making potassium (per) chlorate

[WSM]

wow..!

OK, so the first have a potentiometer for voltaje regulation?

Best,

=)

 

Yes. Well, not voltage regulation as much as adjustment, which I take to mean "fine tuning". Most folks use a supply like this for a computer type circuit which needs exactly 5Vdc. If the supply voltage varies, the output can vary and it's brought back to exactly 5.00Vdc with the voltage adjust.

 

Now for our purposes, we can turn the adjust down for lower output voltages or up for higher outputs.

 

If you look at the photo, the white device under the V ADJ sign is a trimmer pot (sort of like a volume control knob) which takes a very small screwdriver (like a jewellers or for eyeglass repair) to change the voltage output.

 

If you search on eBay for 5V 30A power supply, one like this from China costs about $20 delivered (if they ship to your country).

 

WSM

Edited April 25, 2014 by WSM

[pyrojig]

WSM.

After reading many some patents I am having conflicting thoughts on what starting material to use for a Starting salt for perch. It seems that the industry uses sodium chlorate for obvious reasons ( solubility) but Swede showed that Potassium chlorate can be directly used as a starting salt for the making of perch. Obviously cell operating temps will need to be much higher to keep kclo3 in sol. ,but I have a large amount of "feed stock" that I would love to turn to a very useful perch we are all after. / The more I read the more I feel there are many avenues tot this process . Although the direct approach may require more equipment ( or not.), this may not be a prob for a amateur ,( where max efficiency isnt the end "total goal.")

 

*It seems that several folks here have a stock of kclo3 , and turning this directly into the perch may be desired approach . .....

Edited April 26, 2014 by pyrojig

[taiwanluthiers]

Yea, I was actually thinking of just doing a double displacement with sodium perchlorate and then feeding that chlorate feedstock back into the perc cell...

 

I think one thing to be aware of is the crystals may grow on the anode as well, whether or not that's a problem is another issue...

[schroedinger]

If you have a stock of kclo3 and want to convert it into perc you can surely do this. Just test that it is free of chloride. Then start by using a cell with some ampere going through it, to keep it hot and start with a liquer of about 50-60ºC.

Btw actually I'm not sure if KClO4 or KClO3 precipates first, does sm1 know for sure?

[WSM]

If you have a stock of kclo3 and want to convert it into perc you can surely do this. Just test that it is free of chloride. Then start by using a cell with some ampere going through it, to keep it hot and start with a liquer of about 50-60ºC. Btw actually I'm not sure if KClO4 or KClO3 precipates first, does sm1 know for sure?

 

KClO₃ is less soluble than KCl, and KClO₄ Is less soluble than KClO₃. With the sodium salts, it's the opposite. I expect the potassium perchlorate to drop out as it's formed unless the cell temperatures are very high.

 

WSM

[pex]

Can somebody help my with a calculator?

I have a cell with 9 kg naclo3. 9 liter cell. 11 amp. 40 degrees Celsius. How long dus it taken to convert to naclo4.

 

Thanks allot

[pyroChile]

Hello!

 

@WSM: thanks for you reply!

 

@pex: run time per gram NaClO3= [100/current ef %]x[3216/(106.5xamp in cell)] (minutes)

 

 

Example:

 

50% current ef.

11 amp in the cell

100 gr NaClO3

 

minutes =[100/50]x[3216/(106.5x11)]= 5.49 minutes for 100 gram of NaClO3 to convert NaClO4.

 

 

 

Best regards,

 

 

 

 

=)

[WSM]

Hello!

 

@WSM: thanks for you reply!

 

@pex: run time per gram NaClO3= [100/current ef %]x[3216/(106.5xamp in cell)] (minutes)

 

Example:

 

50% current ef.

11 amp in the cell

100 gr NaClO3

 

minutes =[100/50]x[3216/(106.5x11)]= 5.49 minutes for 100 gram of NaClO3 to convert NaClO4.

Best regards,

=)

You're welcome. If I can help or be helpful, I'm glad.

 

WSM

Edited April 29, 2014 by WSM

[WSM]

WSM.

After reading many some patents I am having conflicting thoughts on what starting material to use for a Starting salt for perch. It seems that the industry uses sodium chlorate for obvious reasons ( solubility) but Swede showed that Potassium chlorate can be directly used as a starting salt for the making of perch. Obviously cell operating temps will need to be much higher to keep kclo3 in sol. ,but I have a large amount of "feed stock" that I would love to turn to a very useful perch we are all after. / The more I read the more I feel there are many avenues tot this process . Although the direct approach may require more equipment ( or not.), this may not be a prob for a amateur ,( where max efficiency isnt the end "total goal.")

 

*It seems that several folks here have a stock of kclo3 , and turning this directly into the perch may be desired approach . .....

Swede has proven that it's possible. Whether we should is the question. Time and experience will tell.

 

WSM

Edited April 29, 2014 by WSM

[WSM]

Yea, I was actually thinking of just doing a double displacement with sodium perchlorate and then feeding that chlorate feedstock back into the perc cell...

 

I think one thing to be aware of is the crystals may grow on the anode as well, whether or not that's a problem is another issue...

 

I'm leaning toward going the sodium route to perchlorate, then exchanging with KCl to KClO₄. I'm not sure, but I think the sodium route might be easier on the anode. We'll see...

WSM

Edited April 29, 2014 by WSM

[WSM]

I'm going out of town this weekend, so I'll set the perchlorate test up to run when I get back.

WSM

Edited April 29, 2014 by WSM

[taiwanluthiers]

I just received the LD anode. From the packaging it was clearly from China... not sure what its use are in industry but the coating appears intact, no sign of shipping or other damages. The anode itself feels heavy (because it's lead). Will see how it works. There are some flaking on the top piece that is connected to the mesh, but I have a feeling it's meant to be that way, since that top section wasn't really MMO (just bare Ti) so it would seem logical that the LD doesn't adhere well to that.

 

I'll let you know once a tank is set up... I think I would like to try a run with potassium chlorate and see how that works...

[MrB]

Since both sodium and potassium chlorate is on the list of things being "banned" in EU, i got a question that might not really belong here, but still seams to be the best place to start... What are the alternatives? Are there even any?

B!

[taiwanluthiers]

I'm not sure... it's got it pretty well covered. I mean the only thing I can think of is sulfur and zinc.

[MrB]

Sodium hypochlorite? I mean bleach. It would be smelly, ineffective, but the upside is, it's "sort of cheap", you get 2L bottle with a "2.5-5%" content for about a buck, at the equivalent of a dollar store. Heating, no, actually boiling it makes sodium clorate fall out of solution, as you concentrate it, and then you just start at page 1 of this thread...

It's not going to be cheap in the end, i mean, what, about of 50-100 grams hypoclorite in 2L, not sure what you could actually get after boiling it down, and losses along the way in the system...

Not sure, but i don't think they are going after KCI yet, so the rest should still be possible to buy in bulk. "Should"....

 

B!

[taiwanluthiers]

Update: I started the perchlorate cell today. I have been doing a sodium chlorate cell and it ran forever (2 weeks or more) at about 10 amps, and the current did not change which made me think the process is going to take a while... I have stopped the cell and will just let the cell liquor evaporate naturally and see what I get... I dissolved as much potassium chlorate into very warm (about 40-50 C) water as it can handle, and started the cell at 5v. The current only went up to 5 amps so I thought I increase the voltage to increase its current, but for whatever reason when I connect +5v and +12v together it does not work at all! I tried everything but in the end I guess the power supply isn't designed to run in that condition (when I measure +5v and +12v with the cell running at 5v, I can see 7v but when I connect them together in the cell it does not work at all). +12v is way too much, the current jumped to about 30 amps when I did that so I stopped it immediately. So far with the cell running only for a few minutes I'm not seeing any anode damage except for some minor discoloration in the cell liquid... lets hope it works. If I can skip the sodium chlorate step it would be great because it feels like making sodium chlorate is a lot more trouble than making potassium chlorate, simply for the fact that sodium chlorate is always in solution so it means hours of boiling in order to purify it.

 

If you want to use sodium hypochlorite it's still much cheaper to just make them in a chlorate cell... commercial bleach is a little expensive and boiling bleach to yield chlorate is troublesome, and the yield is very limited (boil for hours and hours only to get about 10g of chlorate from a bottle of bleach)

 

Update: Cell has been running for a few hours now. No evidence of any erosion, and I can definitely smell ozone when I open the cell to inspect it. I didn't notice it at first but I opened the cell just to confirm, and yes there's a strong smell of ozone in there... So I know perchlorate is being produced. Yield is probably not that good since the cell volume is about 2.5 liters but I can probably just keep adding dry chlorate to the solution as chlorate is consumed... cell temperature holding steady at 50C

Edited May 5, 2014 by taiwanluthiers

[MrB]

If you want to use sodium hypochlorite it's still much cheaper to just make them in a chlorate cell... commercial bleach is a little expensive and boiling bleach to yield chlorate is troublesome, and the yield is very limited (boil for hours and hours only to get about 10g of chlorate from a bottle of bleach)

From what precursor tho, thats the problem were facing over here.

Right now it's not an issue, but in only a couple of months they stop selling the stuff, and another 2 years from then, you cant even store it anymore. Making it when you need it, seams to be a valid solution, illegal to, of course, but no storing means less likely to be, uh, caught red handed, so to speak.

B!

[taiwanluthiers]

The only precursor you need (apart from MMO for chlorate and LD for perchlorate) is potassium chloride, sodium chloride (if you want to make other perchlorates such as ammonium), ammonium chloride, etc.

 

From that + electricity you will have all the chlorate and perchlorate you will ever need. It's much better than trying to boil down a bottle of bleach.

[Arthur]

Using an atx psu you will find that the 5v rail is rated at lots of amps and the 12v rail rated at much less. plus did you series the 5 and 12v rails giving you 17v or reverse series them giving you 7v?? (oh and the -ve rails are rated at even LESS current -maybe only half an amp), it's to do with what a PC usually needs not what hackers want.

[pex]

Hello,

 

I have a question. Maybe somebody can help my with calculate. I put 8.8 kilo of naclo3 in a perchlorate cell. After. A few weeks. when its done how much kilo of naclo4 will i have? I want to clean it with sodium metabisulfite. How many sodium metabisulfite. Do i need? And wen everything is clean.how much water and kcl do i need for te total batch. To make kclo4.

And how many kclo4 will i harvest? I am not realy great in calculate these things.

 

Thanks allot

 

Pex

[pyroChile]

Update: I started the perchlorate cell today. I have been doing a sodium chlorate cell and it ran forever (2 weeks or more) at about 10 amps, and the current did not change which made me think the process is going to take a while... I have stopped the cell and will just let the cell liquor evaporate naturally and see what I get... I dissolved as much potassium chlorate into very warm (about 40-50 C) water as it can handle, and started the cell at 5v. The current only went up to 5 amps so I thought I increase the voltage to increase its current, but for whatever reason when I connect +5v and +12v together it does not work at all! I tried everything but in the end I guess the power supply isn't designed to run in that condition (when I measure +5v and +12v with the cell running at 5v, I can see 7v but when I connect them together in the cell it does not work at all). +12v is way too much, the current jumped to about 30 amps when I did that so I stopped it immediately. So far with the cell running only for a few minutes I'm not seeing any anode damage except for some minor discoloration in the cell liquid... lets hope it works. If I can skip the sodium chlorate step it would be great because it feels like making sodium chlorate is a lot more trouble than making potassium chlorate, simply for the fact that sodium chlorate is always in solution so it means hours of boiling in order to purify it.

 

If you want to use sodium hypochlorite it's still much cheaper to just make them in a chlorate cell... commercial bleach is a little expensive and boiling bleach to yield chlorate is troublesome, and the yield is very limited (boil for hours and hours only to get about 10g of chlorate from a bottle of bleach)

 

Update: Cell has been running for a few hours now. No evidence of any erosion, and I can definitely smell ozone when I open the cell to inspect it. I didn't notice it at first but I opened the cell just to confirm, and yes there's a strong smell of ozone in there... So I know perchlorate is being produced. Yield is probably not that good since the cell volume is about 2.5 liters but I can probably just keep adding dry chlorate to the solution as chlorate is consumed... cell temperature holding steady at 50C

 

 

Hello!

 

 

When you connected, you set the 5v line as cathode and 12v line as anode?

 

 

Why do you do it in two steps? if one assumes that it can be done in one go .. or not?

 

 

 

 

=)

Edited May 5, 2014 by pyroChile

[taiwanluthiers]

Update: The solution has turned transparent brown and I'm seeing specks of black at the bottom of the solution. I'm not sure if it's because the anode is poorly made or if it's just surface coming off that will (hopefully) only happen once... I'm not sure what kind of run time I should be looking at but thought maybe it would be safe to add more chlorate every other day or so...

 

Another update: I checked in 5 more hours, and now the cell has run for a full 24 hours. The brown has stayed the same and has not deepened at all, so I can safely assume it won't erode anymore (probably just surface stuff coming off). The anode originally was more smooth than Patsroom's Chinese anode so it appears there are of higher quality than that... I'm not really sure what kind of run time I'm aiming at but I'd dropped maybe 100 more grams of potassium chlorate into the cell just to make sure it does not run out.

Edited May 6, 2014 by taiwanluthiers

[taiwanluthiers]

I have some crystallization at the bottom of the cell, there is a bit of black stuff mixed in but most of them washes off... I probably have maybe about 400 grams of potassium chlorate in the solution, so as much as I love to clean it up right now I don't want to waste all that feed stock... I'm not sure how good the anode is but it's holding up but it has shed some black bits, not sure from where, if it came from the top of the anode where it wasn't coated in MMO (therefore it wasn't even sticking at all) or the bottom... If it works, it's great, but if it ends up becoming useless after a few days of run, I might just switch to platinized titanium.

 

I don't have any methylene blue at the moment so using a very unscientific way of testing for perchlorate, I tried dissolving about a teaspoon of it in ice cold water, and not much has dissolved (maybe a 10% loss in about 200ml of ice water). Then I went and forced dried a small amount of the crystals (it has a distinctly different crystal structure than known K Chlorate, more like table salt than flat sheet like structure of chlorate), ground it up and made a small amount of buell red with it. When I previously tried to make buell red using potassium chlorate, without changing the chlorate amount (1:1 substitution), the comp would burn very slowly and leaves behind a huge amount of dross (almost as much as the pile). Well this time it burned nice and fast. Some dross were present but based on how fast it burned, I'd say the oxygen balance was right and the dross were due to errors in measurement of the individual chemicals. So after 2 days of run, I have about 50 grams in dry weight of K Perchlorate...

Edited May 7, 2014 by taiwanluthiers

[WSM]

I havcollect the me crystallization at the bottom of the cell, there is a bit of black stuff mixed in but most of them washes off... I probably have maybe about 400 grams of potassium chlorate in the solution, so as much as I love to clean it up right now I don't want to waste all that feed stock... I'm not sure how good the anode is but it's holding up but it has shed some black bits, not sure from where, if it came from the top of the anode where it wasn't coated in MMO (therefore it wasn't even sticking at all) or the bottom... If it works, it's great, but if it ends up becoming useless after a few days of run, I might just switch to platinized titanium.

I don't have any methylene blue at the moment so using a very unscientific way of testing for perchlorate, I tried dissolving about a teaspoon of it in ice cold water, and not much has dissolved (maybe a 10% loss in about 200ml of ice water). Then I went and forced dried a small amount of the crystals (it has a distinctly different crystal structure than known K Chlorate, more like table salt than flat sheet like structure of chlorate), ground it up and made a small amount of buell red with it. When I previously tried to make buell red using potassium chlorate, without changing the chlorate amount (1:1 substitution), the comp would burn very slowly and leaves behind a huge amount of dross (almost as much as the pile). Well this time it burned nice and fast. Some dross were present but based on how fast it burned, I'd say the oxygen balance was right and the dross were due to errors in measurement of the individual chemicals. So after 2 days of run, I have about 50 grams in dry weight of K Perchlorate...

Sounds good, taiwanluthier. Keep up the good work. I think that's a good indication of perchlorate based on your tests and observations.

 

I like the methylene blue solution indicator because it's accurate and stable, unlike the three chlorate tests I've used in the past (accurate but unstable; not keeping much more than a month when mixed). I've kept methylene blue solution for many years (decades) and it's an excellent test for perchlorate, even in the presence of nitrate and chlorate.

 

Keep us updated on your progress as you continue the run. Also, if you can collect the black residue, maybe we can come up with a test to positively identify it.

 

WSM

[taiwanluthiers]

It's not that I can't find methylene blue, they are cheap and readily available at any science/chemical shops... the issue is I just did not happen to have them on hand so I tested it with a really unscientific method... Of course best way to be sure is methylene blue... I just have no idea if there's a good test for residual chlorate.

 

I'm pretty sure the black bit is from the anode, I just can't be sure where... The anode itself looks like nothing has happened but then I have all these black bits. The smell of ozone is also very pervasive when the cell is opened for inspection. Only way I know it's ozone (and not chlorine) is because it smells like one of those air purifier (that makes ozone by the way). In fact people buy ozone generator all the time thinking it will improve indoor air quality but the fact is, surface level of ozone isn't good for you.

 

I need to find another power supply so I can also run a potassium chlorate cell concurrently.