Making perchlorate

[pdfbq]

I have also two Chinese Lead oxide anodes. Did not try them yet but I'm very pessimistic about their usability though.

Why would industry would not use these if they work and work well?

 

@WSM:

If you plan a test in the near future let us know.

I we both start a test simultaneously we might both end up with a messy poison liquid.

One would be enough I guess

[WSM]

I have also two Chinese Lead oxide anodes. Did not try them yet but I'm very pessimistic about their usability though.

Why would industry would not use these if they work and work well?

 

@WSM:

If you plan a test in the near future let us know.

I we both start a test simultaneously we might both end up with a messy poison liquid.

One would be enough I guess

 

Hi pdfbq,

 

I have a lot of other things on my plate just now, but I'm interested. Perhaps in a month or two. I know Swede is interested in studying the perchlorate side of things and is working on setting up experiments right now. I bet he'll chime in when he's free .

 

WSM

[WSM]

On the "making (per)chlorate" thread I mentioned using a solution of Viton rubber to protect metals in the chlorate cells. If properly applied it could seal defects on my Chinese LD anodes.

 

This would be the second best solution to the problem. I believe the best fix would be to plate more beta form LD over the damaged electrodes to make them whole.

 

WSM

Edited August 31, 2012 by WSM

[taiwanluthiers]

Is there a guide somewhere on making perchlorates, are platinum wires really necessary for this or is there a cheaper electrode that can be used?

[patsroom]

Is there a guide somewhere on making perchlorates, are platinum wires really necessary for this or is there a cheaper electrode that can be used?

 

There is a lot that can be answer in this forum to the making of per-chlorate. and yes there are some guides out on the internet as well. One of the best things to do is a lot of reading from difference sources, take notes and check your facts. I have found that by reading this forum from start to finish that it contains the one of the most up-todate information in-regards to chlorate production at this time.

The next part to answer about anodes is that one of the other matieral used is a Lead Dioxide anode which has been most difficult to get a good working one. I tried to buy some from China but the anodes where of such poor quality that they may be useless in the continue production of chlorates. But the good news is: Thre are some trying to make good quality one at home!

I will try and find you a web site that has a lot to do with chlorate making and the likes..............Pat

[patsroom]

Is there a guide somewhere on making perchlorates, are platinum wires really necessary for this or is there a cheaper electrode that can be used?

 

There is a lot that can be answer in this forum to the making of per-chlorate. and yes there are some guides out on the internet as well. One of the best things to do is a lot of reading from difference sources, take notes and check your facts. I have found that by reading this forum from start to finish that it contains the some of the best and most up-todate information in-regards to chlorate production at this time.

The next part to answer about anodes is that one of the other matieral used is a Lead Dioxide anode which has been most difficult to get a good working one. I tried to buy some from China but the anodes where of such poor quality that they may be useless in the continue production of chlorates. But the good news is: Thre are some trying to make good quality one at home!

If you will try typing in how to make per-chlorate in the web search engine it will give you some sites to check like this one (http://www.vk2zay.net/article/63) ,,,,,,,,,,,,,,,,,Pat

Edited September 1, 2012 by patsroom

[pyrojig]

patsroom,

the link posted doesnt work.

I believe that Swede was working on one of these as well. It was a heavily coated electrode , of which shedded nuggets during the test run. I hope more time goes into a method for the use of LD. It is a material all pyros could source. But the plating process is a very toxic one, and would require much care and skill to obtain usable electrodes,( and not kill the maker in the process) .

[taiwanluthiers]

The question is, if I am paying 20 dollars per pound for potassium perchlorate (more for ammonium perchlorate), am I going to save any money by making them myself with rock salt and KCl?

 

Titanium is expensive but not overly so (unless you're making an entire car or airplane out of it) but Platinum is really expensive, so I was wondering is there something cheaper that can work as anode? I know graphite pretty much only works for chlorates.

Edited September 1, 2012 by taiwanluthiers

[pdfbq]

@WSM:

Should a proper lead anode just not mind the cracks, like MMO does not mind them? Same with the Pt anodes I have, there is no issue when bar Ti is exposed.

 

@pyrojig:

just remove the '........pats' at the end of the link and you'r fine (http://www.vk2zay.net/article/63). It is very 2005 though ..

 

The question is, if I am paying 20 dollars per pound for potassium perchlorate (more for ammonium perchlorate), am I going to save any money by making them myself with rock salt and KCl?

I already made a lot of perc (NaCl way) but my Pt anodes are wearing out.

I think its cheaper to make perc 'anode wise' (I mean, you might be able to make 2 kilo or more with a $35 dollar anode) but all the other things like jars, power supply current etc will make it more expensive.

 

If we find a way to keep a Pt anode alive to say 10 kilo's we will make a big leap in perc production i think.

 

As WSM states keep the chlorate level high might be the solution and I think its a very good idea, but in a NaClO3->4 cell I have no idea at this moment how to seperate the Na-chlorate from the Na-perchlorate.

Adding KCl does not make sense because you are polluting you mother liquid with NaCl. For Ammonium perc you want clean NaClO4 and no KlCO4.

 

-- or would it be just as simple a boiling down your liquid, cool and have the NaClO3 crystallize out and pour of the NaClO4? ... hmmm

Edited September 1, 2012 by pdfbq

[WSM]

@WSM:

Should a proper lead anode just not mind the cracks, like MMO does not mind them? Same with the Pt anodes I have, there is no issue when bar Ti is exposed.

@pyrojig:

just remove the '........pats' at the end of the link and you'r fine (http://www.vk2zay.net/article/63). It is very 2005 though ..

I already made a lot of perc (NaCl way) but my Pt anodes are wearing out.

I think its cheaper to make perc 'anode wise' (I mean, you might be able to make 2 kilo or more with a $35 dollar anode) but all the other things like jars, power supply current etc will make it more expensive.

If we find a way to keep a Pt anode alive to say 10 kilo's we will make a big leap in perc production i think.

As WSM states keep the chlorate level high might be the solution and I think its a very good idea, but in a NaClO3->4 cell I have no idea at this moment how to seperate the Na-chlorate from the Na-perchlorate.

Adding KCl does not make sense because you are polluting you mother liquid with NaCl. For Ammonium perc you want clean NaClO4 and no KlCO4.

-- or would it be just as simple as boiling down your liquid, cool and have the NaClO3 crystallize out and pour off the NaClO4? ... hmmm

 

With LD, I'm afraid the adhesion to the substrait can be compromised much more easily than MMO over titanium. Basically, I think MMO sticks to titanium better than lead dioxide does. Even MMO can be compromised if fluorine or fluorine compounds find their way into the cell (one such failure is where the titanium is attacked and separates from the MMO, yielding poor conductivity and performance). I think LD sticks to MMO really well if done properly. Swede only had problems with the LD nodules over the bare titanium. The LD on the MMO was (and is) stuck on there pretty good.

 

Since the sodium chlorate is less soluble than the perchlorate, crystallizing the chlorate out (and away from the perchlorate solution) sounds like a very reasonable approach to separating the two. What does industry do? In most of this, we copy industry to one extent or another. Why not here?

 

Let us know what you decide to do...

 

WSM

Edited September 1, 2012 by WSM

[WSM]

With LD, I'm afraid the adhesion to the substrait can be compromised much more easily than MMO over titanium. Basically, I think MMO sticks to titanium better than lead dioxide does. Even MMO can be compromised if fluorine or fluorine compounds find their way into the cell (one such failure is where the titanium is attacked and separates from the MMO, yielding poor conductivity and performance). I think LD sticks to MMO really well if done properly. Swede only had problems with the LD nodules over the bare titanium. The LD on the MMO was (and is) stuck on there pretty good.

Since the sodium chlorate is less soluble than the perchlorate, crystallizing the chlorate out (and away from the perchlorate solution) sounds like a very reasonable approach to separating the two. What does industry do? In most of this, we copy industry to one extent or another. Why not here?

Let us know what you decide to do...

WSM

 

I know I'm answering myself here, but this applies:

 

The patsroom, Chinese LD electrodes seem to have the LD flake off the substrait too easily. Maybe something in their process is lacking and, therefore, good adhesion is not happening. Swede's home-made LD anode number two worked out really well, except for the nodules breaking off where they were over bare titanium rather than the MMO coating. Where the LD was on the MMO, there seems to be a good bond, and I suspect a totally coated MMO substrait would be the best base layer for a solid, beta-form LD anode.

 

WSM

[WSM]

The question is, if I am paying 20 dollars per pound for potassium perchlorate (more for ammonium perchlorate), am I going to save any money by making them myself with rock salt and KCl?

Titanium is expensive but not overly so (unless you're making an entire car or airplane out of it) but Platinum is really expensive, so I was wondering is there something cheaper that can work as anode? I know graphite pretty much only works for chlorates.

 

Solid platinum is certainly very expensive, BUT we only need the surface to be platinum, so just 50-150 microns thickness will do, typically. Of course, the thicker the plating, the longer it will last in our cells if everything else is right.

 

The less expensive option is beta-form lead dioxide (PbO₂) which is the harder, crystalline form of LD. The more common and easier to produce, but spongy alpha-form is undesireable for our cells unless filled and covered by the beta-form. There are other perchlorate electrode options; but, so far, these two seem to be the most available to amateurs. Let's see what the future holds .

 

WSM

[Arthur]

I doubt that there will be a cost advantage for DIY production but for some people there is an availability advantage.

 

Neither chlorate not perchlorate are retail in the UK now unless you want lab grade (*99.99% pure for silly money) Some private suppliers exist on and off ebay. The original project started to try to preserve perc supplies when the market dries up totally. Remembering that importing a white crystaline powder may attract all the wrong attention when passing international trade and customs.

[taiwanluthiers]

I know the polish suppliers should happily sell to the UK, and it does not pass through customs because it is within EU (Poland to Switzerland goes through custom because while Switzerland is in the Schengen Agreement, it is not in the EU). You pass through immigration when going from France to the UK because the UK is in the EU, but not the Schengen Agreement, and customs and immigration are not the same thing in the EU. Immigration checks papers (like if you're an EU citizen, if you have a visa, etc.) but they're not interested in what you're bringing. It is only customs that care about these kind of stuff. Most of the issue is whether or not carriers allows you to ship the materials. If they have no issue customs won't have any issue either. I've ordered plenty of white powder looking thing and no one really cared, custom people are trained to tell the difference between illegal drugs and any other substance. That polish supplier is also quite cheap. There are numerous suppliers within the EU that sells perchlorates in fact. The only issue would be if you're too young for pyro suppliers to sell to you.

 

I don't think you need a license to import chemicals (correct me if I am wrong), unless that chemical is already illegal in that country for whatever reason, however that's not to say you don't need permission to ship the said chemical through that carrier. The only issue would be any arms related export restriction that the US have, and I would think only chemicals that would be under that classification are chemicals you shouldn't have anywhere near you (like Mustard gas).

 

 

I do not know what is silly money for 99.99% percs but in Taiwan that purity is 20 dollars a pound. For power supplies I might find a cheap PC power supply or laptop AC adapter but I do not know what kind of currents are needed. Jars and bottles are cheap. The issue I am having is purity of the product, and I guess for AP it would be totally worth it because it's silly expensive no matter the source. I believe you need to chemically destroy all trace of chlorate before you convert the mother liquid into AP to avoid forming Ammonium Chlorate. I wasn't sure if platinum plated anodes are good enough, I was under the impression I needed Pt wires that costs about 16 dollars per cm (for a .5mm wide wire).

 

It's illegal to have more than 50kg of perchlorates in Taiwan so even if I make more than that quantity, I'd be breaking the law.

[patsroom]

@ taiwanluthiers

 

 

 

I really think that if you was to read - making potassium (per) chlorate :

 

 

http://www.amateurpy...m-per-chlorate/

 

and Swede's works you would find many of your answers. His blog is at You'll put your eye out:

 

http://www.amateurpy...put-youreye-out

These are the most up-to-date informantion sites that I know of and the other site I listed will help you in you studies to determine if it is feasible or not for you.............Pat

[WSM]

@ taiwanluthiers

I really think that if you was to read - making potassium (per) chlorate :

http://www.amateurpy...m-per-chlorate/

and Swede's works you would find many of your answers. His blog is at You'll put your eye out:

http://www.amateurpy...put-youreye-out

These are the most up-to-date informantion sites that I know of and the other site I listed will help you in you studies to determine if it is feasible or not for you.............Pat

 

patsroom is right, Swede's work is a good read and you can learn a lot from his experiences chronicled in these references. I've read them through several times and avoided many pitfalls by following his blogs. Enjoy...

 

WSM

[ANFO]

In an effort to educate myself about the process of making LD electrodes, I was reading through some patents, and I found this pretty useful: from http://www.google.co...tents/US4064035 sorry if you've seen this before

A look into the more industrial way of doing it..

Edited September 3, 2012 by ANFO

[WSM]

In an effort to educate myself about the process of making LD electrodes, I was reading through some patents, and I found this pretty useful: from http://www.google.co...tents/US4064035 sorry if you've seen this before

A look into the more industrial way of doing it..

 

A member here has made an excellent LD anode and documented it in his blog, "you'll put your eye out". There is a wealth of information here at APC, but you have to dig it out. If you go the patent route, you'll be reinventing the wheel. If you follow those here who've already "traveled the road" you seek, you'll be miles ahead of where you'd be on your own.

 

Do your homework; a lot of what you're seeking is already here...

 

WSM

[Swede]

As WSM states keep the chlorate level high might be the solution and I think its a very good idea, but in a NaClO3->4 cell I have no idea at this moment how to seperate the Na-chlorate from the Na-perchlorate.

Adding KCl does not make sense because you are polluting you mother liquid with NaCl. For Ammonium perc you want clean NaClO4 and no KlCO4.

 

I read a very interesting article on how perchlorate was made in WW2. As expected, they used Pt anodes. The mixture at the end was an aqueous NaClO3 and NaClO4. I remember distinctly that the end liquor was something like 99% perchlorate, 1% chlorate, trace chloride.

 

To create the potassium salt, they carefully measured out not a stoichiometric amount of KCl, but slightly below that. Added to the Na mixture, at a cool temperature, the displacement took place, generating solid KClO4, and aqueous NaCl. The perchlorate solid was spun out in a centrifuge, and the aqueous portion was now basically... brine. This was fed back into their chlorate cells, thus the chloride ion from the KCl became part of the starting liquor.

 

How cool is that? They didn't need to buy any more NaCl once the process started, because they regenerated the NaCl in the displacement phase. Only mechanical losses had to be replenished with new NaCl.

 

This means that if you can somehow determine the exact amount of NaClO4 in your liquor (not easy), using a slightly below stoich. amount of KCl would introduce almost no aqueous K+ ions, and you'd be left with a liquor containing NaCl, NaClO3, and just traces of K+. These traces would probably remain aqueous through subsequent processing.

[WSM]

I read a very interesting article on how perchlorate was made in WW2. As expected, they used Pt anodes. The mixture at the end was an aqueous NaClO3 and NaClO4. I remember distinctly that the end liquor was something like 99% perchlorate, 1% chlorate, trace chloride.

To create the potassium salt, they carefully measured out not a stoichiometric amount of KCl, but slightly below that. Added to the Na mixture, at a cool temperature, the displacement took place, generating solid KClO4, and aqueous NaCl. The perchlorate solid was spun out in a centrifuge, and the aqueous portion was now basically... brine. This was fed back into their chlorate cells, thus the chloride ion from the KCl became part of the starting liquor.

How cool is that? They didn't need to buy any more NaCl once the process started, because they regenerated the NaCl in the displacement phase. Only mechanical losses had to be replenished with new NaCl.

This means that if you can somehow determine the exact amount of NaClO4 in your liquor (not easy), using a slightly below stoich. amount of KCl would introduce almost no aqueous K+ ions, and you'd be left with a liquor containing NaCl, NaClO3, and just traces of K+. These traces would probably remain aqueous through subsequent processing.

 

That sounds excellent! Can you share a copy of that article?

 

WSM

[WSM]

I read a very interesting article on how perchlorate was made in WW2. As expected, they used Pt anodes. The mixture at the end was an aqueous NaClO3 and NaClO4. I remember distinctly that the end liquor was something like 99% perchlorate, 1% chlorate, trace chloride.

 

To create the potassium salt, they carefully measured out not a stoichiometric amount of KCl, but slightly below that. Added to the Na mixture, at a cool temperature, the displacement took place, generating solid KClO4, and aqueous NaCl. The perchlorate solid was spun out in a centrifuge, and the aqueous portion was now basically... brine. This was fed back into their chlorate cells, thus the chloride ion from the KCl became part of the starting liquor.

 

How cool is that? They didn't need to buy any more NaCl once the process started, because they regenerated the NaCl in the displacement phase. Only mechanical losses had to be replenished with new NaCl.

 

This means that if you can somehow determine the exact amount of NaClO4 in your liquor (not easy), using a slightly below stoich. amount of KCl would introduce almost no aqueous K+ ions, and you'd be left with a liquor containing NaCl, NaClO3, and just traces of K+. These traces would probably remain aqueous through subsequent processing.

 

This looks like an excellent continuous process, I'd like to know more details.

 

WSM

[taiwanluthiers]

I would chemically destroy all chlorates though before doing the reaction... even a small trace of chlorate can make the perchlorate very sensitive. Also if you're making ammonium perchlorate any trace of chlorate can be dangerous.

 

As for the brine solution being fed back... the concern is contamination from the further handling... plus NaCl is cheap... much cheaper than KCl that's for sure. Not much savings to be had unless its done on an industrial scale.

[pdfbq]

I found this small but nice article.

What I find nice about it is that it describes what I have noticed also namely an increase in current at the end of a perc run, as the decrease of efficiency.

 

encyperc.html

 

It also says something about separating the perc from the chlorate. It comes down to the same principle as seperating chlorate from chloride after a NaCl run.

Because the leftover chlorate is little what will com out of solution first is the perchlorate. One needs a mutual solubility table to get precise

 

One other interesting point I want to mention is that I did an entire KCl -> KClO3 run with my Pt anode and it did not got destroyed by it.

Reason why I did this run is that I was lazy and did not know about the Cl^- ion being that bad for a Pt anode.

I don't say that it does not do any harm, it just did not ruin my Pt anode as an MMO anode really gets ruined in a perc run.

 

I'm starting up again.. I want to experiment with keeping the chlorate level high. Thinking about a way to determine where I am about in a run.

I made my current perc stock by simply letting everything run until the current goes up and the anode gets gold-brown but I really believe that is not good.

[Swede]

If you ran KCl to KClO3 using Pt, you probably also generated some quantity of perchlorate as well.

 

Pt won't be ruined quickly by excess chloride, but it will definitely erode faster than if chloride is minimized. I think in the end, with Pt at least, the goal is to get enough perchlorate out of it so that the cost per kilo remains below (hopefully WELL below) commercial perc.

 

That's a good article, and emphasizes again that industrially, they make this stuff very quickly with high power. I keep thinking I'd like to try this - a very small cell with HUGE electrodes and high current, and a stock chloride trickling in at some low flow, let's say 500ml per hour. The cell is going to get to near boiling. If using KCl what comes out is going to be very high in chlorate, and as it trickles into a cooling tank, the KClO3 is going to crystallize out quickly. From there, the depleted liquor flows into a replenishment tank, which has a thick bed of KCl at the bottom.

 

There are a bunch of interesting ways to do this, that's for sure.

[WSM]

I found this small but nice article.

What I find nice about it is that it describes what I have noticed also namely an increase in current at the end of a perc run, as the decrease of efficiency.

encyperc.html

It also says something about separating the perc from the chlorate. It comes down to the same principle as seperating chlorate from chloride after a NaCl run.

Because the leftover chlorate is little what will com out of solution first is the perchlorate. One needs a mutual solubility table to get precise

One other interesting point I want to mention is that I did an entire KCl -> KClO3 run with my Pt anode and it did not got destroyed by it.

Reason why I did this run is that I was lazy and did not know about the Cl^- ion being that bad for a Pt anode.

I don't say that it does not do any harm, it just did not ruin my Pt anode as an MMO anode really gets ruined in a perc run.

I'm starting up again.. I want to experiment with keeping the chlorate level high. Thinking about a way to determine where I am about in a run.

I made my current perc stock by simply letting everything run until the current goes up and the anode gets gold-brown but I really believe that is not good.

 

Hi pdfbq,

 

What is the original source of this article?

 

It was an interesting read (especially after I cleaned it up with Word). Thanks for sharing it.

 

WSM