making potassium (per) chlorate

[WSM]

The electrodes are about 5" x 1.5". New batch running for 2 days now and I got about 1cm in the bottom, I think I am on the good way now.

I did put the cell in a water bucket, this way the temp of the bucket is around 28-30C and the cell in about 40C.

Another question... I know the PH should be in the 6,7 - 7 spot, but how do you adjust it ? When it's too low you add HCL and too high what do you do ?

Also, if some liquer just evaporate, lets say about 1 inch, do you just add saturated kcl to top the cell up ?

 

By my calculation your electrodes will demand about 14.5A, maximum. Maybe the internal resistance is higher because of the distance between the electrodes.

 

The cell goes alkaline as it runs (high pH), so adding HCl lowers the pH. You don't want the pH to get below 6.0 and a bit higher (6.7- 6.8) is the ideal for highest efficiency.

 

The liquor isn't evaporating; the water is consumed in the process. The electrodes break the water into hydrogen and oxygen. The hydrogen basically bubbles away and the oxygen is forced onto the salt (really it's much more complicated than that but, simply speaking, this description describes the idea). Adding KCl solution, as you said, is a good idea.

 

WSM

Edited April 11, 2013 by WSM

[schroedinger]

If you got high PH add HCl

If you over acidified add Soda or Pottash

[ChloRure]

Thank you very much, I have about 2,5cm now in the bottom. How do you know when you need to stop ?

[WSM]

Thank you very much, I have about 2,5cm now in the bottom. How do you know when you need to stop ?

 

I stop a "batch system" when the current drops to about 50% of the highest level reached during the run (it's helpful to constantly monitor the amperage throughout the run). Longer than that gets into the "diminishing returns" area described by others, and wastes power plus stresses the electrodes unneccessarily.

 

WSM

[WSM]

Thank you very much, I have about 2,5cm now in the bottom. How do you know when you need to stop ?

 

If this is the first run, your yield will be low. There's a lot of dissolved chlorate plus precursors in the liquor. By recharging the used liquor with KCl (just let the crystals dissolve in the used liquor till it's saturated again, decant and run it again) your following yields will be much higher and will develop crystals of chlorate sooner.

 

Have fun.

 

WSM

Edited April 12, 2013 by WSM

[ChloRure]

I stoped the cell after 5 days running and got about 300grams. Pretty happy for a first run.

 

I let the cell cooling for about 2 hours and filtered with cofee filter. (I kept the liquor for future run)

 

The final product is mostly really white, but have some kind of sand grain and it still smell chlorine a bit. Can I use safetly the product? Should I put it back in fresh water or left liquor, boil it then filter again?

 

[WSM]

I stoped the cell after 5 days running and got about 300grams. Pretty happy for a first run.

I let the cell cooling for about 2 hours and filtered with cofee filter. (I kept the liquor for future run)

The final product is mostly really white, but have some kind of sand grain and it still smell chlorine a bit. Can I use safetly the product? Should I put it back in fresh water or left liquor, boil it then filter again?

 

One step others use during the filtering is to follow with chilled distilled water to rinse the liquor off the chlorate crystals. Next, recharge the depleted liquor & rinse water with KCl and run it again.

 

Be sure NOT to leave the electrodes in the liquor without power on. Soaking the electrodes in the liquor without power, damages them.

 

WSM

[THEONE]

Is there any way about to find the temperature when you know the amps and the volume of electrolyte? for example i have a Shell that is has got a 2LT of electrolyte... how much must be the amps to keep the solution at about, lets say, 60 oC

 

Also i read somewhere that you can make lead dioxide electrodes with battery graphite by electrolysis. You only need lead nitrate- acetate and copper nitrate- acetate and the acetate chemicals are easy to make 50% vinegar (CH3COOH), 50% hydrogen peroxide (H2O2). heat them up then add metal. Copper and lead both work....

 

Also one more idea.

What if you make some Mn metal by reacting mno2 (from batteries) - al (termite reaction) and after collect the Mn and add it to nitric acid to form manganese nitrate...?

Edited May 17, 2013 by THEONE

[WSM]

Is there any way about to find the temperature when you know the amps and the volume of electrolyte? for example i have a Shell that is has got a 2LT of electrolyte... how much must be the amps to keep the solution at about, lets say, 60 oC

Also i read somewhere that you can make lead dioxide electrodes with battery graphite by electrolysis. You only need lead nitrate- acetate and copper nitrate- acetate and the acetate chemicals are easy to make 50% vinegar (CH3COOH), 50% hydrogen peroxide (H2O2). heat them up then add metal. Copper and lead both work....

Also one more idea.

What if you make some Mn metal by reacting mno2 (from batteries) - al (termite reaction) and after collect the Mn and add it to nitric acid to form manganese nitrate...?

 

As for temperature monitoring, the simplest method is either using a compatible thermometer, or (if you like technology the way I do) a digital panel thermometer with a compatible sensor. Many such units are available from China for under $20 US, but most have sensors that aren't compatible with the cell's liquor. Sensors that are covered with Teflon are ideal, but pricey.

 

A low cost compromise I've found is PVDF (Kynar, or "poor man's teflon", as I call it) shrink tube. If you get a low cost digital panel thermometer with an unprotected sensor, the sensor can be toughened with a thin coating of PVDF this way and survive for a LONG time in the corrosive environment of the cell. With a little ingenuity, you can wrap the point where the sensor lead goes through the cell wall with some compatible material and seal that point through a Kynar compression fitting so no salt creep gets out.

 

I can't answer for the other questions, but others may offer suggestions. I have much more experience with the metering and power supply end of things, lately. A lot of research is going into better options for converting chlorate into perchlorate, but more time is needed to settle on a hobbiest-friendly solution with endurance.

 

Good luck.

 

WSM

[Peter8]

What do you thing from this PTFE (TEFLON) Pickling tank ? Only 10 dollars.

 

200mm x 120 mm 150 mm (7.87 inch x 7.72 inch x 5.9 inch)

 

http://i00.i.aliimg.com/photo/v3/657045986/Ptfe_pickling_tank.jpg

http://welldosource.en.alibaba.com/product/657045986-213571965/Ptfe_pickling_tank.html

 

http://welldosource.en.alibaba.com/productgrouplist-213571965-3/Ptfe_products.html?isGallery=Y

[WSM]

What do you thing from this PTFE (TEFLON) Pickling tank ? Only 10 dollars.

200mm x 120 mm 150 mm (7.87 inch x 7.72 inch x 5.9 inch

http://welldosource....kling_tank.html

http://welldosource....tml?isGallery=Y

 

Sounds excellent, but wait! Is shipping included?

If not, how much is it?

How many do you have to buy? One? Excellent!!!

 

I wonder how long it'll take for delivery?!

 

 

WSM

[WSM]

I was chatting by phone with pyrojig tonight when a stroke of inspiration came to me.

 

For the continuous system I've been referring to, I need to build a "heat well" in the crystallizer where the pump and float switches will live so they won't be fouled by crystals. It occured to me that I could use one of the PVC electrical boxes without the lid, instead of building a box from PVC sheet. All I'd have to do is put some holes in the sides for the depleted liquor to enter, plus populate it with the requisite articles. I may also remove the mounting tabs from the outside of the box since they're not neccessary in this application.

 

I think this will work out well! More later...

 

WSM

[WSM]

What do you thing from this PTFE (TEFLON) Pickling tank ? Only 10 dollars.

 

200mm x 120 mm 150 mm (7.87 inch x 7.72 inch x 5.9 inch)

 

http://i00.i.aliimg.com/photo/v3/657045986/Ptfe_pickling_tank.jpg

http://welldosource....kling_tank.html

 

http://welldosource....tml?isGallery=Y

 

Okay, I bit the hook and contacted the seller. Apparently the price is wrong. The quote I got for 4 units was $450 each (1800 total) plus $70 shipping.

 

That's too rich for my blood, so I'll pass. For that kind of money I could buy some amazing equipment on eBay and have funds left over.

 

Lesson for the day,... If it looks too good to be true, it probably is.

 

WSM

[taiwanluthiers]

Is there any mention for anodes for the production of perchlorate, or MMO pyrochlore/LD/etc.?

 

Seems the discussion is all centered around containers these days. Something more affordable than platinum would be nice.

[WSM]

Is there any mention for anodes for the production of perchlorate, or MMO pyrochlore/LD/etc.?

Seems the discussion is all centered around containers these days. Something more affordable than platinum would be nice.

 

Probably, but I haven't looked yet.

 

WSM

Edited June 4, 2013 by WSM

[WSM]

Probably, but I haven't looked yet.

 

WSM

 

Probably, but I haven't looked yet.

WSM

 

I'll look later and post the results here !

 

WSM

[taiwanluthiers]

I mean I am looking for someone who can make a LD anode for me, because I don't have the sophisticated lab equipment Swede has and so I don't think I'll be able to plate my own anode without a heap of money and lots of failure. There hasn't been any discussion on this recently and the discussions have been centering on container setup which I feel is not really that big of a concern compared to anode availability. I got a pile of chlorate and I don't know what to do with them because stars made with them burns too fast, and the safety problem isn't really helping either.

[WSM]

I mean I am looking for someone who can make a LD anode for me, because I don't have the sophisticated lab equipment Swede has and so I don't think I'll be able to plate my own anode without a heap of money and lots of failure. There hasn't been any discussion on this recently and the discussions have been centering on container setup which I feel is not really that big of a concern compared to anode availability. I got a pile of chlorate and I don't know what to do with them because stars made with them burns too fast, and the safety problem isn't really helping either.

 

I haven't tried to make an LD anode either, though frankly I'm better set to make an MMO anode than the LD anodes. The discussions vary as the needs/wants of the posters change. If you have a chlorate anode and your need is for a perchlorate anode, you're in good company. I have a couple platinum anodes I haven't tried yet and a couple LD anodes that haven't been tried because of damage on them that hasn't been repaired yet. The LD anodes are of Chinese origin but came damaged due to poor handling I think. I fear if they are put into service without repairing or sealing the damaged parts, the LD coating will be compromised and could separate from the titanium substrate.

 

Have you signed onto the Alibaba.com website and shopped for LD anodes? They're there, and ship worldwide. I don't know how trustworthy the listers there are. I was made aware of the Teflon tanks listed for $1-$10 and inquired about them, but found they're actually about $468 each! I was hesitant to buy at a fraction of that price, but If I had a serious need for them would shop domestically first (I'm in the USA).

 

We have some patent information claiming that a bismuth-ruthenium pyrochlore coated anode is capable of cleanly and (relatively) cheaply producing ozone as well as convert chlorates to perchlorates. These claims, as yet, are unsubstantiated and need to be proven by experimentation. If the claims are true and proven then we have a third viable option for home production of perchlorate; probably the best option yet.

 

Hope springs eternal. I hope its true and will pursue it as soon as I can get things ready for the effort.

 

WSM

[taiwanluthiers]

I never thought of Alibaba.com because they all have a minimum order of about 10 containers... I mean for that matter you could buy perc from alibaba.com but they have a minimum order of about 100 tons too.

[WSM]

I never thought of Alibaba.com because they all have a minimum order of about 10 containers... I mean for that matter you could buy perc from alibaba.com but they have a minimum order of about 100 tons too.

 

I think some of the LD anode suppliers have a minimum of either one or ten units. Patsroom purchased them from one of these sellers, I believe. Several of the LD anodes are roughly 10cm x 10cm (4" x 4") plus the lead strap. The main problem with the LD anodes is their fragile nature; they're electrically and chemically tough, but physically brittle in the LD coating (not at all like the MMO layers on titanium).

 

With the two I have I plan to spot weld a titanium tube to the strap so I can mount the anode in a modified PVDF compression fitting. I first have to repair damage to the LD in spots. I wouldn't want to see the LD flake off because the liquor was getting in between the LD and the substrate.

 

WSM

Edited June 7, 2013 by WSM

[taiwanluthiers]

So is there not something that can be done to address the fragile nature of the LD? Like maybe not plate it so thick for one thing, or just being more careful with it. How fragile is it? Is it like egg shells or even more fragile than that?

[WSM]

So is there not something that can be done to address the fragile nature of the LD? Like maybe not plate it so thick for one thing, or just being more careful with it. How fragile is it? Is it like egg shells or even more fragile than that?

 

I like the notion of plating the LD thinner on an MMO/titanium substrate. That would make the whole anode physically stronger I think. Being more careful with LD anodes goes without saying. The fragility of the LD coating might aptly be described as "like eggshells" but possibly more like a thin candy coating which can crack with rough handling.

 

I imagine the thicker the coating, the more prone to problems the LD layers may be. If the MMO coating is uncompromised, I believe the LD will adhere better and be less likely to chip or break away. At least that's my best guess considering I've never made an LD coated anode. I don't have enough lead salts around to even make an attempt at plating LD, but if I ever score a bunch I may try it one day.

 

WSM

[WSM]

I've noticed on several of my fabricated PVC tanks with flat lids (especially the larger ones), the lids tend to warp over time.

 

As I was waking this morning, it occurred to me that I could use tempered glass as a lid; thick enough for mechanical strength but thin enough to keep the weight down. For larger tanks, I could use several narrow sheets side by side with silicone seals between them.

 

These sheets of tempered glass would have the edges ground round by a professional shop for safety in handling.

 

These thoughts are still developing so any contributions are welcome...

 

WSM

Edited June 18, 2013 by WSM

[taiwanluthiers]

So as far as the LD chipping away, is it one of those things where as soon as there's any crack in the LD the whole anode is toast? As in the Ti cannot absolutely be exposed to the electrolytes?

 

Why not just make the coating only a few microns thick like the MMO coating, or at least a few mils thick? I think if the MMO were like 1 or 2 mm thick like the LD it would be fragile as well.

[WSM]

So as far as the LD chipping away, is it one of those things where as soon as there's any crack in the LD the whole anode is toast? As in the Ti cannot absolutely be exposed to the electrolytes?

Why not just make the coating only a few microns thick like the MMO coating, or at least a few mils thick? I think if the MMO were like 1 or 2 mm thick like the LD it would be fragile as well.

 

The problem with a crack in the LD (when it's running in the cell liquor) is the LD may begin separating from the titanium substrate causing a loss of electrical conductivity and the total effectiveness of the electrode suffers.

 

As long as the titanium is energized, the liquor has minimal effect on it.

 

I'm not making these LD electrodes (yet). If I do then I'll try the thin LD approach you suggest. I think it would be mechanically tougher, too, but may not be as hardy chemically or electrically. If I ever set up an LD plating rig, I may have to try it.

 

WSM

Edited June 21, 2013 by WSM