making potassium (per) chlorate

[WSM]

Yesterday I replaced the power supply with the larger supply I talked about earlier.

 

 

The smaller supply is in the foreground of the photo above, on the right and looks larger than it truly is. The larger supply should operate normally with the load applied.

 

As soon as the salt reservoir is complete and filled with pool salt, I'll reassemble the cell and run it again. I still need to repair the panel display so it works properly.

 

Much more to come...

 

WSM

Edited May 26, 2016 by WSM

[memo]

i am expecting more of a yield from my 3 liter cell, going from sodium cloride to clorate to sodium perclorate . then mix with saturared solution of potassium cloride. first run i got 255 grams . the second run that i just finished drying was 416 grams. I am saturating the salt at 60 c. and the potassium chloride at 80 c. 1100 grams of salt (3 liters ) and 750 grams of potassium (2 liters ). am I expecting too much ?

 

memo

[Arthur]

Memo

Without a full set of numbers and an appreciation of your cell mechanism its too hard to estimate what you should get with any accuracy. However if you have produced 416g of good perc then you are probably the first to get anywhere near that among this group.

[WSM]

i am expecting more of a yield from my 3 liter cell, going from sodium cloride to clorate to sodium perclorate . then mix with saturared solution of potassium cloride. first run i got 255 grams . the second run that i just finished drying was 416 grams. I am saturating the salt at 60 c. and the potassium chloride at 80 c. 1100 grams of salt (3 liters ) and 750 grams of potassium (2 liters ). am I expecting too much ?

memo

After your run of sodium perchlorate has reached the point of completion, it's recommended to destroy the residual chlorate before adding the potassium chloride solution to make the potassium perchlorate.

 

If you add sodium metabisulfite (used by wine makers, sometimes) solution, slowly and deep under the surface of the electrolyte, and test for chlorate between each dose; you can achieve a decent clean-up of the sodium perchlorate before you convert it to potassium perchlorate.

 

After you get the potassium perchlorate precipitated, you can give it a good soak in cold (<5^oC), distilled water before filtering the very fine crystals out of the filtrate. This will help to dilute and wash away the soluble sodium contaminants from the new potassium perchlorate precipitate.

 

I highly recommend using a vacuum filtration setup with slow (to keep the powdered potassium perchlorate from going through the filter) lab grade filter paper (check out my blogs and see the way I did it).

 

Good luck.

 

WSM

Edited May 27, 2016 by WSM

[memo]

Memo

Without a full set of numbers and an appreciation of your cell mechanism its too hard to estimate what you should get with any accuracy. However if you have produced 416g of good perc then you are probably the first to get anywhere near that among this group.

 

Arthur when you say I am getting more grams than anyone else it concerns me. I am very new at this and have just the basics when I precipitate the perchlorate out. I wash it in a tub in cold water then run it thru a coffee filter, the kind in a coffee pot that doesn't need a paper filter it is a very fine mesh screen then wash it again in cold water. if I don't have percolate what do I have ?

 

memo

[Arthur]

Don't be concerned. Swede did research, WSM is doing research in conjunction with another person. Several people have contributed electrochemistry theory. BUT No-one has simply gone into production like you have. You are lucky that the research is now available here to let you make your own cell system. BUT I still think that you are the first to actually go into sub kilo production and get yield.

 

KCl to KClO3 is easy. Getting to KClO4 is not trivial though IMO there are easier methods, but they rely on correct quantities during the crystallisation process.

[taiwanluthiers]

I have gotten several pounds of chlorate just with a 2 liter cell. I don't have the means to make perchlorate because of the anode requirement, LD is impossible to buy and it's almost looking like platinum plated anode is cheaper and easier to use than LD.

[memo]

im using pt.plated ti

[WSM]

im using pt.plated ti

 

If you can get an MMO anode, it will make the chlorate easily (but not perchlorate).

 

I'm using platinum plated titanium just for turning the sodium chlorate to sodium perchlorate. I'm also using lead dioxide plated titanium for perchlorates, also.

 

In a high chlorides electrolyte, the platinum is subject to erosion; but not so much in a high chlorates solution.

 

WSM

Edited May 27, 2016 by WSM

[WSM]

Don't be concerned. Swede did research, WSM is doing research in conjunction with another person. Several people have contributed electrochemistry theory. BUT No-one has simply gone into production like you have. You are lucky that the research is now available here to let you make your own cell system. BUT I still think that you are the first to actually go into sub kilo production and get yield.

KCl to KClO3 is easy. Getting to KClO4 is not trivial though IMO there are easier methods, but they rely on correct quantities during the crystallisation process.

 

I've put my perchlorate research on hold because I've used up my meager sodium chlorate stock. This is why my focus has turned to making sodium chlorate.

 

I think you're on the right track starting with sodium chlorate. Do go on the make potassium chlorate as well; many of us have made a LOT of it with MMO on titanium anodes (going from KCl to KClO₃), and it's good experience.

 

If you harvest a good supply of sodium chlorate, going on to make sodium perchlorate is an excellent use for it. See if you can locate a source of sodium metabisulfite, to reduce the residual chlorate and make a pure (chlorate-free) perchlorate. If there is much chlorate in your perchlorate, it should be treated as if it were chlorate (only), for safety.

 

WSM

Edited May 27, 2016 by WSM

[WSM]

Arthur when you say I am getting more grams than anyone else it concerns me. I am very new at this and have just the basics when I precipitate the perchlorate out. I wash it in a tub in cold water then run it thru a coffee filter, the kind in a coffee pot that doesn't need a paper filter it is a very fine mesh screen then wash it again in cold water. if I don't have percolate what do I have ?

memo

 

I suspect you might have perchlorate and chlorate, mixed in unknown proportions. Have you thought of testing it?

 

WSM

[WSM]

Yesterday, I rearranged my monitoring system (panel meters to display Voltage, Amperage and Temperature in ^oC) and mounted the display boxes to a wooden board. I tested them and everything looks good.

 

 

This evening, I'm picking up some fiberglass cloth and using it to hold the fine pool salt inside the salt chamber (PVDF filter housing), without falling into the plumbing or being blown into the RC (Reaction Chamber) by the force of the hot electrolyte being pumped through it. When the salt reservoir is prepared and sealed up, I'll put the system back together and start the first run up again (I shut the initial run down because the original power supply kept over-heating and shutting down).

 

This should work out because after work today, I'm off work for four days and I can monitor the progress of the cell and respond more quickly if something goes wrong. I'd rather be here while the system runs the first few times,

just in case... !

 

WSM

Edited May 28, 2016 by WSM

[memo]

I did a small test today on what I thought was potassium perchlorate, I mixed it 50 / 50 with powdered sugar and put a drop of sulfuric acid on it. it burst into a bright yellow fire it looks like I have chlorate. what next. with the yellow flame is it sodium chlorate ?

 

memo

[WSM]

I did a small test today on what I thought was potassium perchlorate, I mixed it 50 / 50 with powdered sugar and put a drop of sulfuric acid on it. it burst into a bright yellow fire it looks like I have chlorate. what next. with the yellow flame is it sodium chlorate ?

memo

If you have, or can get methylene blue solution, it's an excellent test for perchlorate. Put a drop of methylene blue solution in a couple drops of the electrolyte; if the methylene blue turns purple, perchlorate is there.

 

The first question is, is perchlorate in there? (you've already got reason to suspect chlorate is there)

 

The second question, how much perchlorate and chlorate (quantities and ratio)?

 

Let us know if you can get the reagent to test for perchlorates.

 

WSM

Edited May 28, 2016 by WSM

[memo]

I will have to look and find what it is called in Spanish. might have to order of ebay

 

memo

[Mumbles]

I can't help you with the name in spanish, but it is used to treat aquariums for certain fungal diseases. It may be a source to try and find some.

[memo]

good thanks

 

Azul de metileno

Edited May 27, 2016 by memo

[WSM]

I will have to look and find what it is called in Spanish. might have to order of ebay

memo

Beware.

If you look on eBay, avoid getting it from the former Soviet Union countries. I ordered 100 grams and what came was NOT what I needed (or wanted). If I'm lucky it can be used for a blue smoke generator, since it's useless for perchlorate testing.

 

Good luck.

 

WSM

Edited May 28, 2016 by WSM

[memo]

i hope the pet store will have some about 35k away

 

memo

[WSM]

At 7:00 PM (19:00 hours), I completed my repairs and started up the system again.

 

I tried the cell in all three configurations and met with some success (the salt reservoir needs a little fine tuning), but no leaks or other problems.

 

 

I'll let it run and warm up over night. We'll see where it is in the morning.

 

WSM

Edited May 28, 2016 by WSM

[WSM]

Ah yes, the system has run overnight and the temperature has stabilized (I think), and things appear to operating normally (I hope).

 

 

Putting the salt reservoir together was a bit tricky, and took a lot of thought to come to a method of adding a filter to hold the salt crystals in the chamber as the system ran. I ended up cutting a piece of fiberglass cloth and folding it into four layers, then using a split piece of PVDF tube for a retainer, and carefully pushed the glass filter down to the bottom of the filter housing.

 

It looked good so I filled the housing with the pool salt, which was fine granular crystals, a little larger than table salt (~14-30 mesh), screwed the housing into the cap and sealed the compression fittings; closing the plumbing assembly.

 

I started the system and tried the different fluid flow paths I planned on and they all seemed to work, but I saw salt flowing through the tubing from the reservoir output .

 

Uh oh, what happened? I can think of two problems:

1. The inside of the housing is tapered from the top where it's ID is larger, down to the bottom where it's smaller
2. The fluid flow from the pump is a higher velocity than the mass of salt could stand (so the salt got carried away)

I suspect the filter pad held by the PVDF ring got pushed out of the way and the newly formed salt slurry was pushed into the cell.

This is not an ideal situation, but not a disaster either. As the cell runs and the dissolved sodium chloride is converted to chlorate, the solid chloride crystals will dissolve in the liquor and continue making more chlorate.

 

It's what I wanted, just not where I wanted it. It'll be okay, but I need to modify the internal arrangement inside the salt reservoir, in an effort to keep the salt crystals in there (and not flowing around in the plumbing and cell).

 

The cell is running and warmed up, plus no more issues with the power supply. I have a lot of studying of this setup to do, so I can figure out how to optimize it. This is going to be fun !

 

WSM

Edited May 28, 2016 by WSM

[WSM]

I took a sample of the pool salt and dissolved it in distilled water. When no crystals remained, I added some 1M sodium carbonate solution. It looked clear and I felt like the pool salt would work out despite the higher cost.

 

Being cautious, I decided to wait. After maybe 20 minutes, I saw the water getting slightly cloudy.

 

Nuts!

 

The pool salt is purer, but not "pure". I let the covered sample sit overnight, and not surprisingly, the contaminant settled to the bottom of the sample bottle.

 

 

The pool salt added to the cell probably contains small amounts of calcium and magnesium, but a lot less than the regular water softening salt I purified before starting the cell. I think my initial run of the sodium system will be okay, but I was hoping for better results from my test of the pool salt.

 

Now I have to decide whether I want to purify ALL the salt I use in my sodium systems. If so, why waste money on the pool salt? If I feel the need to purify my brine before use in a chlor-alkali cell, I may as well set up a brine purification system, independent of the other things I'm doing.

 

It's tough being a perfectionist in such an imperfect world .

 

WSM

 

Edit: I never purified the potassium chloride water softening salt used for making potassium chlorate. I've considered purifying it before, but NOW I'm giving the notion a lot more weight.

 

Your end product can only be as good as the materials you start with. If I'm going to make my own oxidizers, they may as well be "as good" as commercial, or even better. This business is going to get more complicated.

Edited May 30, 2016 by WSM

[WSM]

The sodium chlorate cell has been running for 65 hours. As an experiment, I've recovered about 3.3 liters of the electrolyte, transferred it into a PETE jar and put it in a spare refrigerator we keep for overstock foodstuffs. The electrolyte in the jar measured about 54.2^oC and the fridge is about 2^oC where the jar is put.

 

Draining the sample from the cell

 

The sample transferred to a PETE jar and placed in the fridge

 

The electrolyte has a distinct yellow tint and looks similar to the potassium chlorate electrolyte I've worked with in the past. I'll wait till the electrolyte is down to 2^oC and see if any sodium chlorate drops out.

 

I plan to continue with the non-pH controlled experiment for a while, and then add in pH control (plus dial it in) and note the difference during later running of the cell.

 

More to come ...

 

WSM

Edited May 30, 2016 by WSM

[taiwanluthiers]

I remember having to purify potassium chloride that I get because all I could get is those stuff with the red substance mixed into it (no idea why it's even in there) at reasonable cost (I could get reagent grade stuff that is pure but it would cost too much). I don't know what the red stuff is, it has the consistency of oil pastel but it looks to be iron oxide.

[WSM]

I remember having to purify potassium chloride that I get because all I could get is those stuff with the red substance mixed into it (no idea why it's even in there) at reasonable cost (I could get reagent grade stuff that is pure but it would cost too much). I don't know what the red stuff is, it has the consistency of oil pastel but it looks to be iron oxide.

 

Yes, the agricultural chemicals often use additives so they can monitor the effectiveness of the coverage by their spraying equipment. Dissolving it, filtering and recrystallizing the agricultural potassium chloride (muriate of potash) is an expedient way of purifying it before use in a chlorate cell.

 

WSM