The Bucket Cell - Start to Finish

[Swede]

I started this off in the giant (per)chlorate thread, but thought it might be worthwhile to stand-alone, mainly because I think it will (hopefully) validate a lot of hard work done in the past. Primarily, the application of the rules and lessons learned that allow someone to run a very simple system that still has high yields, and a high efficiency.

 

This system will have no moving parts, and the only electricity will be for the electrodes themselves. I am going to use a drip acid system for pH that is based upon the acid demand ROT (rule of thumb) derived earlier. It'll also use the efficiency and length-of-run formulas we calculated from a number of runs in the past.

 

Behind the scenes, I am going to verify certain things like pH, chloride ion concentration, and temperature.

 

I left it with the bucket cell pretty much put together:

 

http://www.5bears.com/s2f/s2f027.jpg

 

It could be run with just what's on the adapter: Electrodes, vent, acid port, thermometer port, sample/topoff port. But I wanted to try something I've thought about but never got around to implementing... a cannister that suspends solid KCl in the hot electrolyte, and which will hopefully deliver "bonus" chloride to the system during the days it is in operation.

 

It's made from standard PVC fittings with size adapters to neck it down from 2" to 1" male pipe thread. The body of the cannister is drilled with hundreds of holes, which was immensely tedious.

 

http://www.5bears.com/s2f/s2f035.jpg

 

http://www.5bears.com/s2f/s2f041.jpg

 

The idea is this: The cannister is loaded with heavy KCl chunks, and suspended from the lid of the bucket with a 1" PVC bulkhead adapter. Hot electrolyte circulates through all the holes and gets resaturated with chloride. No solid KCl gets out through the holes. If it does, it should dissolve as the Cl- level drops.

 

http://www.5bears.com/s2f/s2f042.jpg

[Swede]

http://www.5bears.com/s2f/s2f043.jpg

 

It does occupy volume, but the density of Cl- in this cannister is going to be at least 3X to 5X more than liquid, saturated electrolyte. We'll found out if it's worth the trouble. If, after a week or two, the amount of KCl dissolved from this thing is small, then it's not worth pursuing. If it all dissolves in 3 days, it can be recharged on the fly with MORE solid KCl, in theory repeating until the bucket is nearly packed with chlorate solid. And if THAT is the case, the system would beg for a tall bucket, with a lot of space at the bottom for solid KClO3.

 

Along with that device, I set myself up with some cool HDPE barrels. Previously, I had 15 to 20 gallons of various used electrolytes sitting in a corner of my shop. This was messy, and a hazard. These will all be replaced with one barrel, which I will layer with maybe a foot of solid KCl. Everything used ends up in there for recycling.

 

http://www.5bears.com/s2f/s2f038.jpg

 

http://www.5bears.com/s2f/s2f039.jpg

 

I tested one with H2O, and as expected, it weighs more than I can lift. And unless you'd want a motorized or crank pump, siphon is the only way to empty it. Therefore, this thing will need to be elevated before filling (on a stand of some sort), and a simple siphon pump obtained, like this:

 

http://www.5bears.com/s2f/s2f040.jpg

 

Along with the pump and the barrels, I picked up some stuff from U.S. Plastics - some bulkhead fittings, barrel plugs and spouts, and importantly, a polymer barrel bung wrench. These things simply cannot be tightened or loosened without one.

 

 

http://www.5bears.com/s2f/s2f036.jpg

 

These are resting in a 5 gallon pail sieve - I cannot think of a better tool for harvesting and washing multi-kilo batches of heavy wet xtals. These are inexpensive, just a few bucks each.

 

http://www.5bears.com/s2f/s2f037.jpg

 

So... conclusion for now - The bucket cell is ready to go. I am working on calibrating the HCl "hospital IV" drip, as the drip does TWO things... obviously, it works on pH, but it must simultaneously form at least part of a top-off system. The ideal solution would have the acid water doing both, and the liquid level in the bucket remains close to where it needs to be.

 

The amount of liquid lost to evaporation and redox gas evolution is going to vary with temperature, and current, and I'd like to get an idea of what that's going to be during this run.

[Swede]

I just realized a fatal flaw in my scheme... at least with regards to the KCl cannister.

 

Length of run calculations are based purely on volume of the cell, and current. The starting chloride is assumed to be 25 C saturated KCl, which is around 15% Cl- by weight. And the ending Cl- is arbitrary. I normally use 6% Cl-.

 

If I make use of the KCl cannister, it is going to skew the calculations badly. I can always use actual Cl- quantitative methods to track it, but the idea behind this system was simplicity. No annoying tests.

 

Hmmm... I may have to do a run without the cannister, then try one with it, and note the difference.

 

I added another couple of low-tech gadgets to the bucket cell, which I'll show later. This will be fun! I haven't electrolyzed much if at all in a long time!

[WSM]

An excellent topic and posts, so far. I hope I can add to it when the bucket cell I'm building is completed.

 

Good job, Swede!

 

WSM

[patsroom]

I do feel that this topic is well worth a listing of it own. The questions that are asked by so many may all be answered in this thead. I know that you are very complete about the work you undertake and as for myself I look forward to watching this topic as it matures. Swede Thank You for all the hard work that you have done and shared so freely to the rest of us................Pat

[pyroshell]

not going to say any thing specific,but for the record you are not doing this the best way.

[Mumbles]

We're all here to learn pyroshell. I'm sure we'd all benefit from your experience and advice on this matter.

[pyroshell]

I said i would not say anything, that is because i am worried about kewl bombers finding out that they can make perc without their parent knowing.So i will partially stick to that but i will provide some help. Addressing the extra kcl though calculations and years of synthesizes i have found that the optimal amount of kcl(for efficiency) is 580 g/l. That will yield respectfully 836 g/l. heat your water and add the kcl what ever is dissolved will dissolve as the reaction continues you will see that it will dissolve dew to a lower percentage of kcl. with this as my electrolyte and treating the liquor every 2to 3 day with hcl has achieved(for me)a 86% efficiency. If i warm up to the idea of posting despite the kewl bombers ,i might make a thread on the chemistry and practical application of this synthesis.It is not a hard synthesis to preform there is just a lot of misinformation, so you have to go back to the chemistry textbooks.Not tutorials posted online by someone who you ether don't know or hardly know.

[pyrojig]

I think your approaching this from a wrong perspective pyroshell.

 

The ability for a amateur to create his own materials( which may not be able to obtain due to location) is great . Your posting on a "pyro forum" not some knewl bomber site with kids asking how to make AP and other things that go boom. This is a site where pyros take their hobbies to the next level, and or get their questions answered.

 

There is a absolute need for kclo3 for many comps, in which no other oxidizer will suffice. SO the ability for one to source this valuable material is crucial.

 

This however is not the main focus of this project. This is a electrochemistry project. It just so happens that the final product is a oxidizer that recieves lots of crap , due to misuse from foolish people.

 

As said, we are all learning, and if one can learn to become "self-sustained" , it is a good thing. If some kids want to learn how to make illegal/dangerous stuff , they will go to other sites for info. We cant stop that nonsense.

 

SO lets get back on topic : making a bucket cell.

 

@ Swede.

Thank you for the hard work you have been putting into this project. It is a worthy topic, and one that deserves attention of its own . I like the round plate for the BCA that WSM suggested. It makes more sense and the simplicity is nice. There is much to be said about a cheap obtainable system, which uses cheap buckets that are simple to modify, and replaceable when things get worn out.

Edited September 25, 2012 by pyrojig

[taiwanluthiers]

When I first read the topic, I thought it meant a cell that I would build before I die...

[ANFO]

When I first read the topic, I thought it meant a cell that I would build before I die...

 

Thanks to the efforts of Swede, you don't have to spend years ironing out the kinks of this project. All the information you need to do this is here, and if you can source the materials it isn't terribly hard to make. If you think it will take a lifetime to build, maybe you shouldn't attempt the project. Otherwise please don't try to derail the thread

[Swede]

I appreciate the kind words. I'm doing this thing to verify some of the numbers we've worked hard at, numbers and procedures that mean a guy doesn't need a pH meter, doesn't have to guess about how much acid to add, how long to run the thing without smoking the anode due to low chloride, or conversely pulling the plug far earlier than needed. Biggest of all is to do it without ever having to check Cl- levels, which is a pain and can get expensive, because Cl- tests almost all use silver nitrate. The Hach "Quantab" Cl- tests rock, but they are about a buck each, and a typical run, checking Cl- every few days, can run through a dozen of the little buggers.

 

Addressing the extra kcl though calculations and years of synthesizes i have found that the optimal amount of kcl(for efficiency) is 580 g/l. That will yield respectfully 836 g/l. heat your water and add the kcl what ever is dissolved will dissolve as the reaction continues

 

I totally agree and understand that KCl solubility is limited. Heating the electrolyte before powering on works very well. But not everyone has the ability to heat 25 liters of electrolyte, and by starting at a typical room temperature saturated solution, we know how much chloride is in there without doing a Cl- quantitative test. And you are probably very correct that excess KCl solids in the liquor will dissolve as the process continues, I'd personally rather keep the solids separate, so if someone dips in there to gather solids, it'll be 100% chlorate. With a cannister, we can eyeball what's going on in there.

 

This isn't cutting edge, it's not supposed to be. Anyway, my internet connection dumped all day yesterday, so I'm playing catch-up a bit. I'll try to get more stuff up. It's not powered on yet, but hopefully will be soon. I'm also in the middle of a massive shop and lab clean up. With fall finally here, my work area is now down to 100 F. rather than 130 F. Seriously, those are real numbers. There's something about the structure (metal. facing South) and the hideous Texas heat, that combines to make it useless for 5 months a year.

[dagabu]

Swede,

 

Do you have a link for that pail sieve? The only one I could find (for beer) was $10.00.

 

@Pyroshell, I don' know what the tirade you posted was all about but frankly, with only 5 posts yourself and with Swede's 1700 plus posts, YOU could be the k3wl b00m3rz and we would not know. Try a little respect here and be part of a solution (irony not lost on me) to the yield problem (preheating was a good catch) and not be so critical.

 

Hell, I don't know a darn thing about this stuff but I have a better understanding every time one of these fantastic guys posts another tut and writes about their experiences here.

 

-dag

[patsroom]

Do you have a link for that pail sieve? The only one I could find (for beer) was $10.00.

 

 

-dag

 

Hopes this helps. At e-Bay I found 5 gal. bucket filters for bio-diesel but the cost was at $ 10.50 and up. My quest is that the mesh size has a lot to do with.

Speaking of mesh size what would be the best size for filtering. If it is to small will it plug up and slow way down to a stop.

And as for Pyroshell I just about quit trying to tell others of the need to research the complete forum. If only they would they would find so much information as to what is easy to find that would help them to understand things. As for the kewls, well there is not much we can do about them but try to guide them in the right direction.

For most set ups that produce chlorate, it the smell that gives them a way and if not done right then there is the salt damages that show up.

@Pyroshell do lots of reading on the forum here it will help you if your interest lies in chlorate production........Pat

Edited September 25, 2012 by patsroom

[taiwanluthiers]

I am getting some what appears to be conflicting information (or I haven't looked hard enough):

 

People said MMO electrodes allow me to make perchlorates, but others said they're only good for chlorates. Plenty of materials are good for chlorates, heck even battery carbon electrode is good for that.

 

So the only material good for perchlorate production is platinum? Would it be possible to simply take apart a car catalytic converter? What about gold, would that be good for perchlorate production too? I heard of lead dioxide, how does that work?

Edited September 26, 2012 by taiwanluthiers

[pyrojig]

MMO is not geared to produce perch. However if you read any of the material that was posted I believe that it was iridium that had the ability to make perch, but not efficiently. It leaves Platinum and LD on the list of best choices .

[patsroom]

@taiwanluthiers

 

There are only a few materials that works for producing perchlorate that are usable for the amatures and they have all been discussed in other topics on the forum. We truly need not to clog up this topic but to allow Swede to develop this writing into the direction that he wishes for all of us to get the best out of this one.

Below is one place that you can look to find some information that you are looking for:

http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/chlorate.html and I think that for the time being this question should have been addressed to the making potassium (per) chlorate section in the forum. I know that you have been there but if you had read it from start to finish, Swedes blog you'll poke you eye out and the rest of the sites located in the APC forum that deal with the production of prechlorate you would have found most of your answers. Your questions are important and the do deserve to be answered but your first step is to do your homework then if something fails to make sense that would be the time to ask.

I hope that it helps you.......Pat

Edited September 26, 2012 by patsroom

[taiwanluthiers]

The link you posted is dead

[patsroom]

I can not seem to get it in right. I tried a few times but the address messes up......Sorry about that

 

http://web.archive.org/web/20091026132303/http://geocities.com/CapeCanaveral/Campus/5361/chlorate/chlorate.html

Edited September 26, 2012 by patsroom

[taiwanluthiers]

Nice informative site... just got confused with all the conflicting info.

 

It seems Lead Dioxide is the best bet, but where does one obtain lead dioxide anode? I read in there that it needed special process to plate it on, but ebay doesn't sell lead dioxide as anode material (only as powder)

[Mumbles]

Read through all of the resources already pointed out to you multiple times, and the majority of your questions will be answered. These include the (per)chlorate thread, the link provided, and Swede's blog just as a start. Attempting to derail a thread with simple questions that have already been answered dozens of times is a good way to annoy the best people to help.

[taiwanluthiers]

Look I am really sorry for derailing the thread, I wasn't trying to do that.

 

I was looking at the thread title and thought of the move "The bucket list" where they were thinking of stuff they'd do before they die, etc. and it was in no way trying to say that it would take me a lifetime to build a cell like this.

 

I've read the perchlorate thread, not the entire (per)chlorate thread because it's quite long and I read up about using MMO and was only trying to figure out the conflicting information I get about MMO producing perchlorates. I am not really interested in making chlorates because I most likely won't use it anyways due to its risk.

 

So if I frustrated you guys I am really sorry. Perhaps I have a long way to go before I earn enough respect to be on passfire or something but please give me some grace.

 

thanks

[Swede]

Believe me, I'm not a chlorate fan in particular, other than as a precursor to perchlorate. That does not mean it isn't a very useful oxidizer... of course it is. I'll be honest - the reason there is so much focus on it in these threads is because we are still struggling (hard) to come up with cost-effective ways to make the perchlorate. WSM and I have some ideas we are going to pursue, but there are several major obstacles that are tough to overcome. The reagents to make acceptable anodes are hard to get, often freaky expensive, sometimes toxic as all get out, and it's hard to make a good anode.

 

We could give up and spend hundreds of dollars on platinum anodes, but where is the fun in that? Also, if the process isn't well understood and refined, we could simply have a $250 Pt anode disappear. It happened to a guy on Science Madness. In the mean time, we can work on the chlorate process, and a lot of the knowledge does carry forward. And we are making an oxidizer that Skylighter sells for $9/lb for 50 cents.

 

I'm working two projects at the same time right now, along these lines. This one, and also some titanium chemistry, which is coming along in a truly fascinating way. I'll get some pictures up in another thread.

 

Yesterday, I prepared a separate bucket for the KCl. The bottom of the bucket was layered with a surplus of KCl nuggets, and regular water from the hose was added. That's Belle the friendly Brittany.

 

http://www.5bears.com/s2f/s2f044.jpg

 

I agitated the bucket and let it set for several hours, until the water was saturated. I checked the temperature, and it was 32C, fairly warm. In the evening, I checked the chloride level using a Quantab chloride test strip. Again, by doing this, I'm simply verifying that it is, in fact, at the correct level. For a simplistic run which this is trying to emulate, there'd be no need to do this.

 

The liquor should be, according to solubility tables, about 380 grams per liter. Since this is way too high for the test strips, it needs to be dilted 50:1. I used a volumetric pipette to extract 5 ml, and diluted this to 250ml.

 

http://www.5bears.com/s2f/s2f046.jpg

 

http://www.5bears.com/s2f/s2f047.jpg

 

The band crept up to 6,8, which corresponds to 3.477 g/l chloride. Multiplying by 50. this equates to 173.85 grams/liter chloride, or 17.3%, very close to what the solubility table says it should be, which is 380 g/l KCl. That's a nice, expected result.

[Swede]

I added a simple gadget to the bucket cell that's worth sharing, I think. A couple of the common tasks when doing a run is to visually verify the liquid level in your cell if the cell is opaque, and also obtain a sample of the electrolyte for analysis, like pH and chloride. Here is a simple and elegant way to do it.

 

I added a small PVC bulkhead fitting to the lid, which I drilled out to 1/4". Next, I took an old 1ml pipette - any glass tube would do fine - and cut off the skinny tip and flame-polished the end. Near the top, I added a little viton o-ring that fits snugly. This goes into the PVC bulkhead.

 

http://www.5bears.com/s2f/s2f048.jpg

 

 

To use, it, simply place your finger over the end of the pipette, and withdraw it. Set it next to the bucket at the appropriate level, and note where the liquid is in the pipette. I plan on using a marker to calibrate the bucket, with the level of the electrode tops clearly marked. The object obviously is to keep the liquid level where it needs to be. And if you need a sample of electrolyte, simply drain the pipette into a sample cup.

 

http://www.5bears.com/s2f/s2f051.jpg

 

While all this is going on, I've been calibrating my drip system. I re-checked the hospital IV regulator devices, and found that the printed flow rate, like 150 ml/hour, simply isn't accurate enough to rely on, because it varies wildly with head pressure - a higher system means higher flow rates. So the way to go with a drip system is to definitely have a transparent drop chamber, where you can count the drops per minute. Knowing that 12 (or 20, whatever) drops = 1 ml, then the flow rate is easy to calibrate.

 

I've got a trip tomorrow that will take me out of town tomorrow, 27 Sep. I hope to have this thing under power next week early.

[pyrojig]

Good point on the drip Iv setup having an inaccurate count. It is true that for different locations depending on heat, elevation, and weather , these readings will have to be visually checked. I like the pipette idea. Edited September 27, 2012 by pyrojig