relates to other packings or problems?

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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Wed Sep 30, 2020 11:00 am

zapata wrote:
Wed Sep 30, 2020 10:49 am
WithOrWithoutU2 wrote:
Tue Sep 29, 2020 3:44 pm
This is why it is important to have SPP that has 10% width and 15% length of the column circumference. This size ratio is needed to protect against flooding. Otherwise you have to run at lower power which would negate one of the advantages of pushing the take of rate with higher power/reflux.
I know we are getting off topic here, but it may come back around? Anyway, does anybody have a reference to the size spec? Not that it exists, I've seen it in many places since the rediscovery of SPP, but why it is what it is? If I ever saw it I've forgotten it, but my initial guess would be that it is an arcane simplification of packing geometry, as in "how many of these thingies will fit in the this box here?", which is astoundingly complicated math. Which of course would affect flooding by affecting fill density, % void etc. But when it's phased simply as "this size is needed to protect against flooding" it occurs to me that perhaps there are specific foundations for that size based more specifically on hydraulics or something.

Or maybe / probably it was just derived experimentally and those ratios had the best performance, with no underlying mechanism understood or theorized.

1 could give insight to optimum sizing of ceramic packing, the other would simply provide a method for determining optimum sizing (test a bunch of different ones). I knew I could get back on topic somehow. So yeah, anybody know how the 10%C x 15%C was determined or if it relates to other packings or problems?
There are books on the topic. Krell Erich Handbook of Laboratory Distillation, With an Introduction to Pilot Plant Distillation (Techniques and instrumentation in analytical chemistry) is one that shows much of the testing & math involved. I've never read it, but it's been cited here quite a few times. There are test results comparing different packings, their differences and performance differences.

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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Thu Oct 08, 2020 5:42 am

I just weighed the Ceramic Rings again after giving it a lot more time to dry.

1 gal = 7.70625 lbs wet
1 gal = 6.4125 lbs dry

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Re: ceramic rings meant for using in an aquarium

Post by Windy City » Tue Oct 13, 2020 8:53 am

I just started putting this together this weekend and am pretty excited about running it.
It will have a valved Carter head to the left and then a shotgun pc on a stand hopefully I can do all my piping and build a two element controller in the next couple of weeks.


E99AEE39-73B8-451C-83E6-AD4C5967CF6D.jpeg
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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Tue Oct 13, 2020 9:23 am

Windy City wrote:
Tue Oct 13, 2020 8:53 am
I just started putting this together this weekend and am pretty excited about running it.
It will have a valved Carter head to the left and then a shotgun pc on a stand hopefully I can do all my piping and build a two element controller in the next couple of weeks.



E99AEE39-73B8-451C-83E6-AD4C5967CF6D.jpegCCF3466E-104A-4E7D-A438-647D6B97FDF4.jpeg
Siporax, that's some expensive stuff if I recall correctly. It should do very well. That stuff appears to be MUCH more porous than these generic ceramic rings here. Their dimensions seem appropriate too for your column's diameter. I look forward to see your results :thumbup:

Quick tip. If/when you rinse the packing, I'd use clean or purified water.

After a run, I removed my reflux condenser and ran well water down through the column. Later I noticed that the top portion of the ceramic packing was stained with rust. I didn't know if this will be a problem, but I didn't like it. I tried vinegar and it didn't work well. I tried Citric Acid and that didn't work well. I tried diluted Muriatic acid (1-part water and 5-parts water), that worked very quickly and didn't harm the ceramic. I had to rinse, soak, rinse soak, but ended up using baking soda & water to neutralize any potential residual acid. More rinsing. What a pain.

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Re: ceramic rings meant for using in an aquarium

Post by zapata » Wed Oct 14, 2020 1:19 am

NIN, Thanks for those numbers. I was reading about holdup today, funnily enough in the book you referred me to regarding size. (Yes, the size question was addressed throughout. It is largely about fluid flow and preventing wall channeling, so good ref for a book you haven't read, cheers) I already had it in my collection but hadn't read or digested this section. Here's a snip and the chapter reference, it goes on from here but makes a case for when why and how holdup is an integral quality of packings and quantifies it as "intensity" to relate to the time required.

I haven't quite parsed it enough to say anything useful like "oh yeah, run it heavily loaded and almost flooded like SPP" or anything, but, well, read the section, and the other sections it refers to if you want, it might give you some insight? My "read it while thinking of someone else's still and sipping whiskey" take is encouraging that this ceramic packing will perform well driven hard at low to moderate reflux rates. At higher reflux rates the static holdup may "get in the way" compared to something more freely draining.
From Erich Krell - Handbook of laboratory distillation
Intensity time and holdup.png
http://libgen.rs/book/index.php?md5=0B4 ... 269B6FBBC7

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Re: ceramic rings meant for using in an aquarium

Post by ideasinbeer » Wed Oct 14, 2020 7:44 am

If you can summarize with Coles notes for an idiot like me it would be appreciated.

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Re: ceramic rings meant for using in an aquarium

Post by shadylane » Wed Oct 14, 2020 11:39 am

NineInchNails wrote:
Tue Oct 13, 2020 9:23 am
Quick tip. If/when you rinse the packing, I'd use clean or purified water.
When I cleaned the new ceramic rings.
I did a 100% reflux sacrificial run.
Afterwards, I removed and inspected the packing.
Every thing was spotless

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Re: ceramic rings meant for using in an aquarium

Post by NineInchNails » Wed Oct 14, 2020 2:19 pm

shadylane wrote:
Wed Oct 14, 2020 11:39 am
NineInchNails wrote:
Tue Oct 13, 2020 9:23 am
Quick tip. If/when you rinse the packing, I'd use clean or purified water.
When I cleaned the new ceramic rings.
I did a 100% reflux sacrificial run.
Afterwards, I removed and inspected the packing.
Every thing was spotless
I meant the water you rinse the packing with after a run. I used well water and it imparted rust stains.

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Re: ceramic rings meant for using in an aquarium

Post by shadylane » Wed Oct 14, 2020 5:22 pm

I also back flush the column after use.
Open the boiler drain, then hook the garden hose to the end of the product condenser

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Re: ceramic rings meant for using in an aquarium

Post by zapata » Thu Oct 15, 2020 4:10 am

ideasinbeer wrote:
Wed Oct 14, 2020 7:44 am
If you can summarize with Coles notes for an idiot like me it would be appreciated.
Is Cole the Canadian Cliff?
Unfortunately the quote I put up was more of a "here's a chapter where this guy talks about holdup which I was vaguely speculating about earlier". I haven't digested it anywhere near enough to give a decent summary. I thought I had earlier today, then in the next chapter he just threw out a "holdup is bad for reasons" kinda quip that made me suspect I don't really have a working grasp.

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Re: ceramic rings meant for using in an aquarium

Post by ideasinbeer » Thu Oct 15, 2020 10:07 am

Zapata,

You are correct. Coles was another source of cheating for us Canucks back in the day.

I looked at your paper, my eyes glazed over and I'm hoping someone can break it down for me.

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Re: ceramic rings meant for using in an aquarium

Post by shadylane » Thu Oct 15, 2020 2:12 pm

Don't look at me if you want some one to break it down for you.
After reading some of it, I'll have to rinse my brain with ethanol.

Seems like almost all the info is on distilling chemicals other than water/ethanol mixtures.

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Re: ceramic rings meant for using in an aquarium

Post by zapata » Thu Oct 15, 2020 3:03 pm

There is a good reason for it, one that we have hit on in the hobby many times. Ethanol / water sucks for testing and quantifying columns and packing due to the non-ideality, different latent heats, the heat of mixing and the azeotrope. Trying to quantify theroretical plates (say for comparing different packings) for us is hard for us because even an empty column can damn near get us over the VLE hump, and almost any packing gets us to a point where .1 degree or ml volume measurements skew things a lot.

But there's practical stuff in there too. Like two different CCVM heads, back in the 80's with most sources from the 50's. And SPP too. But yeah, figuring out what applies to our system is not obvious.

EDIT to add:
Here's an understandable quote regarding holdup from p. 157
A knowledge of the total hold-up is of importance, since - as we have already seen in section 4.7.1 - its influence increases with the number of separating stages and is unfavourable for separation at a high reflux ratio, but favourable at a low reflux ratio, whilst with a very high hold-up the reflux ratio loses almost all its influence on the separation.

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Re: ceramic rings meant for using in an aquarium

Post by shadylane » Thu Oct 15, 2020 5:03 pm

Long story short
The more reflux pouring down the column
The more the liquid "hold up" gets in the way of the rising vapors.
When its bad enough, the column will flood
This becomes more of a problem, the taller the column and the higher the reflux ratio

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Re: ceramic rings meant for using in an aquarium

Post by Sk8brew » Sun Oct 18, 2020 7:02 am

How are you cleaning this packing prior to filling the column? Hot water rinse, boiling, vinigar? I have a new colunm and will be doing a sacrificial run, but just want to see if I should do anything prior to filling the column.

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Re: ceramic rings meant for using in an aquarium

Post by shadylane » Sun Oct 18, 2020 9:53 am

Instead of cleaning the rings before packing the column
Fill the boiler with water and run the packed column at 100% reflux.
Then give the boiler a good rinse after draining it.

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Re: ceramic rings meant for using in an aquarium

Post by bunny » Fri Oct 23, 2020 8:33 pm

I'm using the Sera Siporax Mini Pro 9.5oz pkg in my 1 inch LM column. This gives me exactly 1 meter(40 inches) of packing.
394620BE-15E3-442D-B974-9CC0CB176979.jpeg
They are a lot smaller than the regular Siporax. These six are dirty from hiding on my garage floor, but I caught them before they got away. I plan to compare them with the lava shown below.
366914D5-3B85-4372-AD41-0A186960AFA4.jpeg
5617B91B-47CC-4EC2-9AB8-C00DA586061E.jpeg
9736CF4F-888E-422B-93E9-B511925FB2C2.jpeg

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Re: ceramic rings meant for using in an aquarium

Post by shadylane » Fri Oct 23, 2020 9:15 pm

Ya got my attention
I'd like to see some packing tests on a 1 inch column
I don't think it's ever been done here before.

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Re: ceramic rings meant for using in an aquarium

Post by bunny » Sat Oct 24, 2020 6:52 am

I'm not really sure how to compare these. I have 9 thermometers in my "pilot plant" and am collecting some very interesting data points that I may require help interpreting. Here's a few pics of my column on top of my corny boiler. I'll get fresh pics with less background clutter.
DF02FC31-2988-4BAB-8D99-DB6348078A1B.jpeg
P1050042.jpeg
I'm using a fixed jet with a birch needle valve.
P1050039.jpeg
P1050036.jpeg
P1050037.jpeg
P1050044.jpeg

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