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greenlight
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Quote: Originally posted by ManyInterests  | Decided to bump this up since I have been working on making nitric acid again, and I am doing it using my new mantle which is being... problematic.
despite making everything as dry as possible I am ending up with azeotropic nitric acid, and nothing wants to distill under 115c. I will figure it out
with a few more experiements I am sure.
At any rate, I do almost 300ml of 70% nitric acid, how much would I need to dissolve it? I don't have the solubility of it in nitric acid.
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Are you referring to distilling a mixture of 70% nitric acid and concentrated sulphuric acid?
I used to use this method to obtain +90% red nitric to further purify thereafter into 99% white nitric.
I used double the volume of 98% sulphuric acid and just set up for standard atmospheric distillation. So for 300ml 70% nitric, I would have used
600ml 98% sulphuric acid. It is a large portion of sulphuric but it always resulted in nice yellow high purity nitric.
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
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ManyInterests
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| Quote: Originally posted by greenlight | | Quote: Originally posted by ManyInterests | Decided to bump this up since I have been working on making nitric acid again, and I am doing it using my new mantle which is being... problematic.
despite making everything as dry as possible I am ending up with azeotropic nitric acid, and nothing wants to distill under 115c. I will figure it out
with a few more experiements I am sure.
At any rate, I do almost 300ml of 70% nitric acid, how much would I need to dissolve it? I don't have the solubility of it in nitric acid.
|
Are you referring to distilling a mixture of 70% nitric acid and concentrated sulphuric acid?
I used to use this method to obtain +90% red nitric to further purify thereafter into 99% white nitric.
I used double the volume of 98% sulphuric acid and just set up for standard atmospheric distillation. So for 300ml 70% nitric, I would have used
600ml 98% sulphuric acid. It is a large portion of sulphuric but it always resulted in nice yellow high purity nitric. |
I think you did mention that to me. Though I did wonder why double the volume. Nurdrage used equal volume of sulfuric acid to nitric acid.
That being said, for purifying my RDX... how much nitric acid is needed? I will obviously do some experiments, but I'd rather get some info first
before barreling in.
[Edited on 1-7-2024 by ManyInterests]
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Sir_Gawain
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| Quote: Originally posted by ManyInterests |
That being said, for purifying my RDX... how much nitric acid is needed? I will obviously do some experiments, but I'd rather get some info first
before barreling in. |
Are you planning on purifying your RDX by recrystallization from nitric acid? Or making RDX?
By the way, you can convert yellow nitric acid to WFNA by cooling to below 0C and adding a few drops of 30% hydrogen peroxide. It works much better
than bubbling air through it.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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| Quote: Originally posted by Sir_Gawain | | Quote: Originally posted by ManyInterests |
That being said, for purifying my RDX... how much nitric acid is needed? I will obviously do some experiments, but I'd rather get some info first
before barreling in. |
Are you planning on purifying your RDX by recrystallization from nitric acid? Or making RDX?
By the way, you can convert yellow nitric acid to WFNA by cooling to below 0C and adding a few drops of 30% hydrogen peroxide. It works much better
than bubbling air through it. |
I am looking to purify the RDX I already have, thus why I am using weaker nitric acid. I assume it won't be an exothermic reaction, but I will do it
very slowly and monitor carefully anyway.
And... really? That simple? does it have to be RFNA or can such a method work with azeotropic nitric acid around 70%?
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greenlight
National Hazard
Posts: 721
Registered: 3-11-2014
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| Quote: Originally posted by ManyInterests | | Quote: Originally posted by greenlight | | Quote: Originally posted by ManyInterests | Decided to bump this up since I have been working on making nitric acid again, and I am doing it using my new mantle which is being... problematic.
despite making everything as dry as possible I am ending up with azeotropic nitric acid, and nothing wants to distill under 115c. I will figure it out
with a few more experiements I am sure.
At any rate, I do almost 300ml of 70% nitric acid, how much would I need to dissolve it? I don't have the solubility of it in nitric acid.
|
Are you referring to distilling a mixture of 70% nitric acid and concentrated sulphuric acid?
I used to use this method to obtain +90% red nitric to further purify thereafter into 99% white nitric.
I used double the volume of 98% sulphuric acid and just set up for standard atmospheric distillation. So for 300ml 70% nitric, I would have used
600ml 98% sulphuric acid. It is a large portion of sulphuric but it always resulted in nice yellow high purity nitric. |
I think you did mention that to me. Though I did wonder why double the volume. Nurdrage used equal volume of sulfuric acid to nitric acid.
That being said, for purifying my RDX... how much nitric acid is needed? I will obviously do some experiments, but I'd rather get some info first
before barreling in.
[Edited on 1-7-2024 by ManyInterests] |
I just learned that way from an old tutorial youtube video and have used it ever since and it has always resulted in quality acid so I never tweaked
it. Theoretically, the more sulphuric floating around, the more molecules available to hold onto the water to a certain extent.
Are you talking about treating already prepared RDX with another nitric acid bath? I've never heard of this. Do you believe your product isn't fully
nitrated?
The only use for an atomic bomb is to keep somebody else from using one.
George Wald
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ManyInterests
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| Quote: | | Are you talking about treating already prepared RDX with another nitric acid bath? I've never heard of this. Do you believe your product isn't fully
nitrated? |
It isn't the the issue. When you are making RDX, the final step involves heating up the nitrating mixture in order to destroy some of the impurities
within the solution. This is something that, obviously, must be done very carefully. I made two small RDX synthesis, the first one I neglected to it
as I was afraid to heat everything up, the second time I had a temperature spike that I feared was going to become a runaway, so I took the safe route
and dumped it in large quantities of water to prevent a possible disaster.
The result of this is that there are very likely impurities in the RDX that cannot be removed by recrystalizing everything in methanol or acetone. If
you read above you'll see that I was advised to bring lower concentration nitric acid (50% would work, but I used around 65%) and heat it until it
stops producing red fumes. I saw the fumes, they weren't large or out of control, after they stopped I let the mixture cool down and I crashed
everything in large quantities of water. then I filtered and washed until it was pH neutral.
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