Purifying Sodium Chlorate

[dangerousamateur]

Sodium Chlorate is one chemical I'm still lacking in my inventory.

 

Since I cannot buy pure sodium chlorate here and I just made my first little steps with the chlorate cell - why not make it myself.

 

Normally one would target potassium chlorate, where purification is quite easy, but how do I separate sodium chloride from the chlorate? It seems to be impossible to separate the two by exploiting different solubilities.

 

Is it possible to run a sodium chlorate cell until all chlorate is converted without ruining the (MMO) anode very fast?

 

 

What kind of method would you choose to get sodium chlorate as pure as possible, at least 96-98%?

Is it even possible?

Edited April 7, 2013 by dangerousamateur

[Mumbles]

I don't know why you'd really want sodium chlorate, but to each their own. It's not a particularly commonly used material due to the hygroscopic nature.

 

Fractional recrystallization should yield relatively pure material. Dissolve it in a minimum amount of boiling water, and cool to close to freezing. Sodium chloride has relatively low change in solubility over this range of temperatures. Crystallization is also natures way to purify things. Generally separate crystals will grow of the separate materials if done well. Unfortunately, several accounts I've seen state that they both crystallize in cubic morphologies, which means you can't physically separate any chloride that might crystallize out. A few crystallizations should give you analytically pure material.

[taiwanluthiers]

I think maybe he wanted to purify it to turn it into perchlorate...

[psyco_1322]

I think maybe he wanted to purify it to turn it into perchlorate...

 

Into sodium perchlorate?

Edited April 8, 2013 by psyco_1322

[Mumbles]

If your end goal is potassium chlorate it makes sense to start from potassium chloride. However, if your end goal is potassium perchlorate, some will electrolyze sodium chlorate into perchlorate first before doing a metathesis. The solubility of potassium chlorate is too low for industry. While it's feasible on a hobbyist scale, there is generally more information about sodium chlorate to sodium perchlorate around.

[dangerousamateur]

No perchlorate, just chlorate.

I really want sodium chlorate.

 

Sodium perchlorate, well, maybe sometime, but not now.

 

 

I guess I will loose much stuff by freezing out but it seems the only way. Hopefully I can recycle the discarded stuff into the cell liquor to keep losses down.

[Mumbles]

For one crystallization, you'll get a maximum of 65% recovery, but you can collect multiple crops.

[taiwanluthiers]

So what are you needing pure sodium chlorate for? It's a good percursor for things but if its to make barium chlorate the sodium still causes problem because barium chlorate is more soluble than potassium chlorate. Sodium chlorate is too hygroscopic to use in pyrotechnics.

[dangerousamateur]

Sodium chlorate is too hygroscopic to use in pyrotechnics.

Some people use even ammonium nitrate for their rockets. Bound in resin it seems to be ok.

 

So I think when stars are bound with redgum or parlon, it should be possible to use it.

[AlteredMatter]

I have a video on YouTube for making sodium chlorate if you're interested. All you need is a computer power supply, titanium, and an MMO anode. Feel free to check it out. I also discuss purification too, but it's difficult to get 100% sodium chlorate because chloride and chlorate crystallize at the same time via recrystallization, but I doubt that sodium chlorate you buy over the counter is really all that pure. https://www.youtube.com/watch?v=D_mHDkfiDa4

 

While it's not pure sodium chlorate, it will still give an ignition when mixed with sugar. Gives a brilliant yellow flame.

 

Cheers.

[SeaMonkey]

An easy way to make Sodium Nitrate non-electrolytically, is to make

dilute Nitric Acid first then use it to react with an inexpensive Sodium

Salt such as Sodium Bicarbonate (Baking Soda.)

 

There are several ways to make the Dilute Nitric Acid, one of the

easiest being the Electrical Discharge method. It is not a fast way

to make Nitric Acid but it is simple, doesn't require distillation or

mixing any chemicals or any expensive laboratory equipment.

 

Cody Reeder has made a video showing how easily it can be

done. His video demonstrates the principle and while he only

produces a tiny quantity, it is possible over a longer period to make

a sizable quantity of very pure dilute Nitric Acid.

 

Reacting this acid with Sodium Bicarbonate will produce a very pure

Sodium Nitrate which will not require any additional purification.

It will only need to be crystallized and dried.

 

A Neon Sign Transformer is not a necessity for producing the High

Voltage Arc Discharge. A small electronic circuit, an Automotive Ignition

Coil and a 12 Volt Power Supply can be used in its place.

 

Knowing how to make Nitric Acid from Air and Water is a valuable skill

which can easily be implemented by anyone, anywhere.

 

Elemental Maker has made a video where he shows how to make the

Ignition Coil Driver Board which can be used to produce the High Voltage

Discharge in the Nitric Acid Generator Device.

 

- - - - -

 

Obviously a Senior Moment here. Sodium Nitrate surely isn't the same

as Sodium Chlorate! Duh...

 

Since this is clearly not in the right place it may be moved if desired

to a more appropriate discussion.

Edited February 19, 2020 by SeaMonkey

[Crazy Swede]

So what are you needing pure sodium chlorate for? It's a good percursor for things but if its to make barium chlorate the sodium still causes problem because barium chlorate is more soluble than potassium chlorate. Sodium chlorate is too hygroscopic to use in pyrotechnics.

Actually, sodium chlorate have successfully been used in pyrotechnics, or at least in rocketry, but of course it is difficult if you live in a damp climate and have no way of controlling the indoor humidity.

 

In 1995 I was demonstrated a few sodium chlorate / polyurethane fueled shotshell rockets that were developed by Arno Hahma. (Petri Pihko brought them to Sweden to show me after the Stockholm Water Festival fireworks competitions. Those were the days...) They worked very well with impressive titanium tails and large thrust. Arno wrote an article about it called "Sodium Chlorate in Rocket Propellants" but I don't know where it was published. Discussions about this were held on the old fashioned discussion forum rec.pyrotechnics and can still be found in Internet archives like: https://yarchive.net/explosives/rocket/chlorate.html

[WSM]

I made very pure sodium chlorate about four years ago. The way I got it "pure", was to purify the sodium chloride brine before running the cell.

 

After the run was complete, the electrolyte was chilled to 0 degrees C, and the crystals began to grow on the bottom of the jar the electrolyte was chilled in.

 

The crystals are gem-like in appearance.

 

WSM

[WSM]

I made very pure sodium chlorate about four years ago. The way I got it "pure", was to purify the sodium chloride brine before running the cell.

After the run was complete, the electrolyte was chilled to 0 degrees C, and the crystals began to grow on the bottom of the jar the electrolyte was chilled in.

The crystals are gem-like in appearance.

WSM

 

 

I have to add that the reason I made the sodium chlorate is because it's not available for reasonable cost where I'm located. My purpose for making it is to continue my perchlorate production experiments, which came to a halt when my limited supply of lab-grade sodium chlorate ran out .

 

WSM

Edited March 1, 2020 by WSM

[WSM]

I made very pure sodium chlorate about four years ago. The way I got it "pure", was to purify the sodium chloride brine before running the cell.

After the run was complete, the electrolyte was chilled to 0 degrees C, and the crystals began to grow on the bottom of the jar the electrolyte was chilled in.

The crystals are gem-like in appearance.

WSM

 

 

Sodium chlorate crystals

 

WSM

Edited March 1, 2020 by WSM

[Crazy Swede]

Very nice crystals! What size are they?

[Andead]

I have managed to obtain some crystals from my sodium chlorate cell however i do not know if they are sodium chlorate of potassium chlorate. The only way to test is via flame test or the crystal structure can help identification?

[WSM]

Very nice crystals! What size are they?

 

If I remember correctly, between 9 and 19 mm on a side; most are the smaller size. These were some exceptional examples, either for size, clarity or both.

 

The drying crystals looked like a plate of gems.

 

WSM

Edited March 3, 2020 by WSM

[WSM]

I have managed to obtain some crystals from my sodium chlorate cell however i do not know if they are sodium chlorate of potassium chlorate. The only way to test is via flame test or the crystal structure can help identification?

 

The crystal structure between sodium and potassium chlorate are definitely different from each other.

 

The solubility is very different, also.

 

Comparing a Google search of both will guide you in the right direction.

 

WSM

[WSM]

The larger crystals were formed by leaving the saturated electrolyte in the 0 degrees C refrigerator longer (2-3 days, I recall).

 

WSM

Edited March 3, 2020 by WSM

[WSM]

I'll post some other photos later.

 

WSM

[WSM]

Here is a couple batches of sodium chlorate crystals, harvested from the electrolyte by chilling to 0^oC for a day or so.

 

 

 

These are from August 2016.

 

WSM

[FlipperFuego]

Thanks for the info, great thread! http://freeimagehost.info/i/MwdSPKnAcg.png

[dangerousamateur]

@Crazy Swede:

Back in 2013 I read exactly that old yarchive.net thread.

 

I even experimented with chlorate, but potassium chlorate. Bound in different kinds of curable resins.

But never got enough thrust for liftoff.

I did not pursue it any further.

 

@WSM:

But what does pure mean?

I mean, lets say I build rockets like I tried to, and there is 5% sodium chloride in there, this might be very bad for my performance. While 0,5% might be fine.

 

Or one batch is 3% but the rocket is perfectly dialed in on that. While the next has only 0,5% chloride and BOOM!! It's too good.

[WSM]

@Crazy Swede: Back in 2013 I read exactly that old yarchive.net thread. I even experimented with chlorate, but potassium chlorate. Bound in different kinds of curable resins. But never got enough thrust for liftoff. I did not pursue it any further. @WSM: But what does pure mean? I mean, lets say I build rockets like I tried to, and there is 5% sodium chloride in there, this might be very bad for my performance. While 0,5% might be fine. Or one batch is 3% but the rocket is perfectly dialed in on that. While the next has only 0,5% chloride and BOOM!! It's too good.

 

 

As far as oxidizers, I'm using MIL-SPEC standards for a reference: KClO₃ 99.5%, and KClO₄ 99.0%, if I remember correctly.

 

If we go to extra effort in preparing our precursors and are careful in our processes, we can exceed these standards and make higher purity oxidizers.

 

I've been studying this out and have a few ideas to test in proving my thoughts about it. I'll post the results here, when I have them.

 

As far as water is concerned, My recommendation for "pure" water, refers to either distilled water or deionized water.

 

WSM