making potassium (per) chlorate

[WSM]

Excellent! As you gain experience, it won't seem like so much effort, and the yields will increase dramatically.

Don't skimp on the wash. And of course, you can recharge the old electrolyte over KCl, and it'll give you a HUGE head start on subsequent runs because the liquor is pre-saturated with chlorate and precursors.

 

Swede is right. Isn't this fun?

 

Do you think you'll scale up or just keep running it the way it is?

 

WSM

Edited December 7, 2012 by WSM

[taiwanluthiers]

I am not sure about scaling up... I don't think I need 10 pounds of chlorate per week as it would be asking for trouble... but how do I recrystalize KCl crystals? I normally dissolve them and filter the red stuff out. Recrystalization would work if KCl dissolves 2 grams per 100mL but its ten times that... I can add the aqueous KCl to the cell but that would not help much... Boiling the liquid off would require too much energy.

 

Why do they have the red stuff in the agricultural KCl, is it to prevent people from using it to make chlorate?

[WSM]

I am not sure about scaling up... I don't think I need 10 pounds of chlorate per week as it would be asking for trouble... but how do I recrystalize KCl crystals? I normally dissolve them and filter the red stuff out. Recrystalization would work if KCl dissolves 2 grams per 100mL but its ten times that... I can add the aqueous KCl to the cell but that would not help much... Boiling the liquid off would require too much energy.

Why do they have the red stuff in the agricultural KCl, is it to prevent people from using it to make chlorate?

 

When you dissolve the agricultural KCl and filter it, does it come out clear or is it still cloudy? If it comes out clear, just use the solution as is. If it's still contaminated, crystallizing the KCl out of solution and giving it an ice water rinse may remove most (if not all) of the impurities.

 

I suppose they add the red color so they can tell which part of the field they've already covered with it. They do the same thing with other agricultural products.

 

WSM

[taiwanluthiers]

the filter comes out clear, a little bit of the red stuff makes it through to give the solution a pinkish color. I have used coffee filter and I am beginning to think that it's not the best tool for this. I will check the lab supplier to see if they have buchner funnel and lab filters.

[pdfbq]

Just use two or three coffee filters or, make a saturated solution and let it stan for 24 hours. Maybe the red stuff sinks to the bottom.

[WSM]

the filter comes out clear, a little bit of the red stuff makes it through to give the solution a pinkish color. I have used coffee filter and I am beginning to think that it's not the best tool for this. I will check the lab supplier to see if they have buchner funnel and lab filters.

 

I've never been a fan of using coffee filters because of their low quality (too much of the wrong stuff gets through and not enough of the right stuff stays). I've been using Buchner funnels and lab grade filter papers for over twenty five years, and I'm not inclined to "go cheap" on such a vital step after all the good work I've put in at this point!

 

Do you have a decent source of vacuum for the funnel? My experience has shown that most of the time, less vacuum but higher flow rates seems to work the best. A fast paper for chlorates sounds like a good idea, too. Let us know how you handle this step.

 

WSM

[taiwanluthiers]

I will have to check around, I am sure I can get good filter papers and buchner's funnel, just not sure at what cost. I don't have much of a vacuum source... can try using the shop vac.

[WSM]

I will have to check around, I am sure I can get good filter papers and buchner's funnel, just not sure at what cost. I don't have much of a vacuum source... can try using the shop vac.

 

Another option would be a water aspirator. It's a low cost source of vacuum that opetates by running water through it, and the vacuum is formed at a side port (usually in the form of a hose barb). Check wikipedia under "aspirator" and other associated listings.

 

I believe one could be made with brass plumbing fittings if you have basic machining skills and tools.

 

WSM

Edited December 14, 2012 by WSM

[taiwanluthiers]

Well, I found a ceramic buchner's funnel. The lab filter paper was an order of magnitude more expensive than coffee filter, and I don't know how they're better than coffee filter...

 

I remember in high school when we used buchner's funnel we would hook a hose to a side port at the water, and turn on the water to generate a vacuum.

[WSM]

I remember in high school when we used buchner's funnel we would hook a hose to a side port at the water, and turn on the water to generate a vacuum.

 

Yes, that's the water aspirator I was describing. They work reasonably well.

 

WSM

Edited December 14, 2012 by WSM

[taiwanluthiers]

Ok this thread has been dead for a while, but I have a question about actually making perchlorate (as if chlorate used in pyro doesn't make me edge enough):

 

I have been reading some stuff about producing lead dioxide anode for perchlorate production, but the reading is long and it seems to require equipments and chemicals that are expensive. Since no one seems to sell LD anodes that work, would it be better if I simply bought Platinized titanium anode (used for plating) on ebay? How long can such an anode last? I've read even when properly used Platinum anode still erodes. A 2" x 3" is being offered for 35 dollars, how much perchlorate can I make with them? Someone seems to have said something along the line of only 10kg, and then the anode is toast.

[pdfbq]

Just try it.

It depends on how thick (how much) platina there is on the anode how much you can make.

I think 2" x 3" for $35 is not much Pt but you'll definitely make perc with it.

 

I bought a Pt anode for $100 2" x 6" and its stil not dead after 10 kg of NaClO4. It's not 'fresh' either.

 

As I said, contribute by trying. This is a forum, not a tutorial.

Edited January 5, 2013 by pdfbq

[pyrojig]

I found some interesting literature From Dr Shimizu, Which he claims Kclo4 can not be derived from Kclo3 alone, but rather NaClo3. I thought this to be odd, and was sure that Swede had already made Kclo4 directly from Kclo3 .

 

 

 

Here is a direct Quote from F.A.S.T. :

 

 

Manufacture. At first sodium chlorate is prepared by the electrolysis

of industrial salt or the milk of lime process described in (2). The sodium

chlorate is further electrolyzed to produce sodium perchlorate, and when

potassium chloride is added to cause double decomposition, crude potassium

perchlorate is obtained. This is recrystallized and crushed to powder. It

is impossible to obtain potassium perchlorate by the direct electrolysis

of potassium chlorate, because of the low solubility of potassium

perchlorate in water.

The electrolysis of sodium chlorate is an oxidizing reaction:

NaClO3 + H2O --> NaClO4 + H2

94

For the industrial process a platinum anode and steel plate cathode are

used, and a small amount of potassium bichromate is added to the electrolyte,

The electric current efficiency is good when the concentration of the

sodium chlorate is high, but it suddenly decreases as the concentration

falls. The double decomposition which produces potassium perchlorate

is as follows:

NaClO4 + KCl --> KClO4 + NaCl

Edited January 6, 2013 by pyrojig

[taiwanluthiers]

I found potassium chlorate has a fairly good solubility at higher temperature (higher than 50 degrees, which is fairly possible for a cell of average size), and in fact at 100 degrees they have the same solubility as potassium chloride (according to the solubility chart). So if you kept the cell large, and the temp. high I don't see how its hard to make potassium perchlorate from its chlorate. I would rather go that route simply for the fact that its far easier to extract relatively pure potassium chlorate than sodium chlorate.

 

Looking at the price of Platinum anode, I do not know if it is even worth at all, when its rate of erosion is still pretty high for the price of the material (I thought I saw figure of around 1 or 2 grams per ton, which translate to about 1 or 2 milligrams per kg, and that's a lot considering how little Platinum is contained in those plated anode). For the price of the 35 dollar anode plus shipping I could buy about 2 kg of pure perchlorate, so I am not sure how economical it is to produce percs myself. Chlorate is really easy and cheap to make in comparison.

[pyrojig]

I think at the moment , people can obtain perch from suppliers cheaper than it can be made for ( once you include the materials and electricity involved). I guess manufacturing it would make sense if the price was ridiculous, or unobtainable. Now if we can only keep the startup cost low, and the anodes cheap, and provide premium cell conditions , it may prove to be cheaper. This is assuming that your kclo3 is produced cheaply ,because your factoring that into the cost as well, and it can get pricey .This is why most amateurs dont take it to that next step. It is a lot of work for a little payout .

[taiwanluthiers]

For some, price is either ridiculous or even unobtainable. I've heard people in the UK had to pay 40 quids a pound for them. I have to pay 20 dollars a pound for them. I just do not know if that price makes making my own worth it. I've found chlorates can be made very cheaply because MMO is cheap and lasts forever. Platinum would be nice too, if it could last forever too but sources seems to say that they erode fairly fast even under optimal condition, at least compared to MMO (which had an erosion rate of milligrams per ton, whereas Platinum is several grams per ton)

[WSM]

I found some interesting literature From Dr Shimizu, Which he claims Kclo4 can not be derived from Kclo3 alone, but rather NaClo3. I thought this to be odd, and was sure that Swede had already made Kclo4 directly from Kclo3 .

Here is a direct Quote from F.A.S.T. :

 

I guess someone forgot to tell Swede, because he did it. Too many people (apparently even the venerable Dr. Shimizu) presume if industry doesn't do it, it won't work. It can work but it's too much trouble, or not cost efficient enough for industry to bother with. As amateur pyrotechnists who may not have access to industrial chemicals, making it for ourselves may be our only recourse and we're willing to go through much more trouble to get some than industry would even consider.

 

Then there's some of us who are nuts enough to do it, just because we can... !

 

WSM

[pyrojig]

And this is why I love this forum and the pioneers who take the lead. It is folks like you guys who by mistake or chance ( or skill) stumble across and idea or method that changes the industry forever .

[dangerousamateur]

Hi,

 

I've got another question:

 

In a chlorate setup, is it recommendable to let the cell simply run until all chloride is converted, and so reduce the chloride contamination in the final product?

 

I read somewhere that this is likely to cause heavy wear on the anodes, can somebody confirm this? How does the laserred stuff react to such conditions?

 

 

And do you perhaps have some kind of chart for the solubility of KClO3 vs KCl?

At what temperature is the greatest difference, for optimal separation?edit: loocking at this one http://www.oocities..../ksolubil.gifIt seems like normal room temperature gives already the best results. How does that compare with your experience?That would mean I will allways have about 10% chloride in chlorate - not very good...

Edited January 24, 2013 by dangerousamateur

[taiwanluthiers]

You don't want to run the chloride level too low, most anodes will be severely damaged by this, except maybe Lead Dioxide anodes.

 

Potassium chlorate is nearly as soluble as potassium chloride at 100C but its solubility drops off at low temperature... washing it in cold water and crystalizing once is usually enough.

[WSM]

Hi,

I've got another question:

In a chlorate setup, is it recommendable to let the cell simply run until all chloride is converted, and so reduce the chloride contamination in the final product?

I read somewhere that this is likely to cause heavy wear on the anodes, can somebody confirm this? How does the laserred stuff react to such conditions?

And do you perhaps have some kind of chart for the solubility of KClO3 vs KCl?

At what temperature is the greatest difference, for optimal separation?edit: loocking at this one http://www.oocities..../ksolubil.gifIt seems like normal room temperature gives already the best results. How does that compare with your experience?That would mean I will allways have about 10% chloride in chlorate - not very good...

 

Don't try to convert all the chloride; you'll waste power and stress your electrodes unnessessarily. If you add an ammeter (reads current, which is the flow of electrons) to your power circuit feeding the cell, you can monitor your power consumption. Note the starting current high point and when your cell drops to half the current (due to chloride levels dropping as chlorate increases), pull the plug.

 

The lasserred MMO holds up very well, but don't push it. It'll be stressed like other MMO, but handle it reasonably well.

 

There is a solubility chart and you'll have to look for it in Swede's blog...(do your homework )

 

taiwanluthiers already answered the (next to the) last one...

 

The last one: running warmer is more efficient for cell performance, though inefficient for power usage (it's a trade off).

 

WSM

Edited January 24, 2013 by WSM

[taiwanluthiers]

Was just wondering, has anyone tried using Palladium to make perchlorate?

[dangerousamateur]

Potassium chlorate is nearly as soluble as potassium chloride at 100C but its solubility drops off at low temperature... washing it in cold water and crystalizing once is usually enough.

 

Since I never worked with homemade chlorate yet, what percentages are considered "enough"?

 

At 20°C I found 344g/l for KCl and 8,6g for KClO3.

 

That makes a factor of 40 - 2,5% Chloride. Can this be achieved in practice?

 

Do you know in which way the presence of chloride will affect common compositions?

[WSM]

Since I never worked with homemade chlorate yet, what percentages are considered "enough"?

At 20°C I found 344g/l for KCl and 8,6g for KClO3.

That makes a factor of 40 - 2,5% Chloride. Can this be achieved in practice?

Do you know in which way the presence of chloride will affect common compositions?

 

The typical affect is to sensitize the composition, I'm told. I don't care to test the theory, so I'll purify the chlorate I plan to use.

 

WSM

[WSM]

Was just wondering, has anyone tried using Palladium to make perchlorate?

 

Not me, nor have I heard of it; but if you tried it and it proved to work, I don't think I'd be overly surprized.

 

Platinum group metals have interesting properties; their use as catalysts is not the least among them. If you have access to some Pd and try it, let us know what you discover !

 

WSM