SPP Packing

carbohydratesn · Post by **carbohydratesn** » Sat Mar 28, 2015 9:23 am

I'm a bit confused by that wording too. At first, I thought you were talking about flooding in the column, and wrote this - but now I see that you're talking about something else entirely.

I've found that to be a matter of heat input - dial it in so the flooding stops somewhere mid-column instead of at the top. I've found a spot on my controller where the flooding stays roughly in the same place. A tiny bit higher on the dial, and the flooding rises very slowly. A tiny bit lower, and the flooding lowers slowly. So I put my ear close to the column and listen up and down it to locate what parts of the column are flooding - you can hear the 'surging', bubbles rushing up through the liquid and packing - and adjust the heat based on that every few minutes.

If there's a better way to manage this, I'd love to hear about it, as I still get flooding sometimes, and the opposite too - I lose the fluid in the column. In either case I just close the takeoff valve, turn the heat all the way up or down momentarily to bring it back to a semi-flooded state, and re-equilibriate for a minute or two. I switch to a new jar, too. I've only done half a dozen runs with SPP, so this will probably get easier with time.

I've been thinking about attaching a few microphone elements up and down the column, and doing some processing on the signals to be able to detect how much of the column is flooding. That sound is very consistent in my experience so far, so it shouldn't be too tough to get a yes/no on whether or not there's flooding at that point in the column. Indicator lights up and down the column would be very helpful!

sergiolis · Post by **sergiolis** » Sat Mar 28, 2015 9:43 am

Sorry about the confusion. The problem is my english is not so good.
When I get a spurt at the begining it's not a big deal because i can regulate it closing the valve and reopen it. And as you say I'm in the foreshots so no problem. But sometimes when I'm collecting the hearts I open slowly the valve to get more flow rate but suddenly when it's open about 20ml/min the valve drips a big spurt as it was completely open (And even if I close the valve the spurt is dripping for a minute or so). Then is chaotic because i lose the equilibrium and I get some tails mixed with the hearts. Basically that's my problem and I don't know how to solve it.
Coluld it be pressure liquid over the needdle-valve? any ideas? thanks a lot and please forgive my ignorance about this issue...

carbohydratesn · Post by **carbohydratesn** » Sat Mar 28, 2015 10:52 am

Ah, no worries

You've described it well after the first post. I'm not familiar with your needle valve, but it sounds like a problem with the valve itself. A good needle valve shouldn't be able to do that - even under pressure, it should be a smooth increase in flow, no spurting.

(I could be mistaken, though - I've only operated my homemade valve of this design)

sergiolis · Post by **sergiolis** » Sat Mar 28, 2015 11:13 am

My needle-valve is that one, but here in Spain I paid much more: http://www.ebay.ca/itm/Parker-V4LR-SS-3 ... 487be2665d" onclick="window.open(this.href);return false;" rel="nofollow
I tested the needle-valve under my water tap and it was working good and I could regulate the flow-rate with accuracy. So I'm trying to trust in my needle-valve. I think it is a good one....
Sometimes I got more than 30ml/min without issues but sometimes it spurts after approximately 20 ml/min.So it's quite difficult to me to find where is the problem... thanks a lot

Post by **rad14701** » Sat Mar 28, 2015 2:33 pm

I can't comment on that particular needle valve but with mine I open it 1/2 turn at a time and my collection is done at 1.5 - 2 turns open... For me, running slow would be 1.25 turns open...

Also, make sure your valve is installed in the right direction... They usually have an inlet and an outlet... Reversing flow direction can give some quirky results...

sergiolis · Post by **sergiolis** » Sat Mar 28, 2015 8:35 pm

Thanks Rad, it's installed correctly. In the other hand, I'm trying to run at abot 30 ml/min and from the closed position of the valve to the aproximately 30ml/min position there is only a turn of 90º, so i have to turn it very carefully. I will test it again with water tap and on my next run i will try some changes (no insulation, more distance between the bottom plate and the packing, etc) and let's see what happens, if the problem persist, i will have to buy a new one... Thanks a lot

sergiolis · Post by **sergiolis** » Tue Mar 31, 2015 9:56 am

Got it!! I removed the insulation and I charged a bit less the boiler... In a 2" column after heads I got an average of 35ml/min, and I achieved 38ml/min... working at 2170W No problems with the needle-valve. Great !!
Thanks a lot

carbohydratesn · Post by **carbohydratesn** » Tue Mar 31, 2015 9:58 am

Awesome

I'm glad you figured it out. I took the insulation off of my column too, it just seems to run better that way.

Norbrewer · Post by **Norbrewer** » Sun Apr 26, 2015 2:22 pm

Is there anyone in here who has suxess running spp from Manu ? Its real tiny , mine is bearly 2,2 mm. I have spent the weekend trying to run my boka with this stuff but my column just keeps flooding. I got some good results when taking of real slow , one drop pr minute at 800w. If i increase the power it floods real bad and i have to shut down to let it drain. I write this here because i am intriqued by this aquatic deal. I had boiling in the top of the column sometimes but it did not seem to be helping my abv or takeout speed. I sent a mail to the polish guy to get some 4mm spp instead.

carbohydratesn · Post by **carbohydratesn** » Sun Apr 26, 2015 3:27 pm

What size column? What are you using to hold the packing in your column? How much open space is there between your packing and your takeoff?

Post by **skow69** » Sun Apr 26, 2015 4:23 pm

What are the symptoms when it floods?

Norbrewer · Post by **Norbrewer** » Sun Apr 26, 2015 10:10 pm

My column is 51mm Id ss . Bottom section is 75cm with a sieve in the bottom to hold the small ssp. The sieve openings is 0,8 x 0,8 mm and ca 0,5mm wire. The fisrst run i had the ssp directly against the sieve and thought the ssp could block it. I allso had ssp in the second section (30 cm)
For the second run i had some 5mm rachig at the bottom and a small piece of mesh over that. The next section is 30 cm and i used a roll of mesh in the bottom of that one to hold 20cm ssp on top. I have a centering ring on top of the bottom section with 30mm opening. About 2cm free spase on both sides of the ring.

The first time i noticed the flooding when temperature at the takeout startet to drop fast. I didnt realise why so i increased power. After a while destilate came out ower the top of the column

I shut down of corse. I drained the fluid ower the outtake and that was 85 abv. The rest of the column drained to the boiler after it cooled down a bit. I released the triclamp on the boiler to check and it was pretty high pressure there.

The second run went better , but the collumn filled wit reflux several times and i had to shut down to let the column drain.
A simple drawing to illustrate :

: Stilltaketwo.jpg (12.53 KiB) Viewed 3661 times

Post by **skow69** » Mon Apr 27, 2015 11:36 pm

Norbrewer wrote: I have spent the weekend trying to run my boka with this stuff but my column just keeps flooding. I got some good results when taking of real slow , one drop pr minute at 800w. If i increase the power it floods real bad and i have to shut down to let it drain.

One drop per minute? That's pretty slow, all right. Increased power promotes flooding, but increasing takeoff rate should avoid flooding. So what happens if you run at 800 watts and collect at one drop per second?

Hound Dog · Post by **Hound Dog** » Tue Apr 28, 2015 1:53 am

skow69 wrote:
Norbrewer wrote: I have spent the weekend trying to run my boka with this stuff but my column just keeps flooding. I got some good results when taking of real slow , one drop pr minute at 800w. If i increase the power it floods real bad and i have to shut down to let it drain.
One drop per minute? That's pretty slow, all right. Increased power promotes flooding, but increasing takeoff rate should avoid flooding. So what happens if you run at 800 watts and collect at one drop per second?

+1, what if you speed your takeoff up to a broken stream coming out? Could you increase the power and not flood?

I would suggest getting rid of the centering ring you mentioned. If the column is flooded, what exactly are you centering? It is just speeding vapor and preventing return. I would also suggest trying a different retainer than a sieve plate. You may be holding too much liquid back here. While beneficial for more open SPP, it may not work as well for your smaller tighter SPP.

carbohydratesn · Post by **carbohydratesn** » Tue Apr 28, 2015 10:51 am

+1 to all of those suggestions.

I built my bok with two centering rings, originally, because some resources here said it was a good idea. They were wrong.

DAD300 · Post by **DAD300** » Tue Apr 28, 2015 10:59 am

I went round and round on centering rings and decided, I didn't care how the reflux got down the packing, in fact down the side might get it lower, faster.

Post by **Kegg_jam** » Tue Apr 28, 2015 11:26 am

You can watch the reflux run down a borosilicate column for about an inch or two before it wicks back into the packing

Norbrewer · Post by **Norbrewer** » Tue Apr 28, 2015 8:42 pm

Thanks for the replies !

My plan to test before the next run :

Loose the collar , less packed column 75 cm should be enough , a little more free space under the takeout , and try to increase takeoff speed .

Anything else i could try ? Hope to get hold of a sightglass by then to

sergiolis · Post by **sergiolis** » Sun May 03, 2015 6:36 am

Hi Guys!!! Just out of curiosity...
I have a 2" Bokakob with 40" filled with SPP and 4 copper scrubbies at the bottom.... I'm collecting Foreshots at 7ml/min, Heads at 15ml/min and hearts at 32ml/min...
What is your collection rate in foreshots, heads and hearts?
thanks in advance

DAD300 · Post by **DAD300** » Mon May 04, 2015 12:20 pm

32ml a minute is almost 2 liters an hour...so I'm right there.

But why collect the heads slower? just use smaller collection jars until you know you are in hearts.

On a 2" I'd collect fores and heads in 250ml containers and hearts in 500ml and switch back to 250ml for tails.

Fores and early heads are the same...shitz...tails can be dif. I get tails that are terrible, next some cloudy oily and them some better tails follow. I throw away the oily stuff.

carbohydratesn · Post by **carbohydratesn** » Mon May 04, 2015 12:52 pm

I collect heads slower too, to ensure they stack better - I was under the impression that you can generally collect hearts faster than any other part of the process, because there are less volatile compounds to stack. Ethanol dominates in the hearts, so you can go faster. But the heads are made of many different compounds, in small amounts - going slower makes sure the heads are as compact as possible.

I'm still very new at this, so that could just be a misunderstanding on my part. I haven't experimented with collecting heads faster/slower to compare yet. And I also slow down to collect tails, again to compress the fractions as much as possible. They get smeared all over the place if the takeoff rate isn't dropped.

Hound Dog · Post by **Hound Dog** » Mon May 04, 2015 3:43 pm

carbohydratesn wrote: And I also slow down to collect tails, again to compress the fractions as much as possible. They get smeared all over the place if the takeoff rate isn't dropped.

Once I hit tails I go balls to the wall. I usually just keep tails for the faints jug so why worry about what smears?

I do get it that some people blend tails back for flavor. I haven't gotten to that point yet. If I am doing a rum or whiskey in my LM I run it a bit faster so the temp drops a bit and pulls a bit more flavor through. Guess that is just smearing as you go instead of blending back. I need to try it both ways really. My way is pulling some early tails through and not condensing just late tails as DAD describes.

sergiolis · Post by **sergiolis** » Tue May 05, 2015 9:34 am

Hound Dog is right, you can go at maximum speed once you decide you are in tails and then you can recycle these tails like feints. In my case at the moment I'm just running Allbran. When I have stripped 4x 25 L washes of Allbran I add these stripping runs to the boiler keeping a 40%ABV (22.5L) and I run it with SPP. Foreshots, Heads and early Tails are divided in 200ml jars. The first 400ml are foreshots, Then I get 5x200ml jars of heads, 6L of hearts at 96%ABV (approximetly) and some jars of tails. When I'm sure I'm in tails I speed up the collection until I'm collecting at 75%ABV.
I throw away foreshots and the rest is recycled. When I have enough feints I run all of them again with SPP and I get similar results, to be honest, a little less.
I'm a bit paranoic with collecting the last tails because I think is harder to clean it up the column filled with SPP. Thats why when I'm collecting at 80 or 75%ABV I stop the run. I'm not sure about that but it is my intuition... What do you think about it??
Thanks for your opinions guys...

sergiolis · Post by **sergiolis** » Fri May 22, 2015 6:33 am

Hi guys, Finally I got a sight glass and it's wonderful because you can control the liquid environment in the column.... Do you recommend to keep the boiling liquid over the packing during the whole run to get the maximum possible reflux ?

DAD300 · Post by **DAD300** » Fri May 22, 2015 6:36 am

I would say in the packing. Over and you might be limiting reflux penetration.

sergiolis · Post by **sergiolis** » Fri May 22, 2015 7:06 am

Do you mean at the same level of the scrubber on the top?

Post by **Odin** » Fri May 22, 2015 7:57 am

Few things on the above posts. Sharing from my experience.
- 2 inch column in perfect conditions should be able to handle 2.8 kw (with the right SPP), producing some 4 liters per hour;
- More power = more reflux = lower HETP = more efficient working;
- I wouldn't go lower than 2 kw, which translates to around 3.25 liters per hour;
- If an uninsulated column works better, the Q is "why?" Maybe the column without insulation creates more passive reflux and more reflux equals ... well, see the point above;
- The squirting Sergiolis faced indicates pressure build-up, which can be caused by by column blockage;
- Column blockage can be caused by a few things:
1. Too much power equals too much reflux and reflux filling up the column, thus creating underpressure above flooding and/or overpressure under it, which - in terms - prevents gasses to rise up from the boiler;
2. Overfilled boiler (boil-up preventing reflux returning down the column);
3. Ethanol blockage: if you redistill >30% the SPP is so efficient that it will take the gasses/reflux to pure azeo in just centimeters from where the column starts ... preventing the possibility of a temperature grade to develop ... thus preventing gasses to rise further => column blocking.

Too small SPP will be relatively inefficient. Not so much because of the relative smallness in relation to the column diameter (size SPP should be < column size devided by 10) but because it has the tendency to compact too much. This prevents good refluxing action and distorts optimal shape.

Too big SPP causes another problem. If size is bigger than one tenth of column diameter, you get vapour channeling. With SPP you can distill with more power and performance. Remember the surface area of evaporation theory is replaced by the bullit in fishtank metaphore to explain what happens to rizing gasses and how they get separated, when working with SPP ... so the one thing you don't want is creating "chimneys" of gasses that can travel (at very high speeds!) directly from boiler to take-off.

If you look at how SPP works in practice, you'll see it creates liquid baths at the beginning of the column (water being refluxed out) and at the top (reflux from the column cooler). That's also why you don't want to put a bigger bubble cap or bubble ball under an SPP packed column. That will prevent a liquid bath to develop at the bottom of the column (among other things). Also, no bigger / wider column parts near the top. Actually, one diameter is pretty essential.

I hope this information helps!

Sergiolis, one last remark: I'd put the copper scrubbers in a separate section under the column. With a stainless screen or scrubber on top. Then the section with SPP, starting with another SS scrubber. That way you prevent (or at least minimize) copper particles blowing into your (already small?) SPP, thus hampering its performance.

Regards, Odin.

sergiolis · Post by **sergiolis** » Fri May 22, 2015 9:34 am

Hi Odin! That's a great explanation and I realize that according to your advices I'm wrong in some points.
My boiler is a 30L keg and I'm filling it to 22.5 or 23L. I hope this is not too much. But I'm charging it wit 38% ABV
I start putting 3 copper scrubbers, then 2 stainless steel scrubbers ( to hold the great weight of the SPP). This first 8 cm are filled with both scrubbers and then 112cm of SPP and finally on the top a stainless steel scrubber.
Yesterday was my first time using the sight glass. And I realised that, at the begining of the run, more than 1950W and the liquid was flooding over the packing. So I guess my last issues with the take-off were about flooding because i were running at about 2150W.
But Odin you say that a 2 inch column in perfect conditions should be able to handle 2.8 kw... I would like to get that power but I noticed my column in equilibrium at about 2000W and at the end of the run I could push until 2200W. I was collecting the hearts at 32ml/min and 95.5 or 95%ABV. But maybe I could go faster. I will try it.
I didn't insulate the column but now having a sight-glass I will try it again.
So according to your experience i could start redistilling the stripping runs at less than 30%. If you think I'm wrong in more matters please let me know.

I really appreciate your help. Thanks a lot!!!
That's my SPP:
http://pracowniametaloplastyczna.pl/en/my-spp" onclick="window.open(this.href);return false;" rel="nofollow

Post by **Odin** » Fri May 22, 2015 10:03 am

Size looks good. HETP for sure aint 1.6 mm. Not even 16 mm. Closer to 25 mm or 2,5 cm or 1 inch. No problem though.

Sergiolis, is the internal diameter of the glass section bigger than the 2 inch column?

You should see flooding in the top part sight glas. If it is the same internal diameter. You might even pack it a bit higher.

Other Q. how did you enter the SPP in the column? 2 kw during stabilization is fine. It should handle more (or be able to do so) when product is being taken off. Product out is actually reflux out, so less reflux in the column and so less chance on column flooding.

I ask, because my guess is you might have overpacked the column. Did you push it down? Throw it in hard?

Also your take off rate should be much higher.

So, yes, a few Q's and a few suggestions. Take the column off, take out the SPP. Boil it in a few liters of water with one liter of vinegar for an hour. Then rinse it. Then pack it but gently. I expect you to see you need less now, to pack it! No problem. Means you might have overpacked.

Cleaning I advice, because you may have overfilled the boiler and you got boil up. That defiantly made copper enter the column.

And I advice you to dilute to 30% next time. With 38% you may well have encountered ethanol blockage, Serge!

Above, someone asked how you can detect column flooding. Not the normal baths at the top and bottom, but like too much reflux. Easy:
- Column starts to make a sound and vibrate;
- Liquid comes out of the top pressure equalization hole;
- Output is irregular with ups and downs;
- Temperature at the top starts to sway up and down (column flooding near the top) or at the bottom (column flooding problem at the bottom of the column.

Regards, Odin.

sergiolis · Post by **sergiolis** » Sat May 23, 2015 11:57 pm

Hi Odin,
I can't measure the ID of the sight glass but the specs about the glass say it has 49mm ID so I guess it is 2mm smaller than my Column ID.
Definitely I will clean the SPP and I will dilute to 30% next run. I need to do a feints run so it's a good chance to make some tests.
I will insulate too and I will try to get a faster take-off. Im a bit worried about wasting water and usually I don't push the take-off too much but next time I will try it.
Let's see if i can get at least 2.5L/h.....
Thanks a lot for your great help!!!

Home Distiller

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