making potassium (per) chlorate

[WSM]

I am using PP container and have not experienced any erosion of the container. Just use whatever they use to put bleach into because that's essentially what a non PH controlled cell is...

I have a few parts that are polypropylene and normally it performs reasonably well in a cell. According to the compatibility list in various catalogs, PP doesn't fair quite as well as PVC, Kynar or Teflon, but much better than many other materials.

 

I think Arthur's right and we're better off using pH control is our systems.

 

WSM

Edited June 7, 2014 by WSM

[oldmanbeefjerky]

hmm, i have been wondering, since i want to do a few automated things with my chlorate cell, are there any amp/hour or watthour progress charts or anything like that with which i could use to base a constant acid release off of?
a chart which would essentially show how much hydroxide/chlorite builds up over so many watthours/amphours of electrolysis.
unless of course its not neccesary, that im safe just injecting an amount based on whatever the current is or how much power has gone into the cell each hour.

Im really looking forward to havving a reason to set up my condenser, to distill some acid, and also finally build a peltier driven liquid cooler also. Plus i need an excuse to put together a stepper driver also.

[Arthur]

Swede never found a good simple and cheap way of monitoring the pH let alone automating the dosage of HCl. We can add HCl at an approximate guestimate of rate but Swede's findings were that cheap pH probes didn't last more than hours and the (hypo)chlorate formed bleached any usual pH indicator (or indicator paper)

 

I do remember from when I worked in a lab, that the auto fill burette system for strong alkalis used to etch the glassware -The etched material must be somewhere and my form deposits just where it's not wanted.

[WSM]

I have a few parts that are polypropylene and normally it performs reasonably well in a cell. According to the compatibility list in various catalogs, PP doesn't fair quite as well as PVC, Kynar or Teflon, but much better than many other materials.

I think Arthur's right and we're better off using pH control is our systems.

WSM

After a little more research, I've learned that polypropylene is compatible with salt solution and chlorate solution, but not hypochlorite solutions. I suppose we can expect eventual degradation of PP components in direct contact with the cell liquor.

 

Too bad, they're much less expensive than a lot of other polymers.

 

WSM

Edited June 9, 2014 by WSM

[WSM]

Swede never found a good simple and cheap way of monitoring the pH let alone automating the dosage of HCl. We can add HCl at an approximate guestimate of rate but Swede's findings were that cheap pH probes didn't last more than hours and the (hypo)chlorate formed bleached any usual pH indicator (or indicator paper)

 

I do remember from when I worked in a lab, that the auto fill burette system for strong alkalis used to etch the glassware -The etched material must be somewhere and my form deposits just where it's not wanted.

 

 

Swede did agree with Dann2 about timed doses of HCl based on current consumption, and shared it as:

 

0.057 ml of concentrated (32%) HCl per ampere, per hour, with the HCl delivery cut by 33% after the chlorate crystals begin to form.

 

At the very least, this is a good starting point!

 

WSM

[taiwanluthiers]

I get the feeling that perchlorate production don't seem to be a priority. Most of the discussion seems centered on producing chlorate either by a continuous process or ph control. Why is that?

[WSM]

I get the feeling that perchlorate production don't seem to be a priority. Most of the discussion seems centered on producing chlorate either by a continuous process or ph control. Why is that?

When we're ready for perchlorate production, we'll need a steady supply of good chlorate for feed stock, won't we?

 

WSM

Edited June 10, 2014 by WSM

[Arthur]

Unless a reliable and environmentally friendly method of making lead dioxide electrodes is found -and I don't know if anyone is trying. We are stuck with two stage production 1/ chloride to chlorate, 2/ chlorate to perc.

 

I've tried to price a platinum electrode and for a small one 20mm x 40mm it's likely to cost £500.

 

I can see that in areas where DIY oxidisers are required then a return to Weingart style formulations may become necessary.

 

IIRC Swede's Bucket Cell Adaptor was created so that cheap and easy tubs could be used and discarded while the expensive electrodes were assembled into a structurally robust piece of cPVC work.

Edited June 10, 2014 by Arthur

[taiwanluthiers]

I keep seeing 1 micron platinum coated anodes out there on ebay for not a lot of money. It certainly costs a lot less than 500 pounds. Honestly for 500 pounds you might as well buy half an ounce of platinum bullion and roll it into something thinner...

[dangerousamateur]

Even If i had a working LD anode, i would rather use MMO for the chlorate work and save my LD for the second half of the work.

 

A problem with the LD anode is that you need HNO3 to make it, but in the EU HNO3 will be forbidden and practically unavailable in future.

 

Weingart style formulations may become necessary.

Can you give an example for such a formula? Are these organic chlorate stars?

[WSM]

Unless a reliable and environmentally friendly method of making lead dioxide electrodes is found -and I don't know if anyone is trying. We are stuck with two stage production 1/ chloride to chlorate, 2/ chlorate to perc.

I've tried to price a platinum electrode and for a small one 20mm x 40mm it's likely to cost £500. I can see that in areas where DIY oxidisers are required then a return to Weingart style formulations may become necessary.

IIRC Swede's Bucket Cell Adaptor was created so that cheap and easy tubs could be used and discarded while the expensive electrodes were assembled into a structurally robust piece of cPVC work.

 

I remember reading a symposia submission from India detailing how a system was set up and run to make chloride to chlorate to perchlorate in one cell. The crux of the system was their anode (LD on graphite) and the addition of a small amount of NaF to the liquor. Over the process of time, the chloride diminished as the chlorate increased, then when the chloride was below a certain low percent the perchlorate increased and the chlorate diminished, ultimately leaving the perchlorate in high enough concentration to be useful.

 

With a standard LD anode (LD on titanium), I suspect the required NaF would attack the titanium and ultimately render the anode inert.

 

If platinized titanium electrodes are that dear, I suggest continuing the search till you find a supplier with more reasonable prices.

 

WSM

[WSM]

I keep seeing 1 micron platinum coated anodes out there on ebay for not a lot of money. It certainly costs a lot less than 500 pounds. Honestly for 500 pounds you might as well buy half an ounce of platinum bullion and roll it into something thinner...

 

 

There are manufacturers of platinized titanium anodes that plate thicker layers of platinum, for longer life of the electrode and harsher conditions. If one had access to platinum foil (or could form it from small bullion pieces), the potential exists for making perchlorate anodes at home.

 

WSM

Edited June 10, 2014 by WSM

[taiwanluthiers]

Yes I've seen anywhere from 1 or 2 microns. I am sure thicker platings exist but they cost exponentially more. Not sure how much the 1 microns last (according to the oxidizing site, they last quite a while if used properly), but a 20 micron platinized titanium costs more than 20 1 micron anodes of the same size. If I could figure out how to plate platinum and renew those platinized titanium, then I could use bullions as a feed stock...

 

The other problem is I can't find anyone who sells thicker platinized titanium. All the ones on ebay and elsewhere are 1 to 2 microns, and are really designed for jewelry plating. The companies who makes them appears to be b2b only.

 

If you know where I can buy them, I'm all ears.

[Arthur]

The electrode I mentioned was a custom pure platinum electrode made by a jeweller with experience in platinum. I can possible find MMO locally and platinised electrodes but at silly money for what little platinum there really is.

[pex]

My perchlorate cell finished a few weeks aggo i almost harvested 8 kilo. Pottasium perchlorate. The run of the cell 1 mond. I tested the finished product with indigo. After cleaning no traises of chlorate. ☺ i can't place picture. Because it's not allowed in my country. The anode looking still good.

 

Pex

[WSM]

The electrode I mentioned was a custom pure platinum electrode made by a jeweller with experience in platinum. I can possible find MMO locally and platinised electrodes but at silly money for what little platinum there really is.

 

I'm curious, is it pure platinum? Typical jeweller's platinum is alloyed with iridium.

 

Iridium adds benefits to an MMO mixture, but I don't know it's effects in perchlorate electrodes.

 

WSM

Edited June 11, 2014 by WSM

[pyrojig]

This is really getting some attention on this thread.!!!!

@ WSM . I think there is a patent that claims some irridium in the mix is fine for the use in perch production . It may have qualities that allow the platinum to adhere better to the substraint on the electrode ( such as MMO coating , coated with this precious metal)

[dangerousamateur]

@Pex:

In what county do you live, where perchlorate is not allowed (but chlorate is???)

[schroedinger]

Iridium is fine for use in these cells. There is are a couple patents writing about it (sorry i read those about 1 year ago, so don't know which patent it where and the hoster where i safed the link is down). One of the patents also claimed that Iridium is better suited ghan the pure platinium.

[Arthur]

My only supply of Pt is pure, but I suspect that the assembly will be soldered with a Pt/Ir mix. IIRC Alan Yates in Australia had some success with a short piece of Pt wire but turning the current up caused the wire to corrode through.

 

Does anyone have reference for the current density at a Pt electrode, and what rate of production could be possible at that current?

 

NO guesses please Pt is too expensive to guess whether it's going to dissolve.

[WSM]

This is really getting some attention on this thread.!!!!

@ WSM . I think there is a patent that claims some irridium in the mix is fine for the use in perch production . It may have qualities that allow the platinum to adhere better to the substraint on the electrode ( such as MMO coating , coated with this precious metal)

 

It is mentioned in several MMO patents (and proven to be there by analysis), and notibly, in the pyrochlore patent application (which was primarily for safe [lead free] and inexpensive [platinum free] ozone production). As an aside, the application mentions that the anode can also turn chlorate into perchlorate.

 

WSM

[WSM]

My perchlorate cell finished a few weeks aggo i almost harvested 8 kilo. Pottasium perchlorate. The run of the cell 1 mond. I tested the finished product with indigo. After cleaning no traises of chlorate. ☺ i can't place picture. Because it's not allowed in my country. The anode looking still good.

Pex

That's brilliant. Can you share more details of your setup, especially the running conditions, such as:

 

Voltage

Amperage

Temperature

Concentration of the chlorate feed stock at the start of a run

pH the cell runs at

the rate of perchlorate production (how much produced per hour or day)

 

These and any other details you can share will help many others attempting to follow your lead.

 

Thanks.

 

WSM

 

edit: is your system sodium or potassium based?

Edited June 11, 2014 by WSM

[taiwanluthiers]

more importantly, are you using those 1 micron platinum coated anode or pure platinum wires, or LD?

[WSM]

more importantly, are you using those 1 micron platinum coated anode or pure platinum wires, or LD?

I think he posted photos a little while ago that clearly show he's using LD with a single cathode. I wonder how his system would work with two cathodes?

 

WSM

Edited June 12, 2014 by WSM

[FlaMtnBkr]

I have easy access to oxidizers so I haven't thought about this to much and know nothing about production and have only read the last few pages. But I do like having the knowledge and experimenting with things.

 

Has anyone figured out how much it costs them to make the various oxidizers? Or how much wattage is required? I don't mind using chlorate and certainly it is cheaper than perchlorate. Is it possible to make ammonium perchlorate?

 

I saw a couple things I was going to comment on but will have to read back through to remind myself. I was going to ask if anyone had looked toward bicycle parts for titanium fasteners, but they are likely the wrong alloy. From a quick search it looks like to medical implants are CP (sp? Pure ti). If that is the case it might not hurt to ask any friends in the medical field if they know someone in the operating room or a equipment rep. My wife works in the OR and she had brought home some Ti screws and plates in the past that could not be used for some reason. Might be a potential source for the right Ti. I will have to ask her if she can still get some and maybe pass them on if they are useable.

 

Looks like there is a lot to learn but that it might be a worthwhile endeavor. Especially if it can be produced for a reasonable cost and is somewhat pure. And hopefully I will remember the other things I was going to mention when I'm not as sleepy.