making potassium (per) chlorate

[WSM]

Well, the tests are quantitative depending on what kind of toys you have access too. A UV/Vis spectrometer makes things a lot easier.

 

The quick test for iron is done by adding acidified Potassium Thiocyanate solution. Equal amounts of 10% w/v KSCN and 2M HCl are mixed just prior to use. A few drops of 3% hydrogen peroxide are then added. A brick red color indicates the presence of iron. It's dependent on Ferric iron, thus the hydrogen peroxide. I think this test is fairly sensitive.

 

My toys are limited (unless you count the old dinosaur AA machine in the corner [haven't used it yet and don't know if it will work]) but a few reagents I do have. Thanks for the Fe⁺⁺⁺ test, I'll have to give that one a try. Does anything interfere or is it specific? Thanks again.

 

WSM

[WSM]

I forgot the exact source I read about the chloride sensitivity. I am reasonably sure it came from Principles of Pyrotechnics by Shidlovskiiy.

 

Hi Mumbles,

 

I'll have to give Shidlovskiy a re-read and see if I can find that reference. Thanks for the heads up.

 

WSM

[WSM]

Knock, knock...

 

Hey, I just wanted to pop in and see what you all were doing.

 

You guys are amazing, I cant understand a thing you guys post but I sure am impressed. One question before you push me back out the door into "neural typical" land, is the manufacturer of (Per) chlorates at all financially feasible?

 

Hi Dagabu,

 

I believe the manufacture of perchlorates is financially feasible; at least it is after you're set up to do it (and that's the rub... getting there is half the fun ).

 

Chlorates on the other hand; definately, yes. It can be done very economically, even with higher end materials (such as MMO and Ti electrodes, etc.).

 

WSM

Edited November 1, 2010 by WSM

[chemid]

thanks for the input.

 

I'm going to separate the liquid while hot, then rinse the crystals with distilled water. (at this point will the crystals be soluble in ice cold distilled water?) I'm still thinking of how I can setup a vacuum to dry them.

 

Bike master, I am very confused by your post. You said to let it cool down, then filter it a couple times. That seems like the opposite of what I should do to get rid of contaminates as recommended form other users.

 

Is their anyway I get get CLO4 instead of CLO3 with my setup? CLO4 is less sensitive and a better oxidizer so I think that would create a safer mix.

 

I heard that I can run table salt (NaCL) in my setup for a lot longer. Boil the entire solution for a quite a bit ~ 50min to get rid of hypochlorites. Then mix it with a hot batch of KCL (water softner). Let the mixed solution rest and the only thing that will percipitate out would be ClO4. Which I would then also wash with distilled water.

 

Is that correct or is there an easier way.

Edited November 1, 2010 by chemid

[Arthur]

Chemid you may get chlorate with a MMO/Ti electrode pair, but you will not get perc. The electrochemistry of perc manufacture is slightly different and needs better electrodes, a slightly higher voltage and freedom from chloride.

SO FAR only lead dioxide and platinum are useful for the chlorate to perc stage, and there must be no residual chloride present or the Pt may be destroyed. Lead dioxide electrodes are very difficult to make but are safe to run straight through from chloride to perc. Read the who;e thread and read all of "Swede"'S blog here.

[bikemaster]

 

Bike master, I am very confused by your post. You said to let it cool down, then filter it a couple times. That seems like the opposite of what I should do to get rid of contaminates as recommended form other users.

 

 

 

Do you know what recrystallization mean?

It mean that you dissolve everything and then you wait for everything to recrystallize. If there is a big difference between the solubility of the different component of the solution, they will recrystalize in stage (one by one). So because KClO3 is less solube that KCl, we can do that to purify the KCL03!

 

The idea under cool the liquor first is to get the most KCLO3 possible, but for sure you will get more impurity if you just want to rince your product.

 

The first filtration is simply to get the solide out of the solution. And yes, at this moment, you have more contaminates in your product that if you take you crystals out when the cell liquor is hot.

 

Then you disolve the crystals and you filters it (at this moment your get rid of all insolubles contaminants (black oxide from the SS anode))

 

Then you let recrystallize ! (at this moment you get rid of almost all high solubility contaminants(KCl,KOH...etc))

 

But if you do like you want to do, you will get rid of the "high solubility contaminants". Maybe your cell is at his at his first run, but with age, your cathode will slowly turn black and make some deposit... They will need to be wash, and the best way to do this is to do a recrystallization!

 

 

 

 

[WSM]

thanks for the input.

 

I'm going to separate the liquid while hot, then rinse the crystals with distilled water. (at this point will the crystals be soluble in ice cold distilled water?) I'm still thinking of how I can setup a vacuum to dry them.

 

 

Hi chemid,

 

The better method may be to first let the hot liquid cool to room temperature (20-30 degree C; 68- 86 degree F), collect the crystals, rinse them with chilled DI water and then dry them. Take the depleated mother liquor, replenish with fresh KCl and start the next batch. I've had better luck (and a cleaner cell) using CP titanium for a cathode (CP is "commercially pure"). The cooler the rinse water, the less your chlorate will dissolve. Save all your liquids and reuse them; this is good H2O economy! Do You have a photo of your setup?

 

 

WSM

Edited November 2, 2010 by WSM

[WSM]

Hi chemid,

 

If you want to purify your chlorate, take the rinsed crystals and dissolve them in distilled water (this goes faster if done on a hotplate with stirring). Remove the chlorate solution from the heat source and let it cool. It will start to form new crystals as it cools. When it reaches room temperature put it in a refrigerator and chill it down to about 5 degrees above freezing to recover the maximum amount of chlorate crystals. Pour off the chilled liquid and separate the crystals from the liquid with a plastic sieve (or scoop them out with a fish net). Dry and store the crystals till you're ready to grind and use them.

 

The rinsed and recrystalized chlorate will be very pure and better than what we get from the regular suppliers. Save the rinse water and the water left over from recrystallizing to dissolve more chloride and make more chlorate. The chlorate cell is more efficient if there are already hypochlorites and chlorates in the mother liquor (you can't get them all out anyway so take advantage of them being there ).

 

WSM

[Bonny]

Hi Chemid,

 

I've had great luck scooping wet chlorate crystals out of the cell with an aquarium fish net (about $1 or so at Walmart and it keeps my hands from smelling like bleach), then put them in a compatible fine mesh fabric sieve over a glass bowl. Rinsing the crystals with chilled distilled water is a good idea plus save the rinse water for make up water in the next run. Swede uses the bucket filters used for biodiesel manufacture to separate and wash his crystals and I think that's a great idea (see Swede's blogs, an excellent source of good ideas).

 

Coffee filters are a fairly cheesy substitute for real lab filter paper. The best setup would be a vacuum filtration setup with a buchner funnel, real filter papers and a source of vacuum (even a water aspirator would work). I know a man who uses a salad spinner with a fine (synthetic) fabric liner in it all set in a small plastic washtub as a "poor-mans- centrifuge" to remove moisture from his chlorate crystals.

 

WSM

 

 

Crystalization is an excellent method of purification (nature's way) and does a very good job of separating what we want from what we don't. My main concern is since we are re-using the rinse water and mother liquor from the cell, are we concentrating the contaminants in our systems? We are, but the crystalization is removing them from our product. Given this reality, I believe we need to limit the number of cycles we put the water through, cut our losses at some point, dump the old solution and start fresh with new. Experimentation is required to determine the best limits to set (Where's Swede when you need him? Maybe I'll have to step up to the plate on this one ).

 

By careful rinsing of our crystals with chilled purified water our product purity is usually 99.9% if we're careful. That's closer to reagent grade than the technical grade material usually used in pyrotechnics. The number one contaminant in commercial chlorate is KCl. If that's the worst we should be okay using our chlorate directly. My ultimate goal is to create feedstock for a perchlorate system (actually it's learning how on a DIY basis). My actual need for KClO4 is low but my need for practical knowledge on producing it is considerable, and my main motivation! It's impressive how small a system will provide more oxidizer salt than most amateurs can use in the normal course of experimenting .

 

WSM

 

(WHEN) I had my cell going ( I have ~30lbs of KClO3), I scooped the crystals into a bucket screen with 200 mesh SS, and allowed to drain before a few hard washings with distilled ice cold water. As the price of KCl is so low, I was not concerned with losses. I only recycled my liquor and/or wash water once or twice, usually starting fresh. The product was then dissolved, (neutralized if I was going to keep it as KClO3) , filtered through several coffee filters and re-crystalized, followed by a final washing with ice cold water. The product tested free of any KCl using silver nitrate to test.

I did use a buchner funnel apparatus a few times on the final stage, made from a plastic strainer (with coffee filters) mounted into a bucket lid and a shop vac for suction...it works quite well.

 

My main intent for the chlorate is also feedstock for making perchlorate, and I have made several lbs. I have still detected trace amounts of chlorate with the NPAA (see Swede's blog) I think my perc is (almost) usable, but have still not finshed the purification and my experiments are on hold right now as currently I have no workshop. IMO opinion, I think the perc can be purified by 2 or 3 recrystalizations, rather than by chemical means, but have not finished my experiments.

 

 

You guys are amazing, I cant understand a thing you guys post but I sure am impressed. One question before you push me back out the door into "neural typical" land, is the manufacturer of (Per) chlorates at all financially feasible?

 

For me ...No.

I've fried 2 platinum anodes so far... If I did the math, my perc is probably costing me .....way too much I can't easily buy it though, so it's my best option.

[WSM]

(WHEN) I had my cell going ( I have ~30lbs of KClO3), I scooped the crystals into a bucket screen with 200 mesh SS, and allowed to drain before a few hard washings with distilled ice cold water. As the price of KCl is so low, I was not concerned with losses. I only recycled my liquor and/or wash water once or twice, usually starting fresh. The product was then dissolved, (neutralized if I was going to keep it as KClO3) , filtered through several coffee filters and re-crystalized, followed by a final washing with ice cold water. The product tested free of any KCl using silver nitrate to test.

I did use a buchner funnel apparatus a few times on the final stage, made from a plastic strainer (with coffee filters) mounted into a bucket lid and a shop vac for suction...it works quite well.

 

My main intent for the chlorate is also feedstock for making perchlorate, and I have made several lbs. I have still detected trace amounts of chlorate with the NPAA (see Swede's blog) I think my perc is (almost) usable, but have still not finshed the purification and my experiments are on hold right now as currently I have no workshop. IMO opinion, I think the perc can be purified by 2 or 3 recrystalizations, rather than by chemical means, but have not finished my experiments.

 

 

 

 

For me ...No.

I've fried 2 platinum anodes so far... If I did the math, my perc is probably costing me .....way too much I can't easily buy it though, so it's my best option.

 

Hi Bonny,

 

Excellent work. I'm hoping to duplicate Swede's LD plating success but in a different configuration. I see LD, if done right, being the most economical option for amateurs. The plating of LD on MMO by Swede was a serious breakthrough in my opinion and a good place to start. Once all that is done, I can see a lot of chlorate feedstock turning into perchlorate !

 

I'm considering plating on some DeNora MMO tubing I acquired. The goal is to end up with a heavy beta form LD coat on a solid MMO surface. The rest will be trivial after the specialized plating process. The next step will be putting the new electrodes through their paces converting chlorate to perchlorate and see how long they (the electrodes) last. All these grandiose plans will have to wait till I'm through tweaking my continuous chlorate system experiments.

 

WSM

Edited November 2, 2010 by WSM

[WSM]

Hi Bonny,

 

Excellent work. I'm hoping to duplicate Swede's LD plating success but in a different configuration. I see LD, if done right, being the most economical option for amateurs. The plating of LD on MMO by Swede was a serious breakthrough in my opinion and a good place to start. Once all that is done, I can see a lot of chlorate feedstock turning into perchlorate !

 

I'm considering plating on some DeNora MMO tubing I acquired. The goal is to end up with a heavy beta form LD coat on a solid MMO surface. The rest will be trivial after the specialized plating process. The next step will be putting the new electrodes through their paces converting chlorate to perchlorate and see how long they (the electrodes) last. All these grandiose plans will have to wait till I'm through tweaking my continuous chlorate system experiments.

 

WSM

 

Then again, patsroom is offering Chinese made LD anodes for $55 plus S&H (in the chlorate cell ?s section). I'd be willing to try one and see how they hold up. If I do get one, I'll report back how it works so all will benefit. Let's see how this turns out .

 

WSM

Edited November 3, 2010 by WSM

[WSM]

Then again, patsroom is offering Chinese made LD anodes for $55 plus S&H (in the chlorate cell ?s section). I'd be willing to try one and see how they hold up. If I do get one, I'll report back how it works so all will benefit. Let's see how this turns out .

 

WSM

 

I just made the plunge and ordered one of the LD anodes from Pat. I sent the funds by PayPal. When it comes I'll set up a trial cell and run it to see how it works. I'll try to gather the basic specs as it runs (at least volts, amps and temperature as well as the time duration of the run; should I try to get anything else?) and share them here. Pat suggested 50 Amps and 7.5 Volts, and I'll see if one of my PS's will happily do that. Now I just need to wait !

 

More later...

 

WSM

Edited November 4, 2010 by WSM

[Bonny]

I just made the plunge and ordered one of the LD anodes from Pat. I sent the funds by PayPal. When it comes I'll set up a trial cell and run it to see how it works. I'll try to gather the basic specs as it runs (at least volts, amps and temperature as well as the time duration of the run; should I try to get anything else?) and share them here. Pat suggested 50 Amps and 7.5 Volts, and I'll see if one of my PS's will happily do that. Now I just need to wait !

 

More later...

 

WSM

 

Sounds good WSM. I'll be ordering an LD anode later today, but won't be testing anytime soon. In the past (using Pt anodes) IIRC I was running about 7.5V @10A using a battery charger. My only other power supply is from a PC (great for chlorate). I might set that up although the voltage will be ~5V, but I can pump about 20+Amps into the cell. Hopefully in a few months I'lll have a workshop set up again.

I'm looking forward to hearing some good results.

[pdfbq]

I use just a PC power supply for perc. I use the 5.2 V and run ~16 Amps.

I convert in 5 days ~1.5 kilo of NaClO3 to NaClO4 with this setup (Pt anode).

For me fast enough

Edited November 4, 2010 by pdfbq

[WSM]

I just made the plunge and ordered one of the LD anodes from Pat. I sent the funds by PayPal. When it comes I'll set up a trial cell and run it to see how it works. I'll try to gather the basic specs as it runs (at least volts, amps and temperature as well as the time duration of the run; should I try to get anything else?) and share them here. Pat suggested 50 Amps and 7.5 Volts, and I'll see if one of my PS's will happily do that. Now I just need to wait !

 

More later...

 

WSM

 

I just read a PM from Pat, the anode is on the way! It's travelling less than 800 miles so it ought to be here in two or three days. I told Pat I'd let him know when it arrives and I'll report it here, too. I have a Pyrex battery jar roughly 6" diameter by 12" high. I'm considering using it for a temporary test cell to convert KClO3 to KClO4. I'll post photos if I do that. More later...

 

WSM

[WSM]

I have the basic structure completely built for the continuous experiment:

The photo shows the EC (gray PVC) the RC (green PVC) and the CC (white polypropylene), all connected with 1" PVC plumbing fittings. I still need to plumb it all for various fluid injections as well as electrical sensors and metering, then fill it with salt solution and start it running.

 

The lid for the CC is not beautiful, just effective. It's fabricated from 1/4" gray PVC plate and is a snug fit for the PP crytalization chamber (which is 18" square by ~7" tall and one piece construction, a tad over 1/4" thick). I will continue to ready this assembly for operation (in my spare time) as quickly as I can.

 

More later...

 

WSM

Edited November 6, 2010 by WSM

[ausgoty]

I just read a PM from Pat, the anode is on the way! It's travelling less than 800 miles so it ought to be here in two or three days. I told Pat I'd let him know when it arrives and I'll report it here, too. I have a Pyrex battery jar roughly 6" diameter by 12" high. I'm considering using it for a temporary test cell to convert KClO3 to KClO4. I'll post photos if I do that. More later...

 

WSM

 

Wouldn't it be converting NaClO3 to NaClO4?

 

I would imagine that the amount of water needed to disolve any quantity of KClO3 would make electrolysis very slow if not impossible?

[WSM]

Wouldn't it be converting NaClO3 to NaClO4?

 

I would imagine that the amount of water needed to disolve any quantity of KClO3 would make electrolysis very slow if not impossible?

 

Swede already proved KClO3 to KClO4 workable and as a "proof of concept", my test doesn't have to be big. I've considered using the sodium salts, but since my goals for the perchlorate would be colors, I'd rather avoid sodium contamination if I can.

 

I may yet try sodium, just to say that I did, and compare the results; Why not?!

 

WSM

[bikemaster]

Swede already proved KClO3 to KClO4 workable and as a "proof of concept", my test doesn't have to be big. I've considered using the sodium salts, but since my goals for the perchlorate would be colors, I'd rather avoid sodium contamination if I can.

 

I may yet try sodium, just to say that I did, and compare the results; Why not?!

 

WSM

 

NaCl will be more friendly will lead dioxide anode because it doesn't cristallizes went it turn into perchlorate. I don't know if you had see some microscope picture of lead dioxide anode surface but it looks like graphite surface (a lot of porosity) and because of that, the crystal tend to form in the hole and that tend to destroy the anose much faster. So like graphite, lead dioxide should have a longer life in a sodium perchlorate cell ( observation from dann22).

 

I also don't think that they will be a lot of sodium, because there is a big difference between the solubility of (NaCl,NaClO3,NaClO4) and KCLO4. The only contaminant that will be harder to get rid of is the chlorate... But read the swede blog and you will see some thecniques.

 

I am waiting to see if your cell will do well!!!

 

[pdfbq]

I've considered using the sodium salts, but since my goals for the perchlorate would be colors, I'd rather avoid sodium contamination if I can.

I do it the sodium way and have no problems at all to get rid of the sodium in the end. I recrystallize two times and job done.

When I do an AgNO3 test there is hardly any chlorine present. Way less than tap water at least.

My Phiko blue and Ruby red:

The only contaminant that will be harder to get rid of is the chlorate...

I think there are some advantages starting with sodium and one of them is that the destruction of the chlorate is very simple. I have a two liter cell for my perchlorate. When the run has finished i put in 60 grams of sodium metabisulphite and heat slowly (I put the jar on a 200 C hotplate and heat until it it starts bubbling a bit ) I test with indigo carmine and HCl.

Edited November 7, 2010 by pdfbq

[nekronuke]

From the stuff i've played with, Aluminum is a nice cover for small pyrotechnics, but not much else... i use it when making wimpy things (such as putting a pack of aluminum ophorate (i believe that is the chemical) coated sand into it. Sounds close to an M80 if you use a whole pack and tamp it tight enough...

But thats off topic, i've never used it as an anode, but from what i've seen (youtuuuube) thats all it really does in any reaction. But i don't know what the released gas is, either.

[Bonny]

From the stuff i've played with, Aluminum is a nice cover for small pyrotechnics, but not much else... i use it when making wimpy things (such as putting a pack of aluminum ophorate (i believe that is the chemical) coated sand into it. Sounds close to an M80 if you use a whole pack and tamp it tight enough...

But thats off topic, i've never used it as an anode, but from what i've seen (youtuuuube) thats all it really does in any reaction. But i don't know what the released gas is, either.

 

That's two idiotic posts of yours I've just read. You should do some reading and some learning...but it sounds like you just want to make big bangs anyway. I'll wait for the mods to take care of this.

[dagabu]

From the stuff i've played with, Aluminum is a nice cover for small pyrotechnics, but not much else... i use it when making wimpy things (such as putting a pack of aluminum ophorate (i believe that is the chemical) coated sand into it. Sounds close to an M80 if you use a whole pack and tamp it tight enough...

But thats off topic, i've never used it as an anode, but from what i've seen (youtuuuube) thats all it really does in any reaction. But i don't know what the released gas is, either.

 

Go away k3wl!!

[inonickname]

From the stuff i've played with, Aluminum is a nice cover for small pyrotechnics, but not much else... i use it when making wimpy things (such as putting a pack of aluminum ophorate (i believe that is the chemical) coated sand into it. Sounds close to an M80 if you use a whole pack and tamp it tight enough...

But thats off topic, i've never used it as an anode, but from what i've seen (youtuuuube) thats all it really does in any reaction. But i don't know what the released gas is, either.

 

Go away you bloody k3wl. You aren't a pyrotechnician, you're a wannabe bomber. Aluminium fulminate and ophorate? Maybe go find a drug forum to go to... You know nothing about pyrotechnics, but you seem to have great LSD!

[kaizoku]

From the stuff i've played with, Aluminum is a nice cover for small pyrotechnics, but not much else... i use it when making wimpy things (such as putting a pack of aluminum ophorate (i believe that is the chemical) coated sand into it. Sounds close to an M80 if you use a whole pack and tamp it tight enough...

But thats off topic, i've never used it as an anode, but from what i've seen (youtuuuube) thats all it really does in any reaction. But i don't know what the released gas is, either.

 

dude u high ???? you can do lots of things with aluminum for example with aluminum and magnesium you will be able to make magnalium and it's thanks to magnalium which provides the colored flashes from festival balls and other firework, nevermind that it is really dangerous, you do not know anything about it and i know that by reading your posts and i even doubt that you know that metal fires are hard to extinguish. go learn some chemistry.... and something about youtube most of those video's about pyrotechnics are just lies and dangerous never use it as an source and if you are going to follow their 'guides' then you deserve to get burned.

Edited November 16, 2010 by kaizoku