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making potassium (per) chlorate


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Posted

Gotta love the math of this science stuff!!! It is the lube that keep these projects running . <_< . I would be the 1st to agree about sticking to the math on the electrodes. I can tell you from experience (bad) ,and burning up a couple Ps's do to way overloading them with excessively large electrodes .

Keep up the great work WSM!! We appreciate your dedication to this electo-chemistry !!! Swede will be thrilled to see you and others are keeping the tread alive. :D

 

Well, math IS the language of science. The gratifying thing about it is, the numbers do work (as proven by my experiment a couple Summers ago).

 

I've recently acquired some CP titanium tubing for filled electrode leads. I got 3/8" OD and some more 1/2" OD tubing. I sought these sizes because they work well with modified PVDF compression fittings, so salt creep is a thing of the past.

 

Anyone interested in custom made electrodes? I'll consult with the purchaser to iron out the details of their cell before having the electrode set made.

 

WSM B)

Posted
Yea, I'd be interested in some LD anodes for perchlorate making...
Posted

Yea, I'd be interested in some LD anodes for perchlorate making...

 

Sorry, I should have specified, CHLORATE anodes. I'm not set up to do other than MMO anodes and CP titanium cathodes,...yet.

 

Maybe some time in the future :whistle:.

 

WSM B)

Posted
Man perchlorate making is so hard, and rarely discussed... Chlorate is about as useful as dirt to me right now because of its various safety issue. But then having my house full of toxic soluble lead compound is more dangerous too...
Posted

Man perchlorate making is so hard, and rarely discussed... Chlorate is about as useful as dirt to me right now because of its various safety issue. But then having my house full of toxic soluble lead compound is more dangerous too...

 

Whoa now, don't be so hard on chlorates. Chlorates can be used relatively safely, just understand and respect their character, and you'll be okay.

 

For that matter, perchlorates aren't totally safe. Perchlorates can hurt you, too. If fact, I believe studies have shown that when perchlorates break down, each three perchlorate molecules will form four chlorate molecules (before giving up their oxygen atoms).

 

One should never be lulled into a false sense of security because they use perchlorates instead of chlorates. The use of chlorates doesn't automatically mean impending disaster, and the use of perchlorates doesn't automatically mean safety; everything is relative. Also, some of the best stars I've ever seen were chlorate stars (wonderful colors and large flame envelopes). Regarding these two oxidizers, I like them both and have used them both. They each have their (well earned) place.

 

WSM B)

Posted (edited)

Man perchlorate making is so hard, and rarely discussed... Chlorate is about as useful as dirt to me right now because of its various safety issue. But then having my house full of toxic soluble lead compound is more dangerous too...

 

If it were easy, everyone would be doing it ;). I believe perchlorate production would be easier if we had free access to the materials to do it. Lacking those materials adds a certain degree of difficulty, but if we're prepared, we can do anything.

 

Don't give up, just be ready to act when the opportunities present themselves.

 

WSM B)

Edited by WSM
Posted

I couldn't find too many decent chlorate formula because people think that chlorate is liable to catch on fire by itself... and it does scare me a bit... especially when every other composition contains sulfur and I don't have space for a separate process building. Especially when I hear stories of people igniting stars simply because they stepped on it.

 

Most perchlorate formula doesn't work with chlorate as oxidizer... oxygen balance is all wrong and when I tried, the star doesn't burn with the right color and it leaves a lot of residue. The other problem is most chlorate formula burns way too fast to be useful in anything but roman candles (Lancaster Red #1 is an example) but perc formula such as Buell Red, Conkling Blue, etc. burns at the right speed for shells. Are there any good chlorate formula that burns at the right speed and has the brightness of a metal fueled star? Some of them are too dark.

Posted
You're clearly not looking in the right spots. There are plenty of great chlorate formulas around. Might I suggest investing in some legitimate literature? Looking around for some of Mike Swisher's posts on rec.pyro or passfire will also likely yield plenty of good chlorate based formulas.
Posted
Passfire is where I looked, but without any instructions on them, I don't know which one is good. Can you give a good example of a great chlorate formula?
Posted (edited)

I second that on chlorates. They have wonderful and well earned place in pyro.

 

(taiwanluthiers) I know you probably arent bashing chlorates as a usefull oxidizer , but one more as a bit more care is needed to handle ,and may not be of interest to you at the moment.

 

I too have used both, and find I favor chlorates for star mix's due to the ease of ignition , clean color, and that awesome large flame . !! Perch is as said safer depending on the comps and how it is handled. Once in a star (bound) the dangers are greatly reduced .

Blesser has comps , and shimizu as well

Edited by pyrojig
Posted (edited)

I second that on chlorates.

Blesser has comps , and shimizu as well

 

Weingart and Davis do as well. Another excellent source is Joel Baechle's "Pyrocolor Harmony, A Designers Guide" (self published), if you can find one. Joel has worked in the pyrotechnics industry since his youth, and is an excellent researcher and designer.

 

WSM B)

 

Edit: I'm told Bill Ofca's "Technique in Fire" series has a good section on chlorate stars. In fact, most pre-WWII pyro literature has a treasure of chlorate star formulas.

Edited by WSM
Posted (edited)

When I started my smaller "experimental system", the external electrode chamber (EC) was supposed to be schedule 80, 6" CPVC.

 

When the material arrived something wasn't right. I discovered that my treasure was PVC and not the CPVC that was advertised. When I notified the eBay seller of the error, he discovered all of his 6" material was PVC so he promptly refunded my payment. He let me keep the heavy wall pipe rather than ship it back so I used a piece for the EC of the "experimental system".

 

Fast forward to July, 2013. An eBay seller in New England is selling 23.5" - 23.75" pieces of schedule 80, 8" CPVC. The problem is they listed it as local pick up rather than offering shipping. I contacted them and asked about shipping to the West coast and they said yes. I ordered two pieces and had them ship them by FedEx Ground service.

 

post-9734-0-11933100-1375492990_thumb.jpg

 

These pieces are heavy (about 21 lbs or nearly 10 kilos each) and expensive to ship, but a fraction of the full price for CPVC (which is about five times what PVC would be). Years ago, I purchased a piece of 1/2" thick CPVC sheet to use for making a high temperature reaction chamber (RC), so I plan to cut a piece of it to use for the base of the chamber, using the new CPVC pipe pieces. I think plain old PVC sheet would work for the lid of the cell.

 

This is for a continuous system since it's so heavy, rather than for a batch system. Tipping this beast to remove the crystals and liquor would be a chore. The wall thickness of the pipe is between 1/2"- 9/16" (about13-14mm). The material can handle up to 200ºF (93ºC) without undue stress so it should make an excellent cell.

 

WSM B)

Edited by WSM
Posted

I cut a piece of 1/2" thick CPVC sheet (that I bought on eBay a few years ago) for a base on the beefy CPVC tube section. The tube section is 23.75" tall, 7.5" ID and 8.625"OD. The base piece is roughly 8.75" square.

 

post-9734-0-83469300-1375582765_thumb.jpg

 

As seen in the photo, this is new material left over from a project and not some old remnant from a junk yard. They cut the piece with a band saw so cleanly that little is required to get a good seal with the CPVC cement to the base plate. I ordered a quart of industrial grade CPVC cement from US Plastics to put my tank together with, and hope it gets here before I leave for Pennsylvania next week.

 

As I mentioned before, I think 1/2" thick PVC sheet should make an adequate lid for this tank (we'll see).

 

I'll add more as I make progress on this system.

 

WSM B)

Posted

Wow that is coming together nicely !!

 

If you design your electrodes like the one in the BCA as a joined pair (with kynar tube woven into the mesh as a standoff) it would serve you well, surviving a lid failure if that where to happen.This hopefully would reduce the chance of a short to your PS. I m sure that your using some beefy pvc plate , so this should not be a big deal , unless your hitting the cell with 150-200A then some heat sink or active cooling may be in need .

Posted (edited)

Wow that is coming together nicely !!

If you design your electrodes like the one in the BCA as a joined pair (with kynar tube woven into the mesh as a standoff) it would serve you well, surviving a lid failure if that where to happen.This hopefully would reduce the chance of a short to your PS. I m sure that your using some beefy pvc plate , so this should not be a big deal , unless your hitting the cell with 150-200A then some heat sink or active cooling may be in need .

 

Thanks pyrojig, I have to wait for the cement before I can put them together but it's ready to go. I haven't decided what configuration of electrodes to use yet but it will probably depend on which power supply I use. I do know I plan to make them tall and narrow to take advantage of the added circulation due to "hydrogen lift" as well as the thermal effects.

 

I think a double cathode, surrounding the anode would make for a highly efficient cell, especially if pH control is used. Your idea of maintaining the electrode gaps with Viton tubing (I knew what you meant) to prevent short circuiting the power supply is a good suggestion. I'm not worried about the PVC lid breaking down. I think it'll work out just fine.

 

As far as the temperature the cell runs at, I'm using a thermal sensor with a digital panel meter so I can monitor the temperature of the liquor in the cell while it's running.

 

I plan to keep track of the temperature in the crystallizer chamber (CC) fluids also so I can check the difference between them while the system is operating. The CC temperature will help me determine how much dissolved chlorate is in the depleted liquor (necessary for calculating the accurate CE of the cell).

 

WSM B)

Edited by WSM
Posted (edited)

For those interested in making chlorates, laserred has more sizes of MMO on titanium mesh anode material listed on eBay than I've seen in quite a while.

 

This is surplus material and works well. His prices have gone up but are still a bargain compared to new anode material from manufacturers.

 

You still need to make cathodes, attach leads and build a cell, but this will get you closer to being self-sufficient for chlorates.

 

WSM B)

Edited by WSM
  • 2 weeks later...
Posted

I received the CPVC cement on Friday before I left for the PGI convention, so I stowed it till I got back (yesterday).

 

This morning I cleaned the end of the CPVC pipe section and glued it to the CPVC base I prepared. I dobbed a heavy coat of the cement (several times) on the end of the pipe, giving it time to soften the pipe and base. I then mashed the pipe and base together and twisted the pipe to get a better seal on the base and put a car battery on top of the pipe to keep pressure on the glue joint. As seen in the photo, everything is going well.

 

post-9734-0-42287000-1376964173_thumb.jpg

 

I'll add more as I make progress ...

 

WSM B)

Posted (edited)

Yesterday I took a piece of half inch thick clear PVC sheet and cut an oversized lid for the CPVC tank.

 

I still need to cut and modify a thin ring of PVC pipe and glue it to the lid for a support for the tubular seal made of either silicone or Viton tubing. If the fit is close enough, it should make a decent seal and keep things tight.

 

I'll try to photograph the steps I take so it'll be clear to others what I'm doing.

 

More later...

 

 

WSM B)

Edited by WSM
  • 2 weeks later...
Posted
Your getting me excited to move toward s a cont. sys . I just fear that I will end up with a stash of kclo3 more than I can manage . May have to start a pyro store lol. :) I like the simplicity of the smaller reaction chamber and the thought of downsizing from the 5gal sys seems more appropriate if grearing up for a cont. sys . I will be interested to see the results and research on the pyrochlore. If there is anything that I can contribute to the research ( materials and or time / kelm , etc ) let me know.
Posted (edited)

Your getting me excited to move toward s a cont. sys . I just fear that I will end up with a stash of kclo3 more than I can manage . May have to start a pyro store lol. :) I like the simplicity of the smaller reaction chamber and the thought of downsizing from the 5gal sys seems more appropriate if grearing up for a cont. sys . I will be interested to see the results and research on the pyrochlore. If there is anything that I can contribute to the research ( materials and or time / kelm , etc ) let me know.

 

A continuous system is a lot more work, but a fun challenge. Once it's dialed in, it'll just keep running and the salt will pile up. You could use the surplus for trading stock if you want to.

 

Thanks for the offer, I may take you up on it.

 

WSM B)

Edited by WSM
Posted
How can i extract the naclo3 from the electrolyte without any nacl ?
Posted
You keep adding NaCl and keep running the cell until the sodium chlorate drops out of the solution... however I read that sodium chlorate has a solubility of something like 2000+ grams per liter... so keep at it.
Posted

You keep adding NaCl and keep running the cell until the sodium chlorate drops out of the solution... however I read that sodium chlorate has a solubility of something like 2000+ grams per liter... so keep at it.

 

Yes but the solubility of naclo3 is better than nacl

Posted (edited)

Hi, this is my first post :)

 

This anode, Work?

 

http://www.amazon.co... titanium anode

 

Best regards,

 

 

Marcelo.-

Edited by pyroChile
Posted

Hello,

 

Are this informations correct or do you have additions?

 

This is a simple operating instruction.

 

WARNINGS:

---------

Avoid using tap water, especially if your water is fluoridated, but use either distilled or purified water to make your electrolyte. Fluorine will eat the titanium and kill your electrodes.

 

The electrolysis process produces a large quantity of chlorine and hydrogen gasses. The toxic chlorine gas is liberated vigorously from the anode and explosive hydrogen pours off the cathode continuously as the current flows, as micro bubbles.

 

For all of you doing electrolysis, please protect the electronics! One good mist spray from the cell will start to wreck the electronics.

 

The hottest point on a chlorate cell is usually one of the electrode straps close to where the PS cable is connected, and these straps can easily exceed 100 degrees °Celsius with little warning. A 25mm x 1.5mm sheet Titanium strap will handle about 40 amps with no additional cooling. At a sustained 40 to 50 amps, the strap will probably become greater than 100 degrees °Celsius, and water will flash to a boil when applied to the strap. So, most home systems of 5 to 10 liters, unless cooled in some manner, will typically reach a practical limit between 40 to 50 amps.

 

A word of caution: if the power goes off or is turned off, remove the electrodes from the electrolyte (to protect them from being damaged by the electrolyte while unpowered). I usually rinse them and store them dry till I set up the cell to run again.

 

INFORMATIONS:

-------------

313 grams KCL per liter distilled water at 10 degrees °Celsius. To dissolve the KCL in the distilled water I use a 5 liter cooking pot with teflon coating. A hot KCL solution will corrode stainless steel pots.

 

Why bother with pH control? The answer is simple – you don’t have to, but if you don’t address pH, the best efficiency you can expect will be 66%, and more realistically, it will be closer to 50%. So, you don't really need to controll the ph.

 

Features of my power supply:

- 5 Volts DC and 120 Amps max Current. So a max power of 600 Watts = 5 Volts x 120 Amps.

- Protections: Short circuit/Over load/Over voltage/Over temperature

- Built-in cooling fan speed control + Built-in constant current limiting circuit + Built-in fan On-Off control

 

Sample the spacing needed to get about 40 to 60 amps (Closer = higher current). It will probably be about 15mm. So the wattage of power supply will be less than 50% of the rated 120 amps, meaning the supply will not struggle. If your power supply is rated for 50 amperes, and you run it for a month at its maximum rating of 50 amperes, you can expect a very hot supply, potential over-temperature faults, and a greater likelihood of failure, when compared to a 100 amp supply loafing along at 50 amps.

 

Thanks,

Philipp

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