making potassium (per) chlorate

[pdfbq]

I try to calculate the % of NaCl that has been converted to NaClO3 by measuring the density of the liquid.

Important is that the volume of the cell is always kept the same by adding water only.

 

I calculated that NaCl has a density of about 2,73 IN SOLUTION and NaClO3 about 2,55 IN SOLUTION.

 

Left the situation at start, right after 100% has been converted.

The weight increase of the entire cell is the weight of the NaClO3 minus the weight of the NaCl minus the weight of the mother liquor that has been replaced by the extra space NaClO3 uses (the pink part in the diagram).

 

I made an excel (OpenOffice) sheet that does the calculation and entered a saturated NaCl solution (from scratch) and my second run where I harvested NaClO3 and reused the liquid (the yellow fields require input).

 

Here is the data.

From scratch

Second run

 

The from scratch table seems quite OK because perchlorate started to develop at 1.33 BUT... I did not look at the temp too much...

One nasty point is that density changes quite a lot with temp. This makes it a bit harder to use.

 

Second run I am testing now.

 

Maybe this is a way to know where you are with your cell. Any comments are welcome.

Edited March 23, 2010 by pdfbq

[Bonny]

Looks like some good info pdfbq. Personally, I'm trying to keep my production along the KISS principle (Keep-It-Simple-Stupid). For chlorate, I simply run a "ballpark" amount of hours and shut down when the amps take a significant dive. In my case that's when I drop from >20 to <15. My MMO anode from Swede still looks brand new after several runs.

 

On another note, my perc harvest is well over 1kg. I'm not sure how much I have (scale only weighs 1kg max), but I will be doing a recrystallization before any further clean up anyway. I'm happy as I should be close to 2kg now of "dirty perc", and still have at least 10kg of chlorate feed stock left to convert. The only bad thing is that my Pt anode took a beating and won't likely last more than another run or 2. If that's the case I'll be retiring the cell until the fall/winter when I can afford another and have the time to get it running.

For now, as long as I can clean up what I have, I should be fine for this pyro season.

[TrueBluePyro]

Finally got my kclo3 cell up and running

 

Can't wait to recrystallise my first batch

 

 

[Bonny]

Finally got my kclo3 cell up and running

 

Can't wait to recrystallise my first batch

 

Looks good True Blue. How are the leads (wires) connected to the electrodes? You will want really solid connections or they will heat up like crazy running that power. Are you using a PC power supply? That's what I used and it worked great. I would watch the temp though if you are running 20A in a 1.75l cell. My cell was~18l and would get hot with 20-22A.

[bikemaster]

Truebluepyro, your connectrion are really bad....One red wire is not enough to drag 20 Amp in your cell. Now you are getting at max 6 Amp into your cell. The best way to get all the current that you can have is to use all red and all black wire. As bonny said, it you really can put 20 Amp in this cell, your cell will start to boil. A good idea will be to use all the black wires(-), and add just the right amount of red wires(+). By this way, you will be able to calibrate the better curent for the size of your cell.

[Arthur]

Lots of criticisms BUT you got it going so that's good.

 

Do the connections in really good thick wire. with good bolts etc. Keep track of the temperature 20a in a cell that size risks boiling it or melting the bucket. Cover the electronics so that fumes cannot get to the kit, vent the cell with a hose or a fan. the gas off can include hydrogen and or chlorine

[TrueBluePyro]

Thanks for all the 'criticisim' but its good, makes this project better.

 

Anyway, this size cell is very small and I wanted it like this for the first batch just to test it out. Yes the connections are really bad, but I will improve them later on when I get some parts. I'm a fair way from town and don't go in much so I use what I have.

 

When I feel that it is mostly working. I was thinking about putting it in a bath tub (outside)? is this a bad/good idea?

 

I'm really new to making kclo3 so I will take any advice.

[ausfire]

TBP,

 

I doubt you will have any need to cool the cell down given thats its probobly only pulling about 6 or 7 amps, however placing it in a another conatanier regardless of wether you decide to fill that with water to provide a bit of cooling is always a good idea as it will stop the electrolyte from being spilt all over the floor in the unlickely event that something does go catostrphicly wrong.

[TrueBluePyro]

When I say I'm thinking of putting in a bath tub I mean, putting the electrodes in the tub and the tub would be the cell. Is this a bad idea. How can I get the most kclo3 out of MMO anodes.

 

What would be the best size cell. 5L? 20L? What are the pros and cons of having a bigger or smaller cell?

[ausfire]

Simpily putting the elctrodes in a tub is probably not be the best idea, Ideally you want your cell to have some form of confinement such that the fumes can be safely vented. How much KClO3 your gonna get out of your anodes is going to be determined by how much current you push through them and the starting chloride concentration. Other factors such as efficiency are going to determine how long thats gonna take. Your anode should last years if you treat it right and keep the voltage down.

 

Really there is no best cell size, putting its Simpily smaller cells are gonna give you less chlorate, larger cells more chlorate however run times will be drastically increased in a larger cell if you maintain the same amount of current as you did in a smaller cell. For example running a 20L bucket cell at 5 amps is going to take *months* to complete but could yield approximately 10kgs of dry chlorate (assuming 50% efficiency and 350g/L chloride conc.), for a smaller cell the run time would be decreased proportionately. Something you may want to look into is a bucket cell.

 

Anyway Ive just purchased a new power supply and should have my cell up and running in the near future.

[Bonny]

When I say I'm thinking of putting in a bath tub I mean, putting the electrodes in the tub and the tub would be the cell. Is this a bad idea. How can I get the most kclo3 out of MMO anodes.

 

What would be the best size cell. 5L? 20L? What are the pros and cons of having a bigger or smaller cell?

 

If you are using a computer power supply, I think an 18l bucket is ideal, heats up, but not too badly.You should esily get several kgs after a few weeks of running. Take a look at some of my earlier posts in this thread for an idea on harvests.

If all you want/need is a little chlorate, then go with a small cell, but put the cell into a tub of water to help with cooling.

 

After you rewire the electrodes, (adding more wires to handle the current and improving the connections), I would move the electrodes closer. I used a PC power supply and spaced mine about 1" apart giving me 20-22A @ just under 5V.

Also, you could pick up a cheap automotive ammeter to monitor current.

[TrueBluePyro]

I have the changes the cell to a 10L bucket and improved the connections with the electrodes. I also moved the electrodes closer together, they are now about an inch apart.

 

I know I'm using about 5v but not sure what amps because the ammeter's we have are blown.

 

I haven't added anymore wires because I don't know how or what part to get them from on the pc powder supply.

 

Thanks for all the help.

 

http://i734.photobucket.com/albums/ww347/TrueBluePyro/PIC_0298.jpg

 

http://i734.photobucket.com/albums/ww347/TrueBluePyro/PIC_0299.jpg

 

http://i734.photobucket.com/albums/ww347/TrueBluePyro/PIC_0300.jpg

[mike_au]

I haven't added anymore wires because I don't know how or what part to get them from on the pc powder supply.

 

Assuming a cheap and/or old computer power supply, the colour of the wires is all that is important. All of the red wires will be 5v.

 

Just grab all of the red wires, cut them off as close to the case as possible and attach them to a thicker gauge wire (to reduce resistance) and run that to the cell, or if you are the adventurous type , open the case up (careful not to touch the caps, discharge them through a high value resistor before you start poking around), all of the red wires probably connect to one place on the PCB, unsolder them and solder a thick wire in their place.

 

Newer high wattage PSUs may have multiple output rails for each voltage, generally this will be advertised somewhere on the PSU. Don't just bundle the wires together if your PSU has multiple rails, if one is putting out 4.95V and one is 5.05V and you short them together the regulation circuitry might get a little confused.

[bikemaster]

Your setup is starting to look better (vent hole is a most). However, your connection are not ready for good chlorate production:P. This is not really hard to make it ready for good harvest. First take all the red (+) and the black(-) wire and cut the end of these wire (take the pin off). Denude all of thoses wire and twist all the red and all the black togetter. Connect all of those wires to the respective electrode. If you want to get you PSU away from the cell, you can use a good size of wire (at least 8 gauge) to make some good extension (welding wire are woking really good because they are big and flexible). For the connection itself, aligator clip work, but they are not really good. You should try to screw your wire to your electrodes (the hole is not there for nothing;)). If you want to see some idea of good connection, take a trip in the Swede's blog. You can find full of good information there.

If you want other idea, i can always send you a picture of my connection.

 

Good luck!

[Bonny]

As Mike and bikemaster said, your wires and connections need some improvement but your new cell is looking good. If you go back to page 24 in this thread, there is a pic of my bucket cell. Note the red bundle (+5) of wires and you can also see the black bundle(-) on the right. You will need a good bundle to handle the 20A your supply can pump out. I also saved the yellow bundle (+12) but have not used it.

Also as suggested, bolt the wires to the electrodes, the clips will result in poor connections dropping current and voltage, as well as heating up. They will also most likely corrode from the chlorine.

[TrueBluePyro]

Ok, thanks for all the advice, I will bolt the connections down once I find some scrap piece of wire I can use and bundle them all.

 

With my power suppler I can only find 5 red wires (+) and 11 black wires (-). Do I use all the black wires or do I only use 5.

[bikemaster]

All, that will reduce the resistance even more.

[Bonny]

Ok, thanks for all the advice, I will bolt the connections down once I find some scrap piece of wire I can use and bundle them all.

 

With my power suppler I can only find 5 red wires (+) and 11 black wires (-). Do I use all the black wires or do I only use 5.

 

If you only have 5 reds, then 5 blacks will be fine, but a few extra won't hurt. You don't really need any extra wire, if you have enough length to reach, just attach a connector to all the wires (stripped and twisted together). You can use a pc of old extension cord to extend if needed, just use all 3 wires.

 

A connector can be made from a pc of brass or copper pipe close to the size of the wire bundle. Make it about 1" long. Slide the wires in, crimp or hammer to hold them , then hammer the end flat, drill a hole and you're good to go. You can also heat the pipe and fill with solder if you want,.

[mike_au]

With my power suppler I can only find 5 red wires (+) and 11 black wires (-). Do I use all the black wires or do I only use 5.

 

Use all 11. Under normal conditions everything has some electrical resistance, putting multiple resistors in parallel reduces the overall resistance which allows more current to flow, admittedly not much more in this case but for the whole 30 seconds it will take to cut and strip a few extra wires you might as well do it.

[FrankRizzo]

I agree with Mike, use all the black wires bundled together. The system is only as good as it's weakest link, and you definitely don't want that to be the ground portion of the circuit.

 

Additionally, if you use a larger tub to keep the electrolyte bucket cool, you might as well take advantage of that heat input and use the same water you'd use for the cell, and add salt to it. You can then use the cooling water as electrolyte later, and the dissolving of the salt will remove more energy (heat) from the tank than just water alone.

[Bonny]

Additionally, if you use a larger tub to keep the electrolyte bucket cool, you might as well take advantage of that heat input and use the same water you'd use for the cell, and add salt to it. You can then use the cooling water as electrolyte later, and the dissolving of the salt will remove more energy (heat) from the tank than just water alone.

 

That's a great idea. makes your whole set up more efficient time and labour wise, as well as helping with the cooling!

[Swede]

Guys, don't forget eBay (for whatever country you are in) when it comes to power supplies. There are some amazing bargains in 5V supplies out there, many of them significantly cheaper than PC supplies, and no hassles with wiring. Many of them are adjustable over a small range, like 4V to 6V, making them even better.

 

Over many months if not years of looking for chlorate and perchlorate power supplies, I have come up with an eBay search string that knocks 20,000 returns down to a manageable number. Here it is.

 

power supply -ibm -antec -converter -atx12v -watts -intel -astec -hp -xm -apex -gateway -charger -usb -cord -adapter -dell -pc -atx -cpu -tattoo -compaq -toshiba

 

Now, you can REALLY narrow it down by adding the following, just after the words "power supply". Let's say you want a fixed 5V supply that can do 50 amps. The string becomes

 

power supply 5V 50A -ibm -antec (etc)

 

Change the amperage value to find bigger or smaller supplies. Keep the amperage at round numbers like 60A, 100A, etc. Or, you can play with a wattage, like 500W or 1000W, but amperage seems to work better.

 

You can find 5V supplies from 30A to 100A from $25 to $50. Here's a 100 amp monster for $50:

 

100 amp supply

 

I bring this up because for raw production, it is hard to beat one of these industrial units for longevity and overall effectiveness. Always look for a bit of overhead in your supply. An electrode set that is 3" X 6", and spaced about 3/4 inch, will draw 40 to 60 amps at a fixed 5V. Thus, look for a 75 to 100 amp supply so that the supply is loafing along at 50% rather than getting hot working at a full 100% Be sure the item is described as "working" or "functional" or "brand new" and that you can return it.

 

If you want to do chlorate AND perchlorate, or you like to calculate efficiencies or otherwise get technical with the process, it is best to get a variable supply. Now the prices can get nasty, but it is still possible to really score. Look for a variable supply of 0 to 10 or 12V, as big as you can afford, at least 50 amps for production, 60 to 100 is better. I found two, each can do 75A to 100A, both less than $100 each. Get a switching supply, they work fine. A linear will too, but shipping will kill because they are about 5X as heavy. Also, be sure you have household power available, either 115 or 230V. DO NOT get a unit described as "three phase." It won't work with household power.

 

Cables - for real production, the cables need to be #4 or #2 copper with heavy lugs that are bolted to the supply and electrodes. If too small, the cables will get VERY hot and you will lose voltage at the electrodes.

 

Sorry for the long post. I think it's great so many guys are doing this, and a good power supply is often the hardest item to locate and put to work. I hope this helps someone. PC supplies are great, but don't forget that there are "real" power supplies out there too!

[Ventsi]

I'm confused... Should I bunch up ALL the red(5V) wires coming out of the power supply or just the ones on the largest ..err plastic attachment?

 

This one:

[mike_au]

Should I bunch up ALL the red(5V) wires coming out of the power supply or just the ones on the largest ..err plastic attachment?

 

The largest plug is the motherboard plug, the other plugs will be mostly hard drive plugs with a couple of other little plugs depending on how old the PSU is and where it came from.

 

You might as well use all the +5v lines, motherboard, disk, whatever.

 

The green wire gets shorted to ground to turn the PSU on and the grey (I could have sworn it was orange) wire goes high to indicate that everything is working OK, so you probably want to keep those two and a ground wire separate. All the others are fair game.

[WSM]

Swede has been encouraging me to take photos of my project, so I can write about it as it develops. For lack of a better name, I'll call it, "The Monster". Like so many projects that start humbly and small, this one has grown almost out of proportion. To start, I've been studying the subject of electrochemistry for several years (literally) and made a few feeble attempts to make a chlorate cell a few years ago. My best efforts culminated in a one gallon pickle jar with a large PVC cap on it with holes drilled for electrodes and a gas vent (hydrogen mostly).

 

It worked, and worked well; but very slowly. It had all the best things I could muster, a glass container (how nice to see what's actually happening in there), a 3/4" tubular titanium cathode (courtesy of a kind friend) and a round rod MMO/titanium anode I purchased from a cathodic protection company. I used no pH control or other fancy gear, just a variable power supply I borrowed from a science teacher friend. It bubbled merrily away, making snowflakes of chlorate on the bottom of the jar and stinking of bleach while turning the potassium chloride water softener salt (bought from a big box home supply center) into potassium chlorate. Simplicity itself.

 

I was semi-content with this arrangement but wondered if I could scale it up? About January, 2008 on pyrobin, I saw a slideshow presentation of a tabletop continuous chlorate system assembled by Carl Tauch. It truly inspired me and I wanted to duplicate and improve on Carl's system (if I could). I communicated and collaborated with him and made slow, but steady progress. I did run into stumbling blocks but slowly got to where I nearly completed a similar system to Carl's.

 

While this was going on, I ran across some intriguing posts by a fellow who calls himself "tentacles" and who seems to be further along on the chlorate to perchlorate trail than I am, but how to contact him? In the meantime, I find the APC Forums (Oh Boy!, This looks good!) and sign up.

 

Over the past two years and lately reading (and rereading) Swede's blogs, I've developed an idea or concept of a larger, hobbyist's continuous chlorate system. Boy, it's amazing how complicated some simple concepts can get when you try to implement them! What started out as a pickle jar now is shaping up to need it's own, stand alone shed. Not wanting to settle for something that can crank out a pound of chlorate a day, I set my goal to a kilo of chlorate a day. The way the monster is shaping up, I'm afraid it will easily surpass even that!

 

In all my studies I settled on PVC for my main building material (compatible, available and relatively cheap). I would prefer CPVC which is compatible but much less available and definately not cheap! A plumber friend of mine donated a sizable piece of schedule 40, 12" pipe to the cause (we all could use more friends like that!), so I based my tank on a 20" tall piece of it.

 

At the level of the union, this tank holds about seven gallons. My original plan involved using an external electrode chamber and plumbing it into this tank for a reaction chamber. It occured to me that I might simplify things if I put the electrodes inside the reaction chamber.

 

I will continue the saga later....

Edited April 3, 2010 by WSM