making potassium (per) chlorate

[pdfbq]

 

There are a few chlorate(s) that are very unstable. And it does not take much to create a unpleasant surprise which could ruin much more than your day................Pat

http://www.preterhuman.net/texts/terrorism_and_pyrotechnics/explosives/Haarman%20-%20Chlorate%20Screen.txt

I found this. Dont mix it with sulfur . I wonder what will happen if one mixes barium chlorate with sulfur.

[Arthur]

It turns out that those chlorine buckets are very thick polypropylene, not HDPE. Which is a bit of a let down

 

 

 

Arthur, would it be possible to wire two SMPSU's in parallel to increase the current output (say two 30 amp computer PSU's for a possible output of 60 amps), provided they were wired on the same voltage obviously.

 

The idea of the "Bucket Cell" was to enable cheap buckets to be used so try polyprop, try it in a safe place in case it fails.

Some SMPSUs parallel better than others, some even have active current sharing. Study ebay and other web suppliers look for a 5v SMPSU at a big current but be satisfied when you find something! Remember that a 100A power supply will make more cxhlorate than you will use as a hobbyist

[ANFO]

On that note, is 3.3v or 5v better for chlorate production?

 

From what I've seen on chemical resistance charts, polypropylene scores very low against chlorine across all temperatures. An easy way to start testing it would be to expose it to a small amount of chlorine gas and seal it up to see what happens. A small amount of standard pool chlorine and HCl releases chlorine gas. Time to get out the PVC gloves and gas mask.

[Swede]

I'm thinking polypropylene and good, thick HDPE are going to behave similarly, i.e. having adequate strength and resistance for a number of good runs before failure. The idea is, since they are extremely cheap, just replace them regularly, shifting the lid (or adapter) to a new one.

 

ANFO, I'm sorry but I was unable to get Viton into any sort of solution with the common shop solvents, heated or not. It's tough stuff, very resistant. Maybe someone else will have better luck.

[ANFO]

Well on that front I've got about 20 chlorine buckets all for free, so even if they degrade fairly quickly (one good run) that's not a problem.

 

Shame about the Viton, thanks for giving it a go though

[Arthur]

Being realistic, how much chlorate do you want or need? No-one has yet perfected the production of perc on an amateur scale but chlorate is readily workable. As an amateur fireworker (I'm guessing) a few kilos a year would probably suffice. If you had a licensed factory for making fireworks Perc would arrive to order in large drums, probably seived to the mesh range that you want.

[ANFO]

I'm looking at a 30-40 amp, 5litre bucket cell, to produce chlorate for amateur pyro stuff, as well as feed for perchlorate production experiments.

 

So about a kilo a month would be just fine, but this isn't just about making chlorate, this cell project has turned into a hobby all on its own

[WSM]

I'm looking at a 30-40 amp, 5litre bucket cell, to produce chlorate for amateur pyro stuff, as well as feed for perchlorate production experiments.

So about a kilo a month would be just fine, but this isn't just about making chlorate, this cell project has turned into a hobby all on its own

 

HEY!!! I resemble that remark !

 

WSM

[taiwanluthiers]

As for the stroke of a pen making perchlorates and chlorates illegal, making them won't be any more legal either.

 

There's just as much of a likelihood that a stroke of a pen will make all pyrotechnics or fireworks illegal.

[Mumbles]

You really need to quit trying to drag these threads off topic with your opinions, regurgitations of things you've read somewhere, and legal rantings. If you're not adding positively to a topic, you really don't need to be posting anything at all.

[patsroom]

On that note, is 3.3v or 5v better for chlorate production?

 

From what I've seen on chemical resistance charts, polypropylene scores very low against chlorine across all temperatures. An easy way to start testing it would be to expose it to a small amount of chlorine gas and seal it up to see what happens. A small amount of standard pool chlorine and HCl releases chlorine gas. Time to get out the PVC gloves and gas mask.

If I am not wrong you should be able to use standard household bleach to do you test. I beleive that it is that chlorate in the liquid form make bleach if in the proper parts per water and chlorate. By adding the bucket to a larger container of hot water and heating the bucket up should help in determination during testing if the bucket is useable or not.

Edited September 15, 2012 by patsroom

[Swede]

I doubt ANFO's chlorine buckets are anything exotic, but may I toss this out...

 

I've got a pool, and I know the drill with pool chemicals. Materials like granulated hypochlorite and chlorine tablets do come in some extremely high quality, heavy-weight buckets, and when you open the lid on one of these, the gas inside generated by the chlorine compounds can hit you like a sledge hammer. I once took a dose of chlorine that almost knocked me over, it was very nasty. So I think they will do fairly well. DOT shipping rules and product liability dictate that the manufacturers of these chemicals are going to package them in containers adequate for the task.

 

I'm jealous of all his containers. They'd be great for bulk storage of oxidizers, charcoal, anything used in bulk. They usually have screw-down lids with nice gaskets, and by design are gas and water tight.

 

ANFO - can you get ahold of some sheet PVC? Slot that for your straps by chain-drilling a series of holes, and blending them together with a thin file. Then, that section of PVC sheet could be secured to the bucket lid... basically a crude bucket cell adapter.

 

I've thought about putting some BCA's together for sale, but they are really labor intensive, and the only way to really make it work would be to set them up for round-shanked electrodes in modified PVDF compression fittings. Slotting thick PVC is a nightmare, but drilling and tapping a hole for a female pipe thread takes just a few minutes. Since round-shank electrodes are not common, the BCA would have to be sold with them.

 

Idea - a BCA that makes use of two very thick titanium sections as leader segments. Picture two Ti pieces, 25mm wide, 150 mm long, 6mm to 8mm thick. These go through the BCA, and are secured in place by whatever means, preferably quality slots, viton gaskets, maybe PVC plastic welds. On the bottom side are two holes. Two matching holes are drilled in regular electrode straps, and these straps are secured to the BCA stubs by 4 total titanium bolts and nuts. Of course, on the top side are simply one hole each for the electrical connection.

 

One giant viton O-ring could surround both straps. A hole is cut in the bucket lid, and the whole thing secured like a sandwich with Ti or stainless hardware.

[ANFO]

 

Idea - a BCA that makes use of two very thick titanium sections as leader segments. Picture two Ti pieces, 25mm wide, 150 mm long, 6mm to 8mm thick. These go through the BCA, and are secured in place by whatever means, preferably quality slots, viton gaskets, maybe PVC plastic welds. On the bottom side are two holes. Two matching holes are drilled in regular electrode straps, and these straps are secured to the BCA stubs by 4 total titanium bolts and nuts. Of course, on the top side are simply one hole each for the electrical connection.

 

One giant viton O-ring could surround both straps. A hole is cut in the bucket lid, and the whole thing secured like a sandwich with Ti or stainless hardware.

 

There are a few plastic companies around that may sell PVC sheet, I'll ask around and see what's available.

 

That's a good idea, and it also allows you to commit to a very permanent kind of bond between the BCA and the stub, which you might not want to try out on an actual electrode. Something like taking two small pieces of square pvc sheet, which are longer than the stub, then solvent welding them into one piece along the edges, with the stub sandwiched inbetween (filing one or two grooves onto the stub would help it bond better). The flat sheet, with the stub in the middle, can be solvent welded to the top of the BCA over a slot. If that worked it would be a permanent air tight bond.

[Swede]

I like your train of thought. Obviously solvent welding won't even slightly grab titanium, but it would fill gaps. And the Ti leader stubs allow for swapping of electrodes as needed.

 

Most pyros have powdered PVC for comps. Take some of that, and some PVC cement, and mix them together to make a PVC putty. PVC "cleaner", the stuff in the yellow cans here in the USA, would probably be a good thinner if the putty gets too thick. I'd keep the putty on the thin side, like regular epoxy viscosity, so that it'll get a good grab on the solid PVC. Heavily priming the PVC would help as well.

 

Solid PVC pieces probably have to be ordered. U.S. Plastics has PVC squares, sheet, and rectangles.

 

If you go for it, use as heavy a Ti stub leaders as you can find, since Ti is poor as a conductor, and there'll be a lot of heat there if they are too thin. Also, the contact area between stub and electrode would need to be abraded with silicon carbide paper to get rid of the oxides prior to mechanically joining them.

[Swede]

Guys - I have looked at literally thousands of articles and papers on this process. Today I found a jewel. I learned more about MMO in its 9 pages than I had previously. This one is a must-have, IMO. Please take a look at it, save a copy.

 

http://www.waterstarinc.com/files/Resources/White_paper.pdf

 

They discuss what the various oxides do in MMO, the history behind it, under what conditions (temperature, pH, voltage, current density) they deteriorate, etc.

[bikemaster]

Guys - I have looked at literally thousands of articles and papers on this process. Today I found a jewel. I learned more about MMO in its 9 pages than I had previously. This one is a must-have, IMO. Please take a look at it, save a copy.

 

http://www.waterstar...White_paper.pdf

 

They discuss what the various oxides do in MMO, the history behind it, under what conditions (temperature, pH, voltage, current density) they deteriorate, etc.

 

Wow! What a nice find! Additionally, it give you the answer on why there is IrO on MMO electrode. It's write than it give better corrosion resistance at high pH (we don't need it if the cell is pH controled), and IrO also help at low chlorine concentration, because RuO-TiO only electrode start producing oxygen (exactly like an HHO cell) at higher chlorine concentration that RuO-TiO-IrO electrode. This is causing faster errosion of the electrodes. So again, if we don't go too low on chlorine concentration,we can live with "IrO less" MMO electrode!

[Swede]

Yes... Ir and Pt are for oxygen evolution, meaning it extends into the perchlorate-making regime. My guess would be a Ir MMO anode would make perc, but Iridium is just as expensive as Pt, so that's no advantage.

 

pH control for Ru MMO extends the life of the anode. And pool chlorinators add Ir so they can survive low Cl- concentrations, and apparently also for bipolar operations.

 

Good info also on why current density is important... too high a current density, and the MMO suffers.

Edited September 19, 2012 by Swede

[WSM]

Yes... Ir and Pt are for oxygen evolution, meaning it extends into the perchlorate-making regime. My guess would be a Ir MMO anode would make perc, but Iridium is just as expensive as Pt, so that's no advantage.

pH control for Ru MMO extends the life of the anode. And pool chlorinators add Ir so they can survive low Cl- concentrations, and apparently also for bipolar operations.

Good info also on why current density is important... too high a current density, and the MMO suffers.

 

Laserred's MMO is reported to be a ruthenium/iridium type and very durable. Has anyone tried perchlorate with it or with any degree of success?

 

WSM

[graumann]

Bought 4 of them, will report back in a week or so.

[pyroshell]

Laserred's MMO is reported to be a ruthenium/iridium type and very durable. Has anyone tried perchlorate with it or with any degree of success?

 

WSM

i have synthesized chlorate (per) chlorate, and mmo are the only long term plates. they are completely invulnerable to the reaction and sides reactions. Just as a test with a milligram scale i weight the electrodes for a cell, i ran that cell to 2 years at 50 amps switching out electrolyte every 2 weeks. then i cleaned the plates with 15% hcl and the total loss was 0.01 milligrams witch could have been weighing error. so they will last for ever and never contaminate you product. hope this helps if you guys need more info on the detailed synthesis just pm me. A lot of people who talk about it have never tried it or it is there first time i have done many synthesizes of chlorate and (per) chlorate. since i live in the USA i just buy mine now. i t cost more but takes less time, but the end product is the same 99.9% pure perc. if i need just chlorate i still make my own as i almost never need it.

[taiwanluthiers]

Is there anyone who sells MMO mesh plates with the proper connection spot welded like the picture on this thread? I do not have a spot welder so even if I managed to get some MMO plate I would have no way of joining them...

 

I've read about using Pt wires and simply soldering the copper (or brazing, whatever) to the Pt, then seal the connection in a glass tube using a torch. However Pt wires are way too expensive.

 

I searched for laserred on ebay and all he has is a bunch of brass rods.

Edited September 22, 2012 by taiwanluthiers

[Arthur]

Laserred has been the best supplier for MMO Mesh sheet. You then have to source the Ti rod or bar or tube to make the electrode holders, and spot weld them yourself. Whether MMO mesh is a stock item or an occasional "surplus" item passing through Laserred I don't know -keep looking

 

Swede did once have some complete electrodes for sale, but that was years ago.

[taiwanluthiers]

I have no way of spot welding anything, much less Titanium (which I am told requires an inert atmosphere). So I guess that's out...

[Arthur]

Swede said once that his first spot welder was made using a rebuilt microwave oven transformer, his second was a commercial unit. Both worked for titanium and MMO in air not inert gas. Somewhere in your town there will be a welder who will do the few spot welds needed as either a chargeable job, or a side (cash) job.

[Swede]

I will make some more MMO anodes soon if anyone is interested... I actually have maybe a dozen sets stashed away. I'll try and get something on the Agora soon. Apologies for the slowness. These would be the traditional flat-strap anodes. I need to source more commercially pure 1/2" Ti tube for the round-shank jobs.

 

I've tried driving MMO hard to make perchlorate, but had zero success. Unless the coating is very heavy in Iridium, I don't think it's going to work. MMO is hugely cheaper than Pt clad anodes, and since the huge perchlorate factories use Pt, that also tells us that MMO is not suitable for perchlorate.