making potassium (per) chlorate

[WSM]

I have never tried a sodium perc cell, but IMO the potassium cell I have running right now is worth it. Even after running less than 24h, there is a healthy layer of crystals on the bottom. I know using a sodium cell would allow much longer run times, but AFAIK the electrical input (time) to convert chlorate to perc, sodium or potassium, is the same gram for gram.

As for separating the chlorate, it is quite easy, although it does require large amounts of water. After harvesting the crystals, a good cold water wash followed by a recrystallization and another cold wash results in a product that reveals almost no chlorate using Swede's NPAA test. I think that a second recrystallization would bring the chlorate to almost undetectable levels...better than Mil spec which allows for 1% chlorate.

Using a Pt anode, I never had any problems like that. I'll know in a few days if it happens with the LD anode I have. I had the cell apart briefly today and the only crystals stuck to anything were a few on the cathode, nothing whatsoever on the anode.

 

Edit:

 

Anyway, I moved the elcetrodes a bit closer today, about 1/2" apart. The cell is chugging along at 4.7V (measured at the top of the electrodes), and just under 10A (hooked up another ammeter I had).

The cell temp is about 35C at the top and 33C at the bottom of the bucket, measured with a laser temp sensor on the outside of the bucket.

Also, when I had the cell open today to move the electrodes closer, there was a bit of dark crap in the bottom, most likely dirt from one of the componenets, but again, I'm sure I saw the tinge of purple colour that we discussed here a year or so ago when I was making perc... WTF is it? Titanium chloride was one idea floated around... I am using an LD anode this time not Pt, so the common thing is the Ti cathode, or maybe the plastic bucket and bubbler tube.

When I harvest the batch I'll have a better look.

 

It sounds good, Bonny. Keep up the good work and keep us up to date with your progress .

 

WSM

[oldmanbeefjerky]

i still dont have my anodes!

i want to be able to do stuff like this too!

[pyrojig]

Im Fascinated with the amazing amount of information on Swedes blog. I know Im risking sounding foolish asking this but, I just wonder what is gained by the use of two cathodes ( front and back of the MMO Anode) . I am pretty sure it does three things , reduces the load on the Ti cathode (reducing heat) , adds more surface area of the cathode( which to my understanding is a bad thing = more catalytic reaction\ break down of the chlorate to chloride.... , and the third is the anode is surrounded by a cathode on ea side making more chlorate, making the best use of all the anodes surface area.

 

It was my understanding that one should keep the surface area of the anode and cathode close to the same. I have been working with graphite 5gal cells for a while now, and Im tired of filtering graphite. I have with Ph control, been able to obtain 75+% CE with no prob. Iv'e been able to yield on average 3-5# a week @ 20+A(of a PC-PS), its just becoming a load of work in the filtering process.

 

So I have to ask , what and how much fudge room is there in anode surface area v.s. cathode surface area?

I see many "kits " that just sell the standard anode and cathode , never a set of 2 cathodes to one anode ( except pool chlorinater's ). But it seems that some of the members on this site have been getting good if not amazing results by altering designs from the normal . (Like a caged cathode surrounding a anode.., see Swedes blog). Any thoughts or ideas are welcome ...

Thanks

Pyrojig

Edited July 22, 2011 by pyrojig

[oldmanbeefjerky]

simple answer. it allows more current to pass through the anode and makes use of ALL of the anodes surface area. remember that when there's only one cathode, electrolysis mainly occurs on the side facing the cathode, the other side may appear to fizzle,but its the other side doing all the work.

really this just evens out things. im pretty sure swede said this in his blog, or someone said thta here 2-3 pages ago along with a photo i think. also that is how pool chlorinators are set up so i dont think it breaks the anode faster.

 

also, if your tired of filtering out graphite, may i consider buying some nylon fluff filters and wrapping your graphite in it, all with inter material of course, or using a very small salt bridge on the cell?

i have done this successfully with converting copper sulfate into sulfuric acid, using cellulose filter paper, however i dont know what the effects of all the chlorine gas will have on the cellulose, probably not good. but still, building a filter should work and if you dont restrict the amount of water access it has, it shouldn't slow the cell down either.

otherwise, if you have no intentional precipitants (such as standard with potassium chlorate cells), get a pool filter , and a cheap plastic pump to constantly filter it for you as it runs, but make sure that if a spillage occurs such as by clogging which is unlikely, have the pump operate through an always off relay, which is tripped when there is current between two electrodes in the filter. if youd like i can draw up a diagram!

i might even consider this when experimenting with different metals so use in place of MMO , like lead, because its very easy to salvage from its oxides once i get my furnace up and running, (reduce the oxides with carbon), and the lead mess is the only problem associated with lead so ive heard.

 

 

i have found a relatively cheap and pure source of potassium chloride, from an online pet store, which can sell me sulfur for $8/kg and potassium chloride $6/kg, and i want to ask, where do most people source their potassium chloride from in australia? and at what price?

[WSM]

i have found a relatively cheap and pure source of potassium chloride, from an online pet store, which can sell me sulfur for $8/kg and potassium chloride $6/kg, and i want to ask, where do most people source their potassium chloride from in australia? and at what price?

 

I don't know about Oz but in the States, potassium water softener salt is available in 40 Lb bags (about 18 Kilos) in some large home supply centers or grocery stores (usually near the more common sodium water softener salt). I haven't found a cheaper source yet (it's about $0.50 a lb or $1.10 per Kilo; US dollars, of course), but I'm still looking...

 

WSM

Edited July 22, 2011 by WSM

[WSM]

i still dont have my anodes!

i want to be able to do stuff like this too!

 

He ships fairly fast, but I imagine the trip across the pond will take a bit longer. I'm sure you'll have them soon enough, if Customs doesn't foul things up (I can't imagine why they would?!).

 

WSM

[Bonny]

Hi Mumbles,

 

I agree except rather than separate the chlorate, destroy it while leaving the perchlorate virtually pure.

 

Swede mentioned using potassium metabisulfite solution to break down the chlorate to soluble products able to be rinsed from the perchlorate with chilled distilled water. This sounded to me like an economical solution to the residual chlorate problem. I believe potassium metabisulfite can be had at low cost from home wine-making suppliers.

 

WSM

 

 

I did try the metabisulfite, but had issues I think due to the poor quality SS pot I was using. I will probably try it again in the near future, as this could allow for only a clean up/recrystallization. Although for small batched I think 2 recrystallizations with good washings will sufficiently clean the product.

[oldmanbeefjerky]

He ships fairly fast, but I imagine the trip across the pond will take a bit longer. I'm sure you'll have them soon enough, if Customs doesn't foul things up (I can't imagine why they would?!).

 

WSM

 

dont jinx it!

 

 

i have come up with a plan to make potassium chlorate without even mildly risking the integrity of my anode!

 

what ill do is electrolyze a saturated solution of potassium chloride, and then after roughly 50% has dropped out as chlorate, i shall filter it off, then super heat the remaining liquid using my furnace as the heat source, until i have a powder whcih i will then react with hydrochloric acid until the ph is neutral, and then i will add more potassium chloride, and re-electrolyze it.

i know this will mean smaller batches, but i think it will also allow me to both be less wasteful and prolong the life of my anodes.

something thats bugging me though, is how i will know once i reach 50%, as thats when i want to stop.

how much weight does chloride gain when it becomes chlorate? also are there any flaws in this idea i havent foreseen?

Edited July 22, 2011 by oldmanbeefjerky

[pyrojig]

I appreciate the response. I will consider the nylon filter idea..., but Im really on the path to use MMO and TI electrodes ..

One Q. I had was, Swede spot welded his Ti shanks or tube to the MMO mesh electrode by a spot weld. Could any spot welder be sufficient to do this job or did it require a specific impulse timed weld ? If I where to use a TIG /MIG to weld it what would it require? (Ti welding wire) I cant imagine that being cheap or worth it ( maybe spring steel would work)... I have access to a spot welder..

I want to basically weld up a set like Swede did. ( but he built his spot/MOT welder )..

 

 

[WSM]

I did try the metabisulfite, but had issues I think due to the poor quality SS pot I was using. I will probably try it again in the near future, as this could allow for only a clean up/recrystallization. Although for small batched I think 2 recrystallizations with good washings will sufficiently clean the product.

 

I think a polymer tank would hold up better. Try PVC, polypropylene or something similar. Either method you describe should work; let us know...

 

WSM

[WSM]

dont jinx it!

how much weight does chloride gain when it becomes chlorate?

 

I once calculated (in a perfect world) 12 lbs of KCl would be converted to 19 lbs of KClO₃. Anything close to that would be awesome !!!

 

WSM

[Tesla]

Does anyone know of a good guide that tells you how to make chlorate/perchlorateout of sodium chloride? I have one for potassium chloride, but now I'm not sureif that's the best choice. Thanks for the help thus far! BTW, can you still use MMO anodes in a sodiumcell?

[WSM]

I appreciate the response. I will consider the nylon filter idea..., but Im really on the path to use MMO and TI electrodes ..

One Q. I had was, Swede spot welded his Ti shanks or tube to the MMO mesh electrode by a spot weld. Could any spot welder be sufficient to do this job or did it require a specific impulse timed weld ? If I where to use a TIG /MIG to weld it what would it require? (Ti welding wire) I cant imagine that being cheap or worth it ( maybe spring steel would work)... I have access to a spot welder..

I want to basically weld up a set like Swede did. ( but he built his spot/MOT welder )..

 

I've had a Harbor Freight spot welder for several years. Later in his work, Swede bought and used a Harbor Freight spot welder, too. They are made in Armenia and seem to work very well if you line up the electrodes properly and face them with a slightly rounded edge on both faces. The cost is near $150 on sale.

 

I apply good pressure and hold the switch till the welder starts to "growl" and a red glow just begins at the weld point. It takes a little practice but soon you'll be spot welding like a pro (of course you should practice on cheap steel instead of expensive titanium till you develop the requisite skills). If you have any other questions on the process, ask and I'll do my best to answer.

 

WSM

Edited July 22, 2011 by WSM

[WSM]

Does anyone know of a good guide that tells you how to make chlorate/perchlorateout of sodium chloride? I have one for potassium chloride, but now I'm not sureif that's the best choice. Thanks for the help thus far! BTW, can you still use MMO anodes in a sodiumcell?

 

What works for potassium works for sodium. The sodium salts get more soluble as they add oxygen, where the potassium gets less soluble as they gain oxygen. Sodium salts (generally) are much more soluble than potassium salts, anyway.

 

MMO with sodium cells? Absolutely. That's what industry does and has for about fourty years.

 

WSM

Edited July 22, 2011 by WSM

[oldmanbeefjerky]

I appreciate the response. I will consider the nylon filter idea..., but Im really on the path to use MMO and TI electrodes ..

One Q. I had was, Swede spot welded his Ti shanks or tube to the MMO mesh electrode by a spot weld. Could any spot welder be sufficient to do this job or did it require a specific impulse timed weld ? If I where to use a TIG /MIG to weld it what would it require? (Ti welding wire) I cant imagine that being cheap or worth it ( maybe spring steel would work)... I have access to a spot welder..

I want to basically weld up a set like Swede did. ( but he built his spot/MOT welder )..

 

 

 

you should try asking swede or looking more thoroughly through his blog, or look up improvised titanium welding on google.

my friend, who knows a thing or two about welding has told me that you need a tungsten welder for titanium (or else it will melt before the titanium), i also suggested a carbon rod too, but he said im might sublime to quickly to be useful though i didnt believe it. its a shame it costs a heap of money to practice titanium welding .

[Bonny]

I appreciate the response. I will consider the nylon filter idea..., but Im really on the path to use MMO and TI electrodes ..

One Q. I had was, Swede spot welded his Ti shanks or tube to the MMO mesh electrode by a spot weld. Could any spot welder be sufficient to do this job or did it require a specific impulse timed weld ? If I where to use a TIG /MIG to weld it what would it require? (Ti welding wire) I cant imagine that being cheap or worth it ( maybe spring steel would work)... I have access to a spot welder..

I want to basically weld up a set like Swede did. ( but he built his spot/MOT welder )..

 

Swede TIG welded Ti using Ti (wire I think) as a filler. There is no reason though that it could not be TIG welded without filler (fused), as the pieces are only about 1/16 thick. I think you are best off going with the spot welder as WSM suggested.

[Tesla]

What works for potassium works for sodium. The sodium salts get more soluble as they add oxygen, where the potassium gets less soluble as they gain oxygen. Sodium salts (generally) are much more soluble than potassium salts, anyway.

 

MMO with sodium cells? Absolutely. That's what industry does and has for about fourty years.

 

WSM

 

 

 

 

 

Ok thanks, I found a guide that tells how to make it bothways. Hears the link if anyone's interested. https://docs.google.com/viewer?a=v&pid=gmail&attid=0.1&thid=12b2f6142ea72542&mt=application/pdf&url=https://mail.google.com/mail/?ui%3D2%26ik%3D4684dcd3ba%26view%3Datt%26th%3D12b2f6142ea72542%26attid%3D0.1%26disp%3Dsafe%26zw&sig=AHIEtbSpAzBVBD_FO6AThzjQxoOa-mYvxQ&pli=1 It says something about a metathesis reaction?(pg9) If I understand it right, youhave to add potassium chloride to the sodium chlorate, a reaction occurs, and you to get potassium chlorate?

 

[Mumbles]

That link isn't working for me.

 

Yes, a metathesis reaction in very simple terms is two molecules swapping parts with each other. In this case it is:

 

NaClO3 + KCl ---> NaCl + KClO3

 

It works because potassium chlorate is significantly less soluble than any of the other parts, so the reaction is driven toward that side of the equation. Some washing with cold water, and one or two crystallizations will get you pretty pure potassium chlorate.

[Bonny]

I opened my cell today to have a look. The botton is covered with a good layer of sugar-like crystals, my previous perc runs also yielded such crystals.

 

The problem is that it's all black!! I think The LD anode is eroding, although visually it looks fine. Maybe this happens on the first run and then it will be OK in future??

 

Once the crop is done I'll try and get a pic. I will most likely pour off most of the liquor before chilling to seperate the black contaminated stuff from what is still in solution.

 

The cell is running about 33C, 8-9A at 4.7V.

 

Oh, and some good news, when I was getting my chlorate out for feedstock, I found a bag with ~5 lbs of raw perc from a year or so ago

[oldmanbeefjerky]

lucky you.

this black layer of lead dioxide which has formed is most probably loose lead dioxide beta, or heaven forbid your anode is composed in any amount of lead dioxide alpha (any as in very slightly or allot ). though i think that there is always some alpha lead dioxide which forms in all LD anodes regardlessly of how its made (all electroplated of course). unless it gets worse there is nothing to worry about. but this is just stuff i vaguely remember from some google blogs or something like that ,so dont take it as anything more than an informed opinion.

 

also i have some great news. I have made a major advancement on my site! due to my own incompetence ive been working on an engine to work out international shipping rates for all my items, an engine which will automatically apply to all new pages i make.

i was building a shipping calculator which had to be used on each page before adding the item to the shopping cart. then i was building a second complex engine to combine all the shipping rates and distinguish between different types of parcel and such, but it was all for waste

i wont ramble on any further about it and steer off topic.

[superstring]

I think we've run out of KCLO4. I need to go to the store and buy another drum. Damn, it's gotten expensive! alomost 4.00 a pound!

[oldmanbeefjerky]

if that price bothers you try searching for a wholesaler or invest for the future and buy in bulk for allot less!

[dagabu]

$2.00 a pound by the drum pre-ordered for delivery to PGI. Ask around Passfire, there are lots of vendors.

 

-dag

[Tesla]

That link isn't working for me.

 

Yes, a metathesis reaction in very simple terms is two molecules swapping parts with each other. In this case it is:

 

NaClO3 + KCl ---> NaCl + KClO3

 

It works because potassium chlorate is significantly less soluble than any of the other parts, so the reaction is driven toward that side of the equation. Some washing with cold water, and one or two crystallizations will get you pretty pure potassium chlorate.

 

 

Cool, I think I get it . Isn’t the sodium method more

expensive though, considering you need to still buy KCI for the metathesis reaction?

Don’t know why the link didn’t work, if you go to Google docks and search Perchlorate_1[1].pdfit might come up.

 

[Mumbles]

Still not working. I possibly don't have permission to view it.

 

Is this the same file though? It fits your description.

http://www.freepyroinfo.com/Pyrotechnic/Perchlorate_1.pdf

 

Yes, it is somewhat more expensive on a chemical level in a way. At least in the US both are really quite inexpensive however. Another thing that I've heard of people doing is recycling the left over solution. When you mix the sodium chlorate and potassium chloride and cool it down, you'll get primarily potassium chlorate precipitating out. The solution you filter off has mostly sodium chloride in it, with a little potassium chloride, potassium chlorate, and sodium chlorate. You can easily reuse that solution, resaturate it with sodium chloride and electrolyze it again. In the long run you essentially are only paying for potassium chloride, and a relatively small amount of sodium chloride to regenerate the liquor.