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Author: Subject: Chlorate Cell - MMO anode + titanium cathode (Swede)
Mickey8
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[*] posted on 23-5-2012 at 00:18
Chlorate Cell - MMO anode + titanium cathode (Swede)


Hi,

I want to make my own high quality potassium chlorate. So, I want to construct a chlorate cell.

I own the following items:

1.) Power Supply / Mean Well HRP-600-5 / 5.0V @ 120.00A = http://www.powergatellc.com/mean-well-hrp-600-5-power-supply...

2.) MMO anode + titanium cathode / 2.8" X 5" size / custom made from Kurt Bjorn



So I need to buy:
1.) 5 foot, 4 AWG copper wire welding cable (Color Black) = http://www.ebay.com/itm/4-Gauge-AWG-Welding-Cable-Rubber-Ins...

2.) 5 foot, 4 AWG copper wire welding cable (Color Red) = http://www.ebay.com/itm/4-Gauge-AWG-Welding-Cable-Rubber-Ins...

3.) 4 AWG Tinned Heavy Wall Lug 1/4 inch = http://www.ebay.com/itm/4-AWG-Tinned-Heavy-Wall-Lug-1-4-/300...

4.) 1/4 in Adhesive Lined Heat Shrink Tubing - $/ft Black = http://www.ebay.com/itm/1-4-Adhesive-Lined-Heat-Shrink-Tubin...

5.) Ampere Meter + Shunt / 100A , 50mV = http://www.ebay.com/itm/Green-0-100A-0-99-9A-DC-Digital-disp...

6.) Fuse holder for 4 gauge wire with 100 ampere fuse = http://www.ebay.com/itm/100-AMP-WATER-PROOF-FUSE-HOLDER-AGU-...

7.) Plastic container / Dimension: 6" x 6" x 10" = http://www.ebay.com/itm/Lock-and-Lock-Airtight-Food-containe...

8.) Potassium chloride

9.) Hydrochloric acid and a dropper

10.) Distilled water

11.) Epoxy glue to seal anode and cathode

12.) Venting the gases to the outside:
a.) Kynar Connector Tube And Hose Fitting 1/4" x 1/4" = http://www.usplastic.com/catalog/item.aspx?itemid=29358&...
b.) Black HDPE Adapters 1/4" x 1/4" = http://www.usplastic.com/catalog/item.aspx?itemid=29609&...
c.) 3/8" OD x 1/4" ID PTFE Tubing = http://www.usplastic.com/catalog/item.aspx?itemid=33596&...

Questions:
- What other items do I need to make a chlorate cell?

- The power supply have a small trimmer potentiometer that allows adjustment between a narrow range.
So, do I also need a voltmeter to set the output circuit to 5 volt? Here is one from the same vendor on ebay:
http://www.ebay.com/itm/3wire-DC0-100V-DC0-99-9V-Red-LED-dig...

Thanks,
Philipp


[Edited on 23-5-2012 by Mickey8]
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hissingnoise
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[*] posted on 23-5-2012 at 01:01


Quote:
What other items do I need to make a chlorate cell?

At a cursory glance, all you're missing is the NaCl!
The low solubility of KClO<sub>3</sub> makes KCl unsuitable as a starting material.
NaClO<sub>3</sub> is used to prepare other chlorates by metathesis . . .

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Swede
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[*] posted on 23-5-2012 at 06:19


I've been away from chemistry for a while... it's good to be back on Science Madness again.

ALL of the info you need (and more) is here on this site, along with many people who know the process thoroughly. The products (chlorate/perchlorate) are powerful oxidizers and can be dangerous, and the cell materials and the electrodes themselves must be carefully selected if you want them to last more than a run or two. The system evolves a number of harsh chlorine/hypochlorite species that can chew materials to rubble. Please do your homework!

Your power supply will make chlorates. IMO it is on the high end in terms of voltage. I'd trim it as low as it will go, probably down to 4.6V or so seems typical for the switching supplies of that type, and do a couple of test runs to determine what sort of electrode spacing will deliver a current compatible with your cables and electrodes.

At high currents, the electrode straps, especially the cathode, can become sizzling hot, with any water dripped on them boiling instantly. This heat can melt plastics and create problems in the liquor itself if not of an adequate volume. Search for a current that is compatible with your materials.

KNOWING the current, via the shunt and a VM, is nice, but not critical. One of the more interesting aspects of this process is calculating the efficiency of your cell, and efficiency will vary with pH and other factors. And to know efficiency, one must know how much current was delivered, amps / time.

Good luck with it, it's an interesting process.
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[*] posted on 23-5-2012 at 06:23



Quote:

At a cursory glance, all you're missing is the NaCl! The low solubility of KClO3 makes KCl unsuitable as a starting material. NaClO3 is used to prepare other chlorates by metathesis . . .


I don't disagree in theory, but for pyrotechnics, keeping all traces of sodium out of the system is important. I've been using KCl for several years now, and it works fine, with respectable yields. One added benefit is the potassium chlorate crystals form as a thick layer in the cell. These can be directly harvested, and the remaining liquor recharged with solid KCl for another run that is kick-started with pre-existing intermediates for the bulk process, away from the anode.
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[*] posted on 24-5-2012 at 14:51



Good to see you back Swede.
For those who do not simply LOVE Lead, perhaps the Pyrochlores would be a good avenue to explore for Perchlorate.

Dann2
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[*] posted on 28-5-2012 at 06:51


Pyrochlores " (Na,Ca)2Nb2O6(OH,F) is a solid solution between the niobium end member (pyrochlore), and the tantalum end member (microlite)."

Nothing like a simple, easy to make pyrochlore anode! :D

I keep thinking there is something we are missing with PbO2. There are many companies that make them, and obviously they have a way to prepare the substrate for plating so that the final product has mechanical and electrochemical integrity. We just need to kidnap a scientist and force him to reveal all his secrets! :P

Not to hijack this thread - I really should re-read our massive PbO2 anode thread - but the PbO2 anode I made a while back is still strong and looking good. I just haven't used it more than once, so I cannot verify that it has real longevity. I got "distracted" by life, so to say. The anode failed mechanically where the PbO2 was plated over shiny titanium. That portion of the coating on the MMO still looks great. I really need to fire up a small perchlorate cell and go for it.
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Mickey8
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[*] posted on 11-9-2013 at 03:27
Instructions for a chlorate cell: Do you have additions?


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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Antiswat
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[*] posted on 11-9-2013 at 09:12


i would say for an such amperage you might consider using wood, which should be very easy to shape etc.
a large glass jar with wooden lid pressed down (put some lead weights or whatever ontop) should do the job
with that much amperage, i just dont understand why you want a such small container? its gonna heat up more than just alot
also, KCl is used in electrolysis alot as you dont need to then spend KCl on crystallizing out the KClO3, and in hot solutions KCl can have a decent solubility, exceeding NaCl, meaning more KCl per mL, thus more effective
as the process goes on you should see KClO3 crystallize out, which is also a beatiful sight

for gasses you might want to consider leading the gas through a PVC hose (PVC is resistant to Cl2 AFAIK) and into some NaOH solution or similar, as this should produce quite the amount of Cl2, also H2 + Cl2 can and will if the UV is strong enough be initiated, and this burns faster than H2 + O2, and ofcourse louder and more destructive, not to mention the HCl formed, and obviously the electrolysis cell thats usually wrecked by the bang (:

if heat is a problem you could consider putting the cell in a bucket of water, if you want to descend it all you need to use diesel or similar, dont know how attractive the idea of using diesel is, however

also.. guys on the PbO2 anodes, why not try to do some reverse-engineering on them?? you can get something to find out how thick µm coating of paint theres on whatever, this should work for PbO2 aswell? problem is if we cant find out what the solution for electroplating PbO2 contains
think i have seen bismuth nitrate mentioned for this, and i have seen an dutch paint store selling bismuth nitrate in kg's




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 5-9-2016 at 13:17


Are there ways, other than spot welding, to attach the titanium straps to the mesh electrodes? I was considering using titanium nuts and bolts to make a secure connection between them. Thoughts?

Thanks!
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yobbo II
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[*] posted on 19-9-2016 at 01:52


You can bolt or rivet the strap to the anode. You need grade 1, 2, 3 or 4 Ti. Grade 5 will corrode.

A supplier of grade two is here

http://www.ebay.co.uk/sch/themetalsupplier5/m.html?item=2320...

http://www.ebay.co.uk/itm/2-pieces-M8x25-Titanium-Screws-But...



The is a discussion of chlorate cells here

http://www.amateurpyro.com/forums/forum/6-chemistry/

Yob

[Edited on 19-9-2016 by yobbo II]
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