making potassium (per) chlorate

[WSM]

I often thought about PVC casings, but made my best out of an acryl food storage box (the round type, with airtight closing lid). It holds up perfect and not much Work. You just need to fit the Anodes, Exhaust and Maintenance port into the lid.

Once if used a Steel one and the used the steel as cathode, worked perfect until i dropped the PH a little low and the Steel corroded. Wasn`t a lot of fun

 

The acrylic food containers sound a lot like Swede's early work (see his blog). The steel cathode sounds more like older industrial systems. I think the careful control of pH plus a little dichromate helped them to survive.

 

PVC is able to handle the cell liquor without problems and is fairly inexpensive and readily available, too.

 

WSM

Edited March 17, 2013 by WSM

[WSM]

CP titanium tanks would be ideal... use it as container and cathode. But it will be expensive...

What about Acrylic and Polycarbonate? They're easy to obtain although a little expensive, and I can weld them together with solvents. I have never managed to find PVC sheets... I'd love to get large diameter PVC pipes anyways for making ball mill jars.

 

I've considered doing that. I have a piece of heavy wall CP titanium tube roughly 90mm OD and some CP titanium plate about 2.5mm thick. I was getting a welder at work prepped to TIG weld the plate to the tube when I transferred to a location closer to home. It may have made a very interesting cell, but putting it inside a larger PVC cell would probably work better.

 

Acrylic and polycarbonate polymers aren't well suited to handle concentrated, hot hypochlorites (etc.). I think they'd have a limited lifespan.

 

Even for ball mill barrels, you'll still need PVC sheet/plate for the ends (if you do it the way "old guy" does it). Keep looking; it must be available somewhere!

 

WSM

[THEONE]

Can we make lead-manganese dioxide from easy obtained material ? Like mno2 from batteries and just a lead metal were it can easily found it

After with a nitric acid form those 2 salts to use them for coating a titanium plate. I believe that it is not so simple, but where is the problem with these scenario ?

[schroedinger]

For lead nitrate there are to ways:

 

If you can get pure lead you mix it with HNO3

If you not sure if it`s pure:

 

Dissolve it in acetic acid. Add Soda to precipate ead carbonate. Whash this god and add HNO3 to form lead nitrate.

 

For MnO2 you can use the stuff from batteries, but need to purify it. Look up the NurdRage video on YouTube on that topic.

If you're going that route you will also need oxalic acid.

 

 

 

 

Yes the cell was quite similar to the one's made by swede. Probably not the right thing for a permanent used cell, but for testing perfekt, or if you don`t want big ammounts.

 

Yes Swedes work is gorgeus. I Specially like the way how he made the terminal he uses in his cell for holding the Anodes

[WSM]

Yes the cell was quite similar to the one's made by swede. Probably not the right thing for a permanent used cell, but for testing perfekt, or if you don`t want big ammounts.

Yes Swedes work is gorgeus. I Specially like the way how he made the terminal he uses in his cell for holding the Anodes

 

Which ones, the flat strap electrode leads or the filled tubular electrode leads?

 

I prefer the filled tubular leads since they can easily be sealed in a modified compression fitting and prevent salt creep which is so destructive to the electrical connections. For the past four years I've been seeking out and gathering various sizes of tubular CP titanium (on ebay) and have a nice collection started for electrode experiments. For systems using computer power supplies (which usually can output 30A) my favorite is 6mm OD by 4mm ID tubing.

 

After heating and pressing flat the electrode end, then spot welding the electrode on, I tap the other end of the tube with 10-32 threads, fill the tube with soft solder and chase the threads with the tap again. I connect the electrical ring terminal on 10 gage wire from the PS with a 10-32 round head, stainless steel machine screw and two stainless washers, and have a perfect connection (see photos in the bucket cell thread).

 

Flat straps are problematic to seal and often leak at the plastic to metal bond, in my experience.

 

WSM

Edited March 18, 2013 by WSM

[WSM]

For lead nitrate there are to ways:

If you can get pure lead you mix it with HNO3

If you not sure if it`s pure:

Dissolve it in acetic acid. Add Soda to precipate ead carbonate. Whash this god and add HNO3 to form lead nitrate.

For MnO2 you can use the stuff from batteries, but need to purify it. Look up the NurdRage video on YouTube on that topic.

If you're going that route you will also need oxalic acid.

 

schroedinger, I love that you add chemistry processes to the discussion, but I find it frustrating that there is no mention of other critical details needed to duplicate your work.

• what mass (or volume) and concentration of acids?
  
• what mass and expected yields from each reactant?
  
• what safety gear and lab equipment is required?
  
• recommended purication techniques?
  

Please, if possible add enough detail that others can follow (without presuming they must have prior knowledge of unspoken details). Some here may not have sufficient chemistry knowledge or lab experience to proceed safely without a FULL description. Let's help keep them safe as they learn. Thank you.

 

WSM

[schroedinger]

No worries, WSM i will do so. For the ways written on top, everyone should be able to do theyr one research or wait. I`m probably writing my tutorial on my method next month, as soon as eastern is over i will have time to do so.

 

Like both ways how he did the terminals.

 

WSM sounds like you have experience with welding the strip to the anode. As i couldn`t find much about this.

Maybe you can tell me what equipment i would need for this? Until now i`ve only used titanium bolts and nuts to fit them together, but these are quite expensive if using just grade 1&2 parts. So i really would like to change that.

[WSM]

No worries, WSM i will do so. For the ways written on top, everyone should be able to do theyr one research or wait. I`m probably writing my tutorial on my method next month, as soon as eastern is over i will have time to do so.

Like both ways how he did the terminals.

WSM sounds like you have experience with welding the strip to the anode. As i couldn`t find much about this.

Maybe you can tell me what equipment i would need for this? Until now i`ve only used titanium bolts and nuts to fit them together, but these are quite expensive if using just grade 1&2 parts. So i really would like to change that.

 

I use a spot welder purchased from Harbor Freight Tools here in the US. The spot welder is made in Armenia and imported by the tool company mentioned. It sells for what would be ~100 Euros, when on sale (about $150 USD). They come in either 120Vac or 240Vac models. I believe Swede shows a photo of his (which is the same as mine) somewhere in his blog (the commercial welder, not the home-made one) .

 

Spot welding works very well with titanium parts and I've learned I can weld some materials of different thicknesses together successfully, which worked out for surrounding the anode with two cathodes by using solid pillars, all of CP titanium (see the photos in the bucket cell thread).

 

When deforming the titanium tubing, be sure to heat it with a torch to at least red heat before forming. Don't try to do it all in one go, but stop when you feel resistance; re-heat it and go some more. If you go too far without heating, the titanium tends to crack or split on the edge of the pressed part.

 

Repeat till the forming is done, cool it in water, then buff the scale off before spot-welding titanium parts together. I recommend NOT removing MMO before welding (but hold your breath and work in a mild breeze to avoid breathing toxic fumes). Besides, MMO is more conductive than the titanium under it!

 

If you need greater details, ask specific questions and I'll do my best to answer.

 

WSM

Edited March 18, 2013 by WSM

[taiwanluthiers]

I used bent titanium nails to secure the strap, I have no spot welder... and there's no harbor freight type stores in Taiwan either.

 

Do not use Ti bolts, they are made from 6Al4V that will dissolve completely in the cell! Unfortunately no one makes bolts out of CP Titanium.

 

The making LD myself bit seems daunting because Swede looked like he had an impressive lab setup, he vacuums it, then cleans the heck out of it, then has spinning jigs and yet he still produced inferior ones for his first one, so unless I can buy enough extra equipments to have his impressive lab setup I don't think I have any chance of producing a halfway decent LD anode.

[schroedinger]

No worries about nuts and bolts, i`ve got acces to grade 2 stuff, not the Grade 5 Al stuff. But every set (1Bolt, 2 Washers, 2 Nuts) is about 7€. So not a lot of fun as you have to purchase at least 5 sets.

 

Ok, i will see what i can do about a spotwelder, maybe i will build the one like on kingsofrandom. Lucky me just got a new microwave last week and the old one is wayting to be harvested^^.

 

The main question about the welding is, can i just use a spot welder or do i need a special one with ti electrode and inert gas.

If i understood you right, this isn`t nessary, right?

 

I have to see, if i got to use the round shenk like svede, or just for the classic Ti strip, it`s depending on what supplies i can get.

 

If i can get the right Ti tube, it will be sealed, and filled with Al and etched in HCl prior to welding

[taiwanluthiers]

So why is Grade 2 more expensive than grade 5? markets?

[schroedinger]

Simply no real marked for that. Nearly nowhere grade 2 is really required and grade 5 is standard.

[frank]

Grade 2 bolts galore!

 

You can make nuts very easily if you purchase a tap (and a drill).

 

 

http://www.ebay.co.uk/itm/10-x-Hex-Socket-M6-16mm-Grade-TA2-Titanium-Screws-Bolts-/320737213674?pt=UK_BOI_Metalworking_Milling_Welding_Metalworking_Supplies_ET&hash=item4aad6d7cea

 

 

Grade TA2 is the same as grade 2.

http://www.aircraftmaterialsuk.com/data/titanium/ta2.html

 

Quite year auld excuses!!!!!!!!!!!!

[WSM]

No worries about nuts and bolts, i`ve got acces to grade 2 stuff, not the Grade 5 Al stuff. But every set (1Bolt, 2 Washers, 2 Nuts) is about 7€. So not a lot of fun as you have to purchase at least 5 sets.

Ok, i will see what i can do about a spotwelder, maybe i will build the one like on kingsofrandom. Lucky me just got a new microwave last week and the old one is wayting to be harvested^^.

The main question about the welding is, can i just use a spot welder or do i need a special one with ti electrode and inert gas.

If i understood you right, this isn`t nessary, right?

I have to see, if i got to use the round shenk like svede, or just for the classic Ti strip, it`s depending on what supplies i can get.

If i can get the right Ti tube, it will be sealed, and filled with Al and etched in HCl prior to welding

 

Just use the spot welder in air with no cover gas. The electrodes and tips are copper. The inexpensive commercial welders Swede and I use are without any special fixtures or accessories.

 

Simply clamp the pieces to be welded with sufficient (you learn by experience what "sufficient" is) force and depress the "on" lever. I generally run the welder till it starts to "growl" and the area immediately around the weld starts to glow; then release the "on" lever.

 

Practicing with scrap material is a good idea (it doesn't even have to be titanium,... luckily). The spot welders are a valuable tool to have on hand; if you can afford one, I recommend it.

 

WSM

[WSM]

If i can get the right Ti tube, it will be sealed, and filled with Al and etched in HCl prior to welding

 

Sealed is good, and etched after welding is a good suggestion (it would help remove any copper left from the spot welder tips); but filling with tin and/or lead is recommended (not aluminum, though). In fact, even putting a bare copper wire in the sealed tube before melting the solder in, is a good idea to add conductivity to the leads, plus they'll run cooler.

 

Let us know how you do it, and how it turns out.

 

WSM

Edited March 20, 2013 by WSM

[dangerousamateur]

I've got another question:

I'd like to use a typical glassbottle with a polypropylene screwcap.

 

To cope with the usual corrosion issues I'd like to make sure the the feedthrough openings in the cap for air exchange pipe/hose and electrodes are properly sealed.

 

I hope I can manage to spot weld my electrodes to pieces of titanium, so that i have two titanium strips leading through the cap.

When I assume the titanium to be proof of anything, anything else like the connection with my PSUs wires will be eaten up by the gas sooner or later.

 

How does one seal the feedthrough openings properly?

Since Epoxy is not the answer, is there anything else?

 

 

I read swedes blog and the idea with the titanium pipe, but thats out of my legue for now, I'm lacking the proper hardware.

Edited March 30, 2013 by dangerousamateur

[ChloRure]

Hi,

 

I want to start to do my own kclo3, because it is a pain to get where I live, and I like the idea to do it my self. I tried my first run this week but I think I did something wrong.

 

I used a hard solid plastic jar (One like northstar pyro is selling). I was able to put about 2 liters of liquid in it, and I left about 1 inch and half empty space on the top.

 

I don't want to do kclo3 ---> kclo4 for now, so I used KCL as starting materials (tried with the "no salt" you can buy at grocery store) On the package it said 0% sodium.

 

I was reading that people are using about 340grams of KCL per liter of distiled wated... So I boiled 2 liters of water and add about 650 grams of kcl... it was a lot of potassium, in fact, a lot has not been disolved and settle at the bottom. After boiling, I let it get a cooler temperature and started the electrolyse. (Titanium MMO Anode and Stainless Steel Cathode) venting with 1/2" hose.

 

Already on the start, about 1/4 of not disolved chloride was on the bottom, a strong chlorine odor, but anyway I left it running. 24 Hours later, I saw a lot of salt around the lid outside the cell and some on the casing. I think the solution boiled and tried to escape, cause about 1 inch was missing in the cell, the color was really yellow/gold and the chlorine smell was almost not there anymore.

 

But the jar was kind of deformed in the middle... kind of melt plastic but the temperature was ok on touch (I say about 40-50C and temp outside has been around 0-5C)

 

So, before doing something wrong I decided to stop it and wait for answer.

 

Did I used too much chloride ? 650grams is a lot for 2 liters no? Do I need to do something else after boiling the chloride in the water before using it as a solution ?

I was using a 5.2v 30amp computer psu, about 12 black wires and 8 red wires used.

 

Thanks

[schroedinger]

Propably quite easy answer. Your cell got tohot. aim for a max of 10 Amps per Litre. Really sounds like your cell just boiled away. Now the cell contains less liquer and the ressisitant raised, because there is less surface of the Anode in the liquer. Also maybe your anode got damaged, as most MMO`s are declared to a max of 80°C

[ChloRure]

The anode look like it was new on the parts that was not in the liquer, but for the part in the liquer it's not a little whiteish, even after rinsed it with cold water for 2 mins. If the anode is shot, can I still use it with low result or it just not work anymore ? As for the saturated solution, is it common to use that much chloride for liter ? (340g/l) or should I pass it in a coffee filter after boiled the solution ?

[pyrojig]

Your anode is probably fine. get some HCL and give it a bath. Let it soak for a few hours if it is really bad, then rinse with water and lightly scrub the anode with a sponge or towel. This is common to get a light white oxide layer on the electrodes, its usually residual chlorides.

 

I max out the chlorides in solution. It is a saturated liquor. If there is a small amount of undissolved salt no biggy. It will get consumed as the cell runs. The boil over is not a uncommon issue. The lid may be lacking a good seal, and or the cell was a tad hot. My HDPE 5gal buckets would run up to 50c and do just fine. I did get salt creep too, as you described.

Edited April 6, 2013 by pyrojig

[WSM]

The anode look like it was new on the parts that was not in the liquer, but for the part in the liquer it's not a little whiteish, even after rinsed it with cold water for 2 mins. If the anode is shot, can I still use it with low result or it just not work anymore ? As for the saturated solution, is it common to use that much chloride for liter ? (340g/l) or should I pass it in a coffee filter after boiled the solution ?

 

Another thought; what type of water did you use? If it was tap water, do they fluoridate the water where you live?

 

Unfortunately, even a little fluoride can permanately damage the MMO by attacking the titanium substrate.

 

If you use DI (or at least purified) water, I believe most problems (related to the water) will be solved. If your salt is contaminated with some additive; that might cause some issues also.

 

Hopefully, what you're seeing is something minor. If not, give us all the details you observe and maybe one of us can help you find a solution.

 

Good luck.

 

WSM

 

edit: The best practice I've seen used to make the salt solution is to dissolve as much as will go into the solution at room temperature. Moving the fluid will dissolve the salt up to seven times faster than still water will. I've successfully used a chemical handling pump to do this quite well.

 

Heat also works faster but can lead to a "super saturated" solution that will drop the salt out of solution quickly (as crystals) as the solution temperature returns to ambient.

Edited April 8, 2013 by WSM

[ChloRure]

Well I did some test this weekend, first the anode looked lime new after 5 min in the new run. So I guess it was chloride deposit. Also, I swaped this no salt substitute for a 20kg water softners potassium chloride... Damn those are hard to find now. I was able to disolve without any depot ... 680grams in 2 liters of deminalized water. I checked the temp after 5 hours and it was around 50C. Also, almost no more chlorine odor after 2 hours running. I wi let it run for maybe 4-5 days and see how much I get.

 

Thanks a lot, will give results when I will be Ble to harvest some stuff, But right now nothimg really precipate yet. ( about 8 hours running)

 

Oh and I have about 4 inchs space between 2 electrodes, maybe it's too much?

[pyrojig]

How big are the electrodes ?

4" was barely enough when I had oversized electrodes . The cell ran at 50c+ in the summer. I learned from WSM to match the electrodes to the PS (80%) of capacity. This will save you PS's ( I burned up a few) and overheating issues( + salt creep from boiling ) . It takes a couple days depending on the size of the cell to show results. Most of the major chem. reactions are taking place in the initial start up. After a couple weeks the cell( referring to a 5gal sys), hit what I call a sweet spot, where it maxed out its production abilities. The liqueur ph stabilizes somewhat and it kicks out some serious kclo3.

[ChloRure]

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 ?

[taiwanluthiers]

I think the Ph generally rises because the reaction creates hydroxide which raises Ph. You add HCl to lower them. If it's too low then let it run until it rises?