making potassium (per) chlorate

[oldmanbeefjerky]

hmm, well my friend told me a while ago my atx will NEVER pull a full 30 amps in the small cell i want to use (1-3L), or even 2 amps.

not unless i went and did electrolysis in something in a large fish tank, thenm maybe ide come close.

 

 

i think ill ask the guy selling ammeters on ebay if they have internal shunts, if not , ill buy one for myself . case closed.

 

this new information though is most distressing!

plastic gets eaten away, glass gets eaten away and poisons the anodes! is there anything that it is safe to build a chlorate cell out of that wont die? or is it just polyurethane?

perhaps i should try getting some massive PVC pipes to build my cell from, as pool chlorinators seem to be made from it, obviously it holds up to years of chlorine gas corrosion!

and i just love building things from PVC pipe like my potato launcher and vandegraff generator.

[WSM]

hmm, well my friend told me a while ago my atx will NEVER pull a full 30 amps in the small cell i want to use (1-3L), or even 2 amps.

not unless i went and did electrolysis in something in a large fish tank, thenm maybe ide come close.

i think ill ask the guy selling ammeters on ebay if they have internal shunts, if not , ill buy one for myself . case closed.

this new information though is most distressing!

plastic gets eaten away, glass gets eaten away and poisons the anodes! is there anything that it is safe to build a chlorate cell out of that wont die? or is it just polyurethane?

perhaps i should try getting some massive PVC pipes to build my cell from, as pool chlorinators seem to be made from it, obviously it holds up to years of chlorine gas corrosion!

and i just love building things from PVC pipe like my potato launcher and vandegraff generator.

 

Hi OMBJ,

 

I build my cells from PVC pipe and PVC plate. It holds up well as a cell tank material. The wall thickness isn't important generally but sometimes you want to wrap the cell with insulation to keep temperatures correct. The maximum temperature workable for PVC is 60^oC, 93^oC for CPVC (which is a great material but MUCH more expensive than PVC and harder to locate).

 

WSM

[oldmanbeefjerky]

i think i might be able to get some for free, but in small peices.

though i plan on keeping my cell cooled for most of the time, as my ventilation, which will run through the cell once bubbling chlorine through before venting into the atmosphere, will also be cooling the cell.

 

i just wanted to say by (yet to be sep) granfather, has said he can get me plain titanium mesh and will send me some in september, he also may be able to get me solid strips for power connectors, so fingers crossed...

[Tesla]

Hi, I'm new to the form and have a few questions.

 

1 Do I need to really worry about ph if I use potassiumchloride instead of sodium chloride?

 

2 Can you sell potassium chlorate/potassium perchlorateonline (Ebay) or do you need a permit?

 

Any help given would be greatly appreciated!

 

 

[Bonny]

Hi, I'm new to the form and have a few questions.

 

1 Do I need to really worry about ph if I use potassiumchloride instead of sodium chloride?

 

2 Can you sell potassium chlorate/potassium perchlorateonline (Ebay) or do you need a permit?

 

Any help given would be greatly appreciated!

 

 

 

 

1) No you don't need to worry about ph, regardless of what the chloride is (sodium/potassium). Ph control increases the efficiency of the cell. I have never bothered with ph control. Although much less efficient, my cell was pounding out the chlorate (much faster than I would ever use...)

 

2) Not sure, but I wouldn't!!

[oldmanbeefjerky]

the answer is no, you cant buy or send chlorate as it is considerd illegal to use in allot of things as it can be used to build plastic explosives with extremely common household materials, and due to its instability will never be allowed on a plane without a permit stating where is going, who its going to what itle used for, and proof its chemically pure and /or stable, or it must be with a international courier , which will cost you $40-70 for anything up to 20kg of chlorate or a standard national courier which will probably cost a little over half that.

 

perchlorate on the other hand is chemically stable, so only dangerous goods laws affect it meaning it cant be sent on a plane without a shipping permit and it must be packed properly if being by plane.

 

potassium perchlorate should be legal to sell on ebay, but askt hem anyway. there are sellers in japan who sell it in super pure lab grade form, for ridiculously large amounts of money, so if they can im sure you can also. but ask them anyway!

Edited July 19, 2011 by oldmanbeefjerky

[dagabu]

the answer is no, you cant buy or send chlorate as it is considerd illegal to use in allot of things as it can be used to build plastic explosives with extremely common household materials, and due to its instability will never be allowed on a plane without a permit stating where is going, who its going to what itle used for, and proof its chemically pure and /or stable, or it must be with a international courier , which will cost you $40-70 for anything up to 20kg of chlorate or a standard national courier which will probably cost a little over half that.

 

perchlorate on the other hand is chemically stable, so only dangerous goods laws affect it meaning it cant be sent on a plane without a shipping permit and it must be packed properly if being by plane.

 

potassium perchlorate should be legal to sell on ebay, but askt hem anyway. there are sellers in japan who sell it in super pure lab grade form, for ridiculously large amounts of money, so if they can im sure you can also. but ask them anyway!

 

Do you live in the USA? If so, you are wrong about the legality of selling chlorate, several suppliers sell chlorate online and ship USPS using ORM-D pub 52, ground shipping at no additional cost. There is a weight limit per package and bulk purchases must be reported but that's it.

 

-dag

[Mumbles]

As far as the US and the UN are concerned you can sell and ship it with somewhat minimal hassle, at least domestically. Australia may have somewhat more stringent laws. It would seem odd that they'd target chlorate and not perchlorate however. I'd think they'd just like to kill several birds with one stone and regulate all inorganic chlorates and perchlorates the same way. Except for sodium chlorate, they have very few if any "accepted" domestic uses.

[oldmanbeefjerky]

i was talking about bulk amounts of chlorate. perchlorate isnt treated any different to nitrate, and as an oxidizer is classed as a harzardous good, so there are restrictions with sending it by air , but not by ground

if it was legal to sell though ide be making heaps and selling it on my site as the only chlorate seller in australia! but of course i cant so i cant at least not without proper permits, and they cost heaps.

 

chlorate is targeted because its less stable than perchorate (more stable than nitrate even), and because the majority of its uses include high explosives, but there arent much (if any) restrictions on perchlorates anywhere

[pdfbq]

I believe 50AE was having issues with his glass cell. I believe we had deduced that the alkaline environment was slowly eating away the glass walls and depositing it on the electrode surface, slowly killing it. I for the life of me cannot find the post right now.

It was me having these problems.

 

(Click the arrow to jump to the post)

I destroyed some anodes before I found out. Swapped to HDPE and problems were over.

 

(Click the arrow to jump to the post)

Maybe a better quality of glass would also prevent these problems but I would not take that risk myself.

Edited July 20, 2011 by pdfbq

[WSM]

It was me having these problems.

I destroyed some anodes before I found out. Swapped to HDPE and problems were over.

Maybe a better quality of glass would also prevent these problems but I would not take that risk myself.

 

I'm not sure about the quality of glass but my first successful chlorate cell was a one gallon glass pickle jar with a PVC pipe cap for a lid. It had no pH control, no temperature control and had no problems whatever. It just ran and ran, batch after batch. I don't know if the mild acid of the pickle juice stabilized the glass but it never showed any degradation. The anode was a DeNora 1/8" diameter MMO on titanium rod and the cathode a 3/4" diameter CP titanium tube.

 

 

It was certainly nothing fancy, but it worked. I later upgraded the anode to the same thing but larger; 1/4" diameter. I set the whole thing aside when I saw Carl Tauch's continuous chlorate system on pyrobin and have worked ever since on my own variation. Mine is a work in progress and is totally a "proof of concept" project. I love the challenge.

 

WSM

[oldmanbeefjerky]

how frightening!

however, a pickle jar is truely perfect for my starting chlorate cell! right size and everything! plus it doesnt destroy the anodes which is great also!

WSM you are a living legend!

 

acetic acid seems to be able to react with anything given the time, so maybe, it has reacted or maybe its a different type of glass or the picklers just use a high quality impurity free glass? impurities make all the difference, especially if barium salts or other poisons to anodes were to find their ways into the glass. im not saying it was barium, but im sure that there are other poisons which could be released and do the damage, or maybe the acetic acid removed these impurities! which makes the most sense!

 

maybe, just maybe!

Edited July 20, 2011 by oldmanbeefjerky

[Mumbles]

chlorate is targeted because its less stable than perchorate (more stable than nitrate even), and because the majority of its uses include high explosives, but there arent much (if any) restrictions on perchlorates anywhere

 

No one makes cheddites anymore. The overwhelming majority of chlorate around the world is used to make matches and oxygen generators, which are far from a high explosive.

[oldmanbeefjerky]

commercially perhaps,

i think ill do some digging into exactly what im allowed to do with my chlorate. i know that a few years back a national product recall was made on anything that had more than 5% chlorate, for all stores everywhere, so i cant be sure of the legality of chlorate for selling.

though if people are willing to buy perchlorate off me, i might get some lead nitrate and copper nitrate or platinized Titanium anodes to convert chlorate to perchlorate for selling, because i know for a fact its legal!

[Bonny]

I started my perc cell today with the LD anode and Ti cathode. I'm using a PC power supply on the 5V wires. My ammeter went for an instant shit though. It was reading ~8A then just quit. I tested between the electrodes with a multimeter and was reading (again)about 8 amps. The cell is an 18l bucket cell. I started with 110g/l of KClO3 assuming the cell will maintain about 30C. I am running a small bubbler into the cell to help regulate temperature, as from my experience the top of the cell where the electrodes are is always hotter. Anyway, as in the past I can smell the ozone being generated.

 

From my notes it takes about 50ah/100g at 100% efficiency for conversion. I have 1980g and am (hoping for) 70% efficiency, although it will likely be much lower.

So, ina perfect world:

 

50 x 19.8 / 8 = 123.75 hrs or 5.15 days.

 

i think I'll run the cell for about 6-7 days and see what happens.

[WSM]

Awesome! Good luck, Bonny.

 

Are you taking photos of the setup and process, as well as the results? It may be informative if you do. Thanks.

 

WSM

Edited July 21, 2011 by WSM

[oldmanbeefjerky]

i look forward to hearing about the results

[Bonny]

I probably won't take any photos, the setup looks the same as my other bucket cell(s). There is one on this thread, back a few years, apge 25 or 26. I will be taking notes though. My first observation (the low amperage) I think is due to the electrode spacing. I set them at ~1" apart, the same distance I had my MMO set up making chlorate. No idea what I was thinking, I looked back on this thread and found when I used my Pt anode, spacing was only about 1/4". I think I'll shut the cell down and bend the shank of the cathode today to try and get more juice flowing.

 

The temp where I live has been very hot the last few days, and I took that into account when I estimated my cell temp. Anyway, the temp dropped last night and the cell temp did too. I'm hoping I did not get much chlorate dropping out of solution.

 

I am going to take better notes this time around, as in the psat my notes have been spotty at best.

[Tesla]

Do you guys think a sodium cloride cell is better than potassium cloride cell, or vice versa?

[Mumbles]

The advantage that a sodium cell has is that t he corresponding chlorates and perchlorates are more soluble. NaCl is typically incredibly inexpensive too. You really cannot run a perchlorate cell on potassium. The solubility is just too low in general.

[WSM]

The advantage that a sodium cell has is that t he corresponding chlorates and perchlorates are more soluble. NaCl is typically incredibly inexpensive too. You really cannot run a perchlorate cell on potassium. The solubility is just too low in general.

 

The first and second sentences are correct. The third sentence isn't technically correct; you can but it has problems (based on the fact stated in the fourth sentence).

 

Because of these facts, I've decided to base my perchlorate experiments using LD mesh anodes on sodium salts rather than potassium. I believe with careful attention to detail, the sodium perchlorate can be converted to potassium perchlorate and washed of nearly all the sodium ions (at least enough to give no sodium contamination to the flames of stars and other pyrotechnic effects). I'll still use the direct route for potassium chlorate (KCl -> KClO₃), but for potassium perchlorate I'm considering (NaCl -> NaClO₃ -> NaClO₄ -> KClO₄).

 

WSM

[Mumbles]

I was talking in practical senses. You can run a potassium perchlorate cell, but it probably is not be worth it. You'd get incredibly sodium free product, but in very low yields most likely. I would imagine that it would be more difficult to separate the chlorate impurity as well.

[oldmanbeefjerky]

Too much precipitation!

i think i saw a photo in one of the blogs a while ago which showed that all the potassium perchlorate forming just stuck to the anode.

[Bonny]

I was talking in practical senses. You can run a potassium perchlorate cell, but it probably is not be worth it. You'd get incredibly sodium free product, but in very low yields most likely. I would imagine that it would be more difficult to separate the chlorate impurity as well.

 

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.

 

 

Too much precipitation!

i think i saw a photo in one of the blogs a while ago which showed that all the potassium perchlorate forming just stuck to the anode.

 

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 electrodes 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 components, 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.

Edited July 22, 2011 by Bonny

[WSM]

I was talking in practical senses. You can run a potassium perchlorate cell, but it probably is not be worth it. You'd get incredibly sodium free product, but in very low yields most likely. I would imagine that it would be more difficult to separate the chlorate impurity as well.

 

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