making potassium (per) chlorate

[pyrojig]

Yes please do keep us in the loop with your new sys..! This is the path I eventually need to be on ( a continuous sys). The bucket systems are "cute" compared to the one WSM speaks of ....I can t wait to learn more about this.Its a brilliant concept ,making for 90%+ CE's when in action.

 

Today I built the circuit into a project box and (except for the terminations that need to be installed for connecting the leads from the three float switches) it's basically complete.

 

 

I put everything in a used PVC project box pictured above. The power cord is an old extension cord converted for the purpose of supplying power to the circuit. On the upper left hand side is the power switch for the whole thing and, going clockwise, the power outlet for the pump, the indicating light for when the outlet has power (and the pump is running) and lastly, the panel mounted circuit breaker I'm using to protect the pump circuit plugged into this box.

 

If I can find a program to help me draw a ladder diagram, I'll post the circuit so others can make one similar if they want to. I still need to build the heat well and populate it; then the experimental system will be fundamentally complete and ready to have it's trial run. I calculate it's total volume at about 8 gallons (about 30 liters)! And this is the small one!!! The Monster will dwarf it . Sheesh! I must be nuts.

 

WSM

[WSM]

Yes please do keep us in the loop with your new sys..! This is the path I eventually need to be on ( a continuous sys). The bucket systems are "cute" compared to the one WSM speaks of ....I can t wait to learn more about this.Its a brilliant concept ,making for 90%+ CE's when in action.

 

To get the most comprehensive view of what I'm trying to do, there are two sources. The first is from www.pyrobin.com and look up Carl Tauch's system (http://www.pyrobin.c...0production.pdf ). Carl's system inspired me in the first place and I went so far as to build a duplicate system but shelved it when I couldn't get a decent PVC to metal seal to prevent weeping seams. I just can't tolerate a leaky system (especially if I plan to let it run unattended most of the time). You should realize that the pyrobin source is an early version of Carl's work and is based on graphite anodes and stainless steel cathodes, as well as using dichromate to catalyze the reaction. He still uses dichromate but has upgraded his system to MMO and titanium electrodes, plus using a gravity fed crystalizer and pumping back to the "rundown tank", or what we call the RC (reaction chamber), rather than actively pumping the mother liquor to the crystallizer and gravity feeding back to the rundown tank as he shows in the photos.

 

The second source is here. The last 50 pages has the bulk of my work described. From about page 30 till here I have postings which include photos and diagrams of several concepts and pieces (as well as assemblies) which combined will outline my own view of a workable table top continuous system. There are several other notes such as personal communications with Carl and Swede that haven't been published, but may have been alluded to in my postings here. Swede encouraged me to start and do a blog of my work, but I've been hesitating to do so. Maybe I should. It could be a sort of lab book for me to reference from time to time, the way Swede's blog was to him. I'll have to consider that.

 

I suppose it's better to put in print and photos what I'm thinking, rather than trust a faulty memory with everything I keep stored in my head . My problem is I have a paper memory; if I write it, I stand a chance of remembering it... a downside of getting older .

 

WSM

[WSM]

I finished the fluid level controller assembly. The added terminal strip allows me to connect the three float switches to the circuits inside to switch on and off the power outlet to control the external pump used for feeding the salt solution to the RC. Now if only the weather and my schedule would cooperate, I could build the heat well and do a test run of the experimental system (a smaller continuous system designed to test various aspects of The Monster, an oversized continuous system I dreamed up a few years ago).

 

 

Like I said before, it's amazing how fast a simple idea can get complicated !

 

WSM

Edited October 6, 2011 by WSM

[oldmanbeefjerky]

I wonder, are there at all any actual benefits to using CP expanded titanium mesh, instead of a solid plate as a cathode?

In most homemade cells i see online, its always solid plate cathode, but in almost all comercial cells, like pool chlorinators, its always mesh.

A friend of mine wants to buy a Chlorate cell setup from me in 2 months for a large mount of money , which included a PSU power supply, a voltmeter and ammeter, Anode and 2 cathodes. However im stumped as to what kind of cathode to get him.

[pyrojig]

My 2 cents would be to stick with the Ti sheet if using 2 cathodes .. Ti mesh may create unwanted reactions and have too high of a surface area for your 1 anode. Now this may work if building a multi- anode setup , if the inner cathode was ti mesh surrounded by two anodes which where surrounded by Ti sheet cathodes outside the two anodes( 5 electrodes total). That would be a HOT sys. Edited October 6, 2011 by pyrojig

[patsroom]

My 2 cents would be to stick with the Ti sheet if using 2 cathodes .. Ti mesh may create unwanted reactions and have too high of a surface area for your 1 anode. Now this may work if building a multi- anode setup , if the inner cathode was ti mesh surrounded by two anodes which where surrounded by Ti sheet cathodes outside the two anodes( 5 electrodes total). That would be a HOT sys.

 

 

I beleive that whether or not that you are using Ti mesh or Ti sheet for the cathode that it would not have an ill effect on the anode. It just mean you increases the cathode working surface when using the Ti mesh by 2X. The only worry would be not too introduct to high of amperage to the anode. Doing so could be the problem that would destory an anode. This damage could also include warping of the anode,destruction of the anodes coating over heating of the cell ect..

Having a cathode on both sides of the anode would increase the working surface area of anode which may be of benfit to the anode.

Having more than on pair of anodes and electrodes in the same cell can reduce the work load of the anodes as well if wired in the proper sequence, by reducing the amp equally between both anodes.

The ideal of having 5 elecrodes total and increasing the amps to the proper level would produce a large yield very quickly in a good designed cell.

[patsroom]

OMBJ>

IIRC you have made some chlorates already. I feel that you know the basics of a chlorate cell now. I would say to use the best materials that you know. Ti mesh cathadodes are good Ti sheet is too. Do the best job you can do for the price he (your Friend) is paying. Be sure it is right and done right and you will be good to go. All of your questions you have can be found here in the forums and Swede's blog. I know that it is a lot of reading but it is all in here. Good Luck Pat

Edited October 6, 2011 by patsroom

[oldmanbeefjerky]

I see. you have all been very insightful , thank you.

I think i will give him sheet cathodes instead of mesh. I did some more reading, and have found that mesh cathodes, having such a high surface area, get corroded and become brittle over time, faster than sheet, because of the high surface area.

So i think ill hold onto my titanium mesh, and use it for making some cobalt manganese MMO anodes instead.

[WSM]

I finished the fluid level controller assembly. The added terminal strip allows me to connect the three float switches to the circuits inside to switch on and off the power outlet to control the external pump used for feeding the salt solution to the RC. Now if only the weather and my schedule would cooperate, I could build the heat well and do a test run of the experimental system (a smaller continuous system designed to test various aspects of The Monster, an oversized continuous system I dreamed up a few years ago).

Like I said before, it's amazing how fast a simple idea can get complicated !

WSM

 

I think I promised a diagram of the circuit I designed for the Fluid Level Controller:

 

 

It's based on two DPST relays which have a 12Vdc coil (R & S) and also a 12Vdc indicator lamp (L) which lights when the outlet is energized. I connected most of the components to terminal strips inside so replacement of defective parts would be easy. The DC transformer is a "wall wart" which converts 120Vac to 12Vdc for the control circuitry (which controls the 120Vac output to run a pump).

 

WSM

Edited October 12, 2011 by WSM

[WSM]

I think I promised a diagram of the circuit I designed for the Fluid Level Controller:

 

 

It's based on two DPST relays which have a 12Vdc coil (R & S) and also a 12Vdc indicator lamp (L) which lights when the outlet is energized. I connected most of the components to terminal strips inside so replacement of defective parts would be easy. The DC transformer is a "wall wart" which converts 120Vac to 12Vdc for the control circuitry (which controls the 120Vac output to run a pump).

WSM

 

The explanation of how the circuit works is this:

 

When the S1 power switch is turned on it powers the transformer to supply 12Vdc to the control circuit.

 

When the low water START float switch closes, it feeds power to the R coil which closes the R contacts.

 

R₁ seals the circuit closed and R₂ feeds power to the S coil which closes the S contacts.

 

S₁ feeds 120Vac to the power outlet that the pump is plugged into, allowing the pump to run.

 

S₂ feeds 12Vdc to the indicating lamp , L, that indicates when the 120Vac outlet is energized.

 

When either of the STOP float switches is opened (by the liquid level reaching the pre-determined top level), the R coil is de-energized and the R contacts open, de-energizing the S coil and the S contacts are de-energized, returning everything to the original state and ready for action again.

 

The circuit breaker is protection for the outlet circuit in case of an overload condition.

 

In reality, this is a very simple circuit, but it does the job .

 

WSM

[WSM]

I finished the fluid level controller assembly. The added terminal strip allows me to connect the three float switches to the circuits inside to switch on and off the power outlet to control the external pump used for feeding the salt solution to the RC. Now if only the weather and my schedule would cooperate, I could build the heat well and do a test run of the experimental system (a smaller continuous system designed to test various aspects of The Monster, an oversized continuous system I dreamed up a few years ago).

Like I said before, it's amazing how fast a simple idea can get complicated !

WSM

 

It looks like the heater for the heat well is coming together. I had problems with using aquarium heaters because of their size and control circuitry, but a friend suggested using a 10W resistor in a test tube for a heater. The heater is designed to run on 12Vdc and will utilize a 15 ohm, 10 watt ceramic resistor and I plan to fill the empty space in the test tube with silica sand. I need to seal everything in with silicone or Viton rubber to prevent corrosive liquids getting in and causing grief.

 

I'll put a prototype together and test it soon, and then report back.

 

WSM

[pyrojig]

Wow! Thanks for sharing such in depth information . It is nice to see a quality system come together ,... I believe Swede was right .. You should start a blog on your setup. I would love to see this. You take after him in your perfection aimed work. You both are machinists, and strive to build grand things.

 

Keep it coming ...

 

 

It looks like the heater for the heat well is coming together. I had problems with using aquarium heaters because of their size and control circuitry, but a friend suggested using a 10W resistor in a test tube for a heater. The heater is designed to run on 12Vdc and will utilize a 15 ohm, 10 watt ceramic resistor and I plan to fill the empty space in the test tube with silica sand. I need to seal everything in with silicone or Viton rubber to prevent corrosive liquids getting in and causing grief.

 

I'll put a prototype together and test it soon, and then report back.

 

WSM

[WSM]

Wow! Thanks for sharing such in depth information . It is nice to see a quality system come together ,... I believe Swede was right .. You should start a blog on your setup. I would love to see this. You take after him in your perfection aimed work. You both are machinists, and strive to build grand things.

Keep it coming ...

 

I hate to argue with you (especially when you're flattering me), but Swede is much more of a perfectionist than I am. I'm willing to say, "that's good enough!", where Swede's projects are a piece of art. Maybe it's because I've learned to know myself well enough to accept function over form, and use things that aren't beautiful (but work) rather than hold out for perfection and never get anything done.

 

Thanks for the vote of confidence. I'll have to look into doing a blog; I've never done one and am hesitant to start. Now for a name,... How about, "Fer Pete's sake, at least wear googles and ear plugs", or "I told you so...", or some other such clever thing? Any suggestions?

 

WSM

[dagabu]

I hate to argue with you (especially when you're flattering me), but Swede is much more of a perfectionist than I am. I'm willing to say, "that's good enough!", where Swede's projects are a piece of art. Maybe it's because I've learned to know myself well enough to accept function over form, and use things that aren't beautiful (but work) rather than hold out for perfection and never get anything done.

 

Thanks for the vote of confidence. I'll have to look into doing a blog; I've never done one and am hesitant to start. Now for a name,... How about, "Fer Pete's sake, at least wear googles and ear plugs", or "I told you so...", or some other such clever thing? Any suggestions?

 

WSM

 

"Oh, that's gonna leave a mark."

 

That's my suggestion.

 

-dag

[WSM]

"Oh, that's gonna leave a mark."

That's my suggestion.

-dag

 

And how do you prevent that mark? Depends!

 

WSM

[dangerousamateur]

Hi there,

 

making my own chlorate could be the only way to get some in the next years, so I'd like to get in touch with that subject.

Perchlorate is not necessary for me. KClO3 can be used for most stars and it's dangers can be coped IMHO. I even found chlorate flash less sensitive than Perchlorate with sulphur (and to my knowledge Shimizu 1 is a common mix).

 

(this tread is so long - please forgive me if my questions have been answered elsewhere)

 

 

1.)

Assuming i've got an average effecient cell - How much Kilowatt-hours will I have to spend per Kg Chlorate?

 

2.)

As far as I read thus far, the main challenge lies in the electrodes.

A combination of MMOanode and titanium cathode seems to work (Is there a better combination?)- only I haven't found a source for MMO sheets or mesh (thus far) in europe.

 

I've got an offer for Mischmetall that comes in little chunks. Will it be usefull somehow? Is there a known technique to use such raw material to coat something else, like graphite rods or some other metal?

 

3.)

What's the best alternative for MMO anodes?

 

4.)

I read somwhere that a small amount of Potassium dichromate helps - is it recommendable to use it?

Right now I might get some, but in future rather not - I'll have to stock NOW.

 

5.)

Are lead covered Graphite rods a viable alternative?

Same as dichromate with lead nitrate - right know I can get it, but chemical paranoya in Europe is rising - I'll have to stock some NOW.

[Arthur]

1/cells range from <30% to >95% chlorate conversion efficiency so it's hard to tell the cost of a future setup.

 

2/The electrode sets used by most seem to come from ebay seller "laser red" so keep looking but they certainly used to ship abroad (from USA)

 

You really do need to read the WHOLE of Swede's blog here he produced a huge and well presented body of knowledge with all the chemistry and calculations.

[oldmanbeefjerky]

heres what ive learned within the last 20 pages, mostly answered from swedes blogs

1. that question is unanswerable , we need to know how much chloride will be in the cell, and wheather or not you are using PH control. the best i can tell you is that it took me roughly 60-80 hours to make 400g of chlorate from 320g chloride, at an average of abount 14A, in a 2.6L cell., using no ph control.

A bigger cell with more chloride would work much faster, a large bucket cell ive heard here and there, can make about a quater-half a kilo per day running at about 30-45A

 

2.MMO is about the best, consiering potential value for money. at cheapest you will be paying about $20 for an anode if you buy online, and thats considering that I am the cheapest (on ebay anyway for an anode ready to use ,anyway). there are other people that sell anode sheet without connections, for about $20, which can potentially make about 250-1000g per day, but dont take my word on that. I cant really answer the other part of your question, sorry.

MMO anodes can be sent in regular letters, so you should widen your search to global, because shipping shouldnt be much of of a problem.

 

3. Platinum is a good substitute for MMO, but then again isnt. Another which works, OK is manganese dioxide and cobalt oxide, but its use is limited, though it isnt that hard to fix up if you have a bit of nitric acid and/or cobalt nitrate manganese nitrate / oxides, necessary to thicken it up.

Graphite can be used, but it is tricky. ive heard graphite can make chlorate rather efficiently, making about 80g of chlorate per 1g of graphite lost, and considering you can get sausage thick graphite rods about $7ea which are roughly 300-400mm thick at the right wholesalers, its an option, but not a very good one, considering MMO lasts much longer.

 

4. potassium dichromate helps protect any Iron in solution from eroding, and perhaps helps preserve MMO, but is more useful in continuous cells where the dichromate never really leaves the cell. I did a quick search and found dichromate is a tad expensive.

 

5. you mean lead dioxide, and they are generally used for making perchlorate, not chlorate, so yes, in that sense they are better, but for chlorate, they are not.

[dangerousamateur]

Hi,

 

thank you for your answers.

 

I would prefer use the KCl -> KClO3 Route.

Is there any reason one should go for NaClO3 first and than get KClO3 via metathesis?

 

 

And with these MMO mesh sheets, they seem to have been cut in shape, and often people cut them down further - how about the cutting edges? Aren't they going to be attacked? Do you protect them somehow?

 

 

Swede's blog

Wow - why haven't i found this source before. Thanks for the hint.

[WSM]

Hi,

thank you for your answers.

I would prefer use the KCl -> KClO3 Route.

Is there any reason one should go for NaClO3 first and than get KClO3 via metathesis?

And with these MMO mesh sheets, they seem to have been cut in shape, and often people cut them down further - how about the cutting edges? Aren't they going to be attacked? Do you protect them somehow?

Wow - why haven't i found this source before. Thanks for the hint.

 

If KClO₃ is your end goal, KCl is an excellent starting point. If KClO₄ is your end goal, NaCl -> NaClO₃ -> NaClO₄ -> KClO₄ is probably the best route, given the solubilities of the salts involved. Swede proved that KClO₃ can be driven to be KClO₄, but it's tough on the electrodes and the solubilities of the salts don't help.

 

The cut edges aren't a problem because titanium is a "valve metal" and is prone to quickly generate a protective oxide coat under favorable electrical conditions. Those of us who've run systems using the MMO mesh know how well it works, and when you set up a system, you'll see it and know for yourself. Laserred has MMO mesh on eBay right now and his prices are very low (considering what commercial companies sell it for).

 

You will learn a vast amount about the whole process by studying Swede's blogs in order. If parts don't seem clear, ask questions here; someone will answer them for you (sooner or later). Have fun with it. This is a great adventure (who knew science could be so much fun !).

 

WSM

[dangerousamateur]

Thank you.

 

Concerning those MMO anodes from ebay:

How long can I expect them to last, without PH regulation?

 

(I would start on small scale with some cheap graphite rods for "training" anyway )

[pdfbq]

1) My rule of thumb for non ph contolled non dichromate NaCl Cell:

You will get 5 grams for every amp over 5.2V per 24 hour.

So running at 25 amps will give you about 875 gram a week.

 

I do not use ph controll (too much hassle) I do not use dichromate (carcinogen I believe)

 

If you do not kill the anodes they will provide you with kilo's and kilo's.

Dont start with graphite, just buy the laserred ones. They are $10.50!

 

All playing with graphite is waist of time and money, trust me .

Edited October 16, 2011 by pdfbq

[WSM]

Thank you.

Concerning those MMO anodes from ebay:

How long can I expect them to last, without PH regulation?

(I would start on small scale with some cheap graphite rods for "training" anyway )

 

I would be surprised if they lasted less than several years. With only occasional use, I expect them to last five or ten years unless they get damaged from misuse.

 

To avoid misuse of your MMO electrodes;

Don't leave them in the cell solution without power

Don't let anything physically damage the MMO coating on the titanium substrate

Don't run the solution to completion (in a batch system, I tend to stop the run when the current levels drop to ~50% of the original level)

Avoid metal and other chemical contaminants in your cell solution

 

I'm sure there are other suggestions I'm overlooking at the moment, but you can see where I'm going with this. The MMO coating is very tough chemically but not physically; and it appears to very tough electrically, while in solution. Treated with care, it will last a very long time.

 

WSM

[WSM]

Thank you.

Concerning those MMO anodes from ebay:

How long can I expect them to last, without PH regulation?

(I would start on small scale with some cheap graphite rods for "training" anyway )

 

You may work with graphite if you wish, but once you try MMO on titanium, you'll wonder why you ever bothered with graphite. It's your choice...have fun .

 

pH regulation improves the cell's efficiency (how much energy is required to complete the desired reaction). It doesn't effect the MMO material per se.

 

WSM

[WSM]

1) My rule of thumb for non ph contolled non dichromate NaCl Cell:

You will get 5 grams for every amp over 5.2V per 24 hour.

So running at 25 amps will give you about 875 gram a week.

I do not use ph controll (too much hassle) I do not use dichromate (carcinogen I believe)

If you do not kill the anodes they will provide you with kilo's and kilo's.

Dont start with graphite, just buy the laserred ones. They are $10.50!

All playing with graphite is waist of time and money, trust me .

 

With a more efficient system and electrode spacing, plus in a larger volume cell; I believe the cell can produce over 500g a day; and more with pH control plus using less electrical energy in the process. I believe dichromate use will provide a marginal improvement in efficiency but I choose not to use it so I don't have to deal with the envionmental issues (and yes, it is a carcinogen and mutogenic compound, as well as having a caustic and corrosive effect on tissues; truly nasty stuff). If you don't have to use it, don't.

 

This is my opinion anyway.

 

WSM