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making potassium (per) chlorate


gods knight

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IIRC nitrate is "MADE" by reacting nitrogen and hydrogen at about 400c and 250bar and making ammonia (toxic and worse!) then oxidising the product to NOx and reacting that to give nitrates. Many difficult bits of chem eng -the chemistry is simple but the high temp and pressures make problems.

 

Nitrate can be found in fertilisers and may possible be suitable for purification by recrystallisation etc.

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To put it into perspective... your average compressor tank are rated to 10 bars (basically around 150 psi), 16 bars tested maximum (about 200 psi). 2 stage compressors are rated at 16 bars, and the tank is rated to obviously 20 bars...

 

So I hate to think what 250 bar is, that's like 3000 psi or something, and at elevated temperature too. What tank could possibly hold that kind of pressure without exploding (you don't want to be around if it does!)?

 

I think for the average hobbyist it is much easier to make nitrates from stale manure like they do in the old days... or use mined Chilean saltpeter (sodium nitrate).

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Make a birkeland-eyde generator and produce nitric acid from the air and with water. I'd like to see them take those two away :D .

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Make a birkeland-eyde generator and produce nitric acid from the air and with water. I'd like to see them take those two away :D .

 

In this case it's not the starting materials, it's the equipment and power :wacko: !!!

 

WSM B)

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TaiwanLuthier, have you ever considered just looking this stuff up. What you want is called the Ostwald process, and has nothing to do with perchlorate production, so quit taking it further off topic.

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The December/January PGI Bulletin arrived yesterday which has the second part of my "homegrown oxidizers" series in it. Anyone here Who's a current PGI member, please comment on it. I'm looking for constructive criticism or suggestions. Thanks.

 

WSM B)

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Hi All,

 

I'm writing part 3 of my series on Homegrown Oxidizers and I'm wondering what others do. My questions are these:

Do you operate you cell indoors or outdoors?

If indoors, what precautions or safety measures do you take?

If outdoors, how do you protect your system?

 

Please answer in the forum so all may benefit. If you prefer not to answer in the forum, please PM me with your answers.

 

Thank you for your help.

 

WSM B)

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I personally have chosen the indoor (garage) setup. Mainly for the reasons : it is easier to monitor, keeps it out of the heat,and the system is visually protected from naive eyes who would report you to the authorities. The Sys needs to be placed into a catch pan ( concrete tub etc) to catch the liquor if you had a bucket failure . Leaks are to be dealt with quickly as they can have collateral damage on ones tools or personal items in the storage area. The electronics should be mounted away from the cell to avoid damage if a leak happened. All your salt , supplies, wash station , and tools can be close to access in a indoor setup v.s. outdoors.

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  • 2 weeks later...

Sorry, I just find that reference just ill made. Not much information or a question about making chlorates.......Pat

P.S. neither is this reply. :wacko:

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  • 4 weeks later...

One question concerning the obviously popular MMO anodes from that laserdude on ebay:

 

If one used them in a typical hobbyist setup - no PH regulation and running the cell until most chloride is converted - how long can you torture these until the coating is gone?

 

How many of these anodes did you guys use up in the past?

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If the chloride drops below 50g/l depending on your voltage and amperes flowing you will typical have about three days until total failure. A better analysis of the behavior is given on the geocities site.
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The best approach is to pull the plug and wash the electrodes. Pull the chlorate out,and recharge the cell when the Amp draw nears the half way point (from start up Amp draw. ) I use the lazzered mmo, and have abused the hell out of them . The chloride level is never allowed to drop too low , or damage will occur. Fluorine and a few other things cause failure to the coating of the mmo. I experienced this with city tap water.

Edited by pyrojig
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So my initial idea to purify the chlorate just by letting the cell run very long seems to be a bad one ;)

 

 

But please give me an idea how many anodes you use up per, lets say 10kg of chlorate.

I ask because I want to save some for a rainy day, in case they wont be available all time. Just to get an idea how big a lifelong supply has to be ;)

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If you treat them propper, you will be able to make 100kg and more from one anode of a normal size.

 

What type of chlorate do you wan't to make? For pottasium chlorate, don't think a lot about purification. Prepare the chlorate straight from KCl, filtrate it hot once and recrystallize it.

Use silver nitrate to test for chloride, most times you will be chloride feee after the first recrystallisation

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If you follow Swedes blog , it is not really necessary to recrystallize the chlorate for most pyro use, as a cold wash (32*f or less) of distilled water will wash off most all clinging chlorides .

@ Mabuse :Size of electrode, or how many , is not based off the material produced . As said above , if the electrodes are kept clean and free from tap water impurities (or left in the liqueur w/o power on), they should last an amazingly long time.


* I use a MMO anode with 2 cathodes , one on ea side to maximize the surface area working for you.

Edited by pyrojig
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Is there any MMO anode supplier in Europe, I can see just one seller on ebay in US. I messaged Swede, but it looks like he is not reading this forum any more.

I found one seller in UK, but the price was just unreasonable.

Edited by ivars21
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Is there any MMO anode supplier in Europe, I can see just one seller on ebay in US. I messaged Swede, but it looks like he is not reading this forum any more.

I found one seller in UK, but the price was just unreasonable.

 

I believe DeNora is based in Italy and they make a superior product (they also have offices in the USA). If you contact them, ask for several distributers in your area so you can shop for the best price (or maybe they can supply you with a sample?! ;) ).

 

Good hunting.

 

WSM B)

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  • 2 weeks later...

I've submitted Part Three of my series on Homegrown Oxidizers for publication in the PGI Bulletin. Watch for it to come out sometime in March.

 

WSM B)

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Awesome!!! glad to see your making progress. If Swede where here, he would be proud to see you take it to the next step. So much to learn , and so much more yet to be learned.

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Awesome!!! glad to see your making progress. If Swede where here, he would be proud to see you take it to the next step. So much to learn , and so much more yet to be learned.

 

Thanks pyrojig.

 

Now, besides wrting these articles, I need to post them as blogs here at APC so everyone can see and critique them (we're all learning as we go, aren't we?!! ;)).

 

WSM B)

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Hey guys, just wanted to get your opinion.

I resently made a ClO3- cell, with a MMO anode and a titanium cathode, my power supply is an ATX 5v 36 amp. The cell itself can hold up to 1.5 liters.

So i just tested it, made a 1.5 liters KCl 300g solution, filtered it, and ran it for exactly 24 hours before i turned it off to see my yield and seems like i have made just about 35 grams.

Is this okay, or should i be producing more than this?

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Hey guys, just wanted to get your opinion.

I resently made a ClO3- cell, with a MMO anode and a titanium cathode, my power supply is an ATX 5v 36 amp. The cell itself can hold up to 1.5 liters.

So i just tested it, made a 1.5 liters KCl 300g solution, filtered it, and ran it for exactly 24 hours before i turned it off to see my yield and seems like i have made just about 35 grams.

Is this okay, or should i be producing more than this?

Hi renaxi,

 

It's useful to track the current consumption (with an ammeter and shunt) and temperature of the cell liquor to monitor how the system is working. If you track the current level, shutting the power off when it drops to roughly half the peak level is a good practice.

 

Also, when measuring the yield, don't forget the amount of dissolved chlorate left in solution which can be approximated depending on the temperature of the liquor.

I don't think that twenty four hours is even close to enough time to get any kind of a decent yield. Also, the first run of the system spends most of its energy making the precursors of chlorate. Subsequent runs with recharged electrolyte will produc a LOT mor chlorate and quickly at the start of the run.

 

Welcome to the discussion.

 

WSM B)

Edited by WSM
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Hi renaxi,

 

It's useful to track the current consumption (with an ammeter and shunt) and temperature of the cell liquor to monitor how the system is working. If you track the current level, shutting the power off when it drops to roughly half the peak level is a good practice.

 

Also, when measuring the yield, don't forget the amount of dissolved chlorate left in solution which can be approximated depending on the temperature of the liquor.

 

I don't think that twenty four hours is even close to enough time to get any kind of a decent yield. Also, the first run of the system spends most of its energy making the precursors of chlorate. Subsequent runs with recharged electrolyte will produc a LOT mor chlorate and quickly at the start of the run.

 

Welcome to the discussion.

 

WSM

Thanks for the fast responding.

 

My liquor runs at about 80 degrees celcius at daytime and don't know about the night time. But i'll have to invest in a ampmeter, that can take so high current (36 amp), as my current meters fuse would burn over at 20 amps.

,

When i extracted the yield from the liquor, i cooled it down in a icebath, so it was roughly 5 dregrees, and then filtered the liquor twice as i saw there was formed new crystals in the filtered liquor.

 

Also the build of my cell, the distance between the anode and the cathode, are 15 mm, is this correct or could i improve here? My liquor container is a closed system with a tube in the lid, running down into some water. Will this water filter out some of the chlorine gas or have i been miss informed?

 

Renaxi

 

Edited by renaxi
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