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ManyInterests
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Yeah. I downloaded all the pages off that site (most of them anyway). I am doing my second run of chlorate as I mentioned.
My first run had some mild discoloration, but it isn't too bad and I think my product is reasonably pure. I did a burn test with some sugar and it
burned in its entirety, leaving only a black lump (the sugar burning?) that is easily crushed.
I still haven't weighted the end product, but I will shortly. It is a good amount, but I want a few hundred grams more just to make sure I have enough
for all my purposes... which as stated above is turning it into sodium perchlorate and then turning that into ammonium perchlorate.
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ManyInterests
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OK a bit of an update after some weeks. I did finally dry my initial product and I got around 211 grams (I did burn around 7 or 8 grams as a test
before weighing) and I am not entirely sure on the purity, but it did burn fairly well. I have some documents on purification of chlorates that I will
need to follow with this batch.
I did start a batch almost two weeks ago and it has been running at around 17.5 amps for almost 312 hours. So assuming a 50% efficiency I would
generated 982.8 grams of chlorate.
Which is impossible because my starting liquid had 420 grams of sodium chloride to 950 ml or so of distilled water. I think I should halt my
electrolysis right now since I don't think it can make any more chlorates.
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Mateo_swe
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Im also planning on making some chlorate and later some perchlorate.
I have ordered a MMO and titanium set for the chlorate cell and a platinum and titanium set for the perchlorate cell.
Im a bit unsure if i should add some dicromate to increase the efficiancy of the cell and protect the electrodes. I read the effects are quite good.
I have both potassium and sodium dichromate but as these are quite toxic i want to separate them from the chlorate/perchlorate and im not exactly sure
on how to do this.
Would some simple recrystallization remove the dicromates from the chlorate/perchlorates?
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DocX
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Yes. Dichromates are very water soluble (which is one of the reasons they are so toxic and environmentally baaad, mkey?), whereas potassium chlorate's
not. You can easily recrystallise the chlorates from warm water into snow white, beautiful crystals.
Also, it's good to have a technique for good pH control. I used a simple dripping setup with dilute HCl.
You can check out this thread I made during my first chlorate cell trials and tribulations: https://www.sciencemadness.org/whisper/viewthread.php?tid=74...
If nothing else, there's plenty of excellent links to external sources of wisdom and knowledge in there.
[Edited on 20222222/6/19 by DocX]
[Edited on 20222222/6/19 by DocX]
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ManyInterests
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So as a final note on my sodium chlorate.
I had two sub-batches in my 2nd run. The first one had a reasonable percentage of chlorate to (possible) chloride as it burned well when I added sugar
to a bit of it.
The second sub-batch was... oh la la! Beautiful! Mostly very pure sodium chlorate as when I added the 50/50 sugar mixture and burned it, it burned
VERY quickly and very viscously! I kept all the batches separated as while I will be working on turning them all into perchlorate, I want to save the
best batches separately.
My first perchlorate run will involve the first bit of sodium chlorate I made, with the off-color metal bits in it. I don't think it'll cause a
problem with my crucible.
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Mateo_swe
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Regarding the added dichromates, i maybe have to find a way to precipitate them and filter to clean the sodium chlorate as just a recrystallize may
not get rid of them.
Sodium chlorate is very water soluble and dichromates are also very water soluble so water recrystallation might not work here (compared to potassium
chlorate that are less soluble in water).
Strangely i havent found any info on it when making sodium chlorate in a cell.
Many places say i can add sodium/potassium dichromate but very few tell how to get rid of them in the workup.
And i must get rid of it from the sodium chlorate as it´s both toxic and could cause unwanted (maybe dangerous) effects when using the chorates for
fireworks.
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Herr Haber
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I was recently reminded that potassium dichromate is used to coat magnesium in fireworks so maybe that's not so big of an issue ?
Though I can only praise your efforts to avoid putting chromium in the environment the % in your final product, even if everything comes along
shouldnt be more than .2 or 1% right ?
It it really worth all your trouble ?
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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B(a)P
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Quote: Originally posted by Mateo_swe  | Regarding the added dichromates, i maybe have to find a way to precipitate them and filter to clean the sodium chlorate as just a recrystallize may
not get rid of them.
Sodium chlorate is very water soluble and dichromates are also very water soluble so water recrystallation might not work here (compared to potassium
chlorate that are less soluble in water).
Strangely i havent found any info on it when making sodium chlorate in a cell.
Many places say i can add sodium/potassium dichromate but very few tell how to get rid of them in the workup.
And i must get rid of it from the sodium chlorate as it´s both toxic and could cause unwanted (maybe dangerous) effects when using the chorates for
fireworks. |
Add a little barium chloride. Barium chromate is not very soluble.
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ManyInterests
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Might as well turn this thread into my 'perchlorate synthesis' thread.
So remember the first batch of sodium chlorate I made? I guess even the 'mild' contamination probably had a very determinental effect on my
perchlorate attempt. I will need to go straight to the good stuff 2nd time around and stop wasting time.
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B(a)P
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| Quote: Originally posted by ManyInterests | Might as well turn this thread into my 'perchlorate synthesis' thread.
So remember the first batch of sodium chlorate I made? I guess even the 'mild' contamination probably had a very determinental effect on my
perchlorate attempt. I will need to go straight to the good stuff 2nd time around and stop wasting time. |
As per my post in the other thread you are posting in, I don't think the contamination is the issue, you are just not getting hot enough for the
reaction to occur.
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ManyInterests
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OK so I got a propane torch and so far it's been almost thirty minutes on the flame. Here is what my setup looks like.
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ManyInterests
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So quick update It seems like it is workign to reduce the volume of chlorate powder I see in there. It hasn't turned into a slurry yet, but I think
with another hour or so it might. It is around half as high as it was. The only thing is that the flame is hitting the crucible on the side instead of
dead bottom. I don't currently have a setup that would allow me to put the crucible directly below it.
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Rainwater
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| Quote: Originally posted by ManyInterests |
looked up what the colors meant for a 3-pronged US power cable (green is neutral, white is live, and black is ground) and I wired it up.
[Edited on 21-5-2022 by ManyInterests] |
Green - ground
White - netural
Black - hot
And when working around liquids, please consider using a gfci power source.
Maybe i missed it but what size electrodes are you using.
A smaller cathode will help reduce side reactions.
As for amps per volume. Ive never heard of that, its usual amps per cm³ of electrode area.
"You can't do that" - challenge accepted
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B(a)P
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If you have a glass stirring rod give it a stir to see if your chlorate has melted. You want it to be fully melted and bubbling to show you that the
decomposition of chlorate is occurring. Have you watched this? It is a pretty detailed description of the procedure.
https://www.youtube.com/watch?v=leexFE_zXe4&t=508s
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ManyInterests
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I don't have a glass stirring rod right now, I am using a butter knife to stir. I see do see it reducing. it hasn't fully melted though.
I did see Chemplayer's video a while ago. Maybe the single torch is insufficient? Or maybe it needs more time. It's been more than 3 hours, I do see
some progress. I will keep it for however long it needs to be.
But I think in order to get perchlorates I will just invest in a platinum electrode. I found a source for it that I wish I found before I made my
sodium chlorate. If I could sodium perchlorate directly it would have saved me a ton of trouble.
edit: I need to mention that when I say it hasn't fully melted meaning I don't see any melting. Some of them look like they might have melted until I
stirred since they formed hard chunks.
Edit2: I have a feeling this might not work. If it doesn't then I am not going to spend any more money on buying equipment to turn my chlorate into
perchlorate using thermal decomposition. I just ordered a platinum electrode (it wasn't too expensive thankfully) and I hope to use that to make
sodium perchlorate.
[Edited on 27-6-2022 by ManyInterests]
[Edited on 27-6-2022 by ManyInterests]
[Edited on 27-6-2022 by ManyInterests]
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B(a)P
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I see no reason why it would not work with what you have, I have successfully done this a number of times with similar equipment. Do you have the
torch positioned to get the most heat out of the flame? The flame from your torch would consist of and outer dull blue flame and an inner bright blue
flame. You want the tip of the inner blue flame to be just about touching the point you are trying to apply heat.
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ManyInterests
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Actually I am not really sure. I altered the setup twice, the first time the flae was hitting more in the lower-middle part of the crucible (with the
wall on the crucible turning red. Both on the inside and the outside) where the flame was hitting.
Then I changed my setup to make the flame hit the lower part more since I thought that would be better... but right after reading your post, I decided
to press the nozzle against the crucible as pictured (I had to turn off al lights and use flash to note the color of the flames).
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ManyInterests
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Maybe it is working? But maybe what I did before was wrong? What I would do is rotate the crucible and let the heat go on at different places? Maybe
that was a mistake?
I think I'll leave it heating one spot no matter what.
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ManyInterests
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OK this didn't work. Period point paragraph. I kept the heat and direct flame on it for more than 4 hours at least and exactly nothing. I rinsed it in
heated acetone (sodium perchlorate is soluble in acetone) but after boiling off the acetone I got exactly nothing.
I threw away the old chlorates I used and got 30 grams of my purest sodium chlorate. I turned the torch back on and I will keep the heat until the gas
runs out. Which shouldn't take long since the tank was considerably lighter than when I started.
I wish I ordered the anode first. It would have cost only a little more than the torch...
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markx
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As far as I understand one needs a certain temperature range to be kept in order to decompose chlorates into perchlorates. So an open flame approach
perhaps is not the most efficient way to proceed. An electrical furnace with PID control might offer a more controlled way of doing it. Also the
chlorate needs to be quite pure and free of metallic contaminants as many of those act as catalysts and the decomposition yields only chlorides then.
Exact science is a figment of imagination.......
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