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jessjabb
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New to energetic materials, need advice
I am new to this site and the manufacture of energetic materials. I have successfully synthesized silver acetylide primary and have the materials for
ANFO what secondaries would you more experienced members suggest I make. I tried making PETN to no avail with just 67% nitric acid. Any help would be
greatly appreciated.
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FeedMe94
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If you have Pentaerythritol stay with it and synth some PETN. Even with 67% Nitric Acid you will be fine. There are many posts in this forum about
PETN synthesis
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twelti
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Search around here for a file called "PETN.XLS" or maybe "PETN2.XLS". It will allow you to tweak your proportions to optimize the nitration. I
recently had similar experience where I thought the PETN was not working but it was, it is just not as sensitive as you might think. I could only
really get it to go off under a hammer, on sand paper. Try that. Or of course with a nice primary. you said you have SADS. That should work.
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caterpillar
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Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid.
Women are more perilous sometimes, than any hi explosive.
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twelti
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Quote: Originally posted by caterpillar  | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
There seems to be some difference of opinion on this matter around here. I think most people agree that using concentrated nitric acid is better, but
I think lower concentration should also work. As for example in Urbanski nitration tables (which the PETN.XLS is based on). I have done it. My only
question is whether maybe I got the di-penta version, which is also explosive.
Regarding the phosphorous pentoxide, can you give me a reference or more detail on that. I have looked around and not able to find a method using it.
I have a source for inexpensive P2O5. I would love to try that. Doesn't P2O5 have some handling issues? Sucks up water out of the air and turns
into phosphoric acid, right?
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jessjabb
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Thank you guys for the advice! ill try to keep you updated
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jessjabb
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| Quote: Originally posted by caterpillar | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
Ok do you think I could dissolve Ammonium Nitrate into the acid? I also have potassium nitrate. When I attempted to synth PETN the first couple times
the PE would dissolve completely into the NA ( I didn't use sulfuric acid) creating a crystal clear fluid that would just decompose into nitrogen
dioxide and smoke up my garage with orange vapor. Do I need sulfuric or can I synth PETN without it?
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Microtek
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Using 67% nitric acid alone will not work properly, but either nitric acid of 95% or more OR 67% nitric plus a suitable amount of
concentrated sulfuric acid to bind the water in the nitric will be fine.
If you have P2O5 you can use that for dehydrating your nitric acid either in situ (like you would do with sulfuric acid) or in preparation
for distillation, but you could also use it for a very efficient synthesis of HMX (for this you also need a slight amount of acetic anhydride though).
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caterpillar
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| Quote: Originally posted by twelti | | Quote: Originally posted by caterpillar | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
There seems to be some difference of opinion on this matter around here. I think most people agree that using concentrated nitric acid is better, but
I think lower concentration should also work. As for example in Urbanski nitration tables (which the PETN.XLS is based on). I have done it. My only
question is whether maybe I got the di-penta version, which is also explosive.
Using weak acid, you'll definitely get not tetranitrate but di-or trinitrate. If you have P2O5 you can use it for many interesting things. In your
case, you need to bind water in weak nitric acid. Make a simple calculation- how much you need add to get 98-100 percent acid. Add pentoxide in small
portions and do not let temp be hi.
Regarding the phosphorous pentoxide, can you give me a reference or more detail on that. I have looked around and not able to find a method using it.
I have a source for inexpensive P2O5. I would love to try that. Doesn't P2O5 have some handling issues? Sucks up water out of the air and turns
into phosphoric acid, right?
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Women are more perilous sometimes, than any hi explosive.
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caterpillar
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| Quote: Originally posted by jessjabb | | Quote: Originally posted by caterpillar | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
Ok do you think I could dissolve Ammonium Nitrate into the acid? I also have potassium nitrate. When I attempted to synth PETN the first couple times
the PE would dissolve completely into the NA ( I didn't use sulfuric acid) creating a crystal clear fluid that would just decompose into nitrogen
dioxide and smoke up my garage with orange vapor. Do I need sulfuric or can I synth PETN without it? |
Of course, I ment solution of some nitrate in sulfur acid. maybe, NH4NO3 is better due to its better solubility in sulfuric acid. And keep temp below
20 Celsius. I could recommend this: Jai_Prakash_Agrawal,_Robert_Hodgson-Organic_Chemistry_of_Explosives-Wiley(2007) The last part described nitration
with N2O5- you may try some methods, dissolving P2O5 in nitric acid.
Women are more perilous sometimes, than any hi explosive.
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jessjabb
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| Quote: Originally posted by caterpillar | | Quote: Originally posted by jessjabb | | Quote: Originally posted by caterpillar | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
Ok do you think I could dissolve Ammonium Nitrate into the acid? I also have potassium nitrate. When I attempted to synth PETN the first couple times
the PE would dissolve completely into the NA ( I didn't use sulfuric acid) creating a crystal clear fluid that would just decompose into nitrogen
dioxide and smoke up my garage with orange vapor. Do I need sulfuric or can I synth PETN without it? |
Of course, I ment solution of some nitrate in sulfur acid. maybe, NH4NO3 is better due to its better solubility in sulfuric acid. And keep temp below
20 Celsius. I could recommend this: Jai_Prakash_Agrawal,_Robert_Hodgson-Organic_Chemistry_of_Explosives-Wiley(2007) The last part described nitration
with N2O5- you may try some methods, dissolving P2O5 in nitric acid. |
Ok Ill pick up a bit of sulfuric acid, because I have done the flask in cooling water method with just nitric acid and it does not work.
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twelti
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I thought the lower nitrates of PETN were soluble in water, thus would not survive recrystalization?
As for P2O5, I thought that was used in distillation of NA, not direct nitration. If you still have to distill it, is there any advantage of the P2O5
over other approaches?
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caterpillar
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| Quote: Originally posted by twelti | I thought the lower nitrates of PETN were soluble in water, thus would not survive recrystalization?
As for P2O5, I thought that was used in distillation of NA, not direct nitration. If you still have to distill it, is there any advantage of the P2O5
over other approaches? |
No, you do not need to perform distillation- only add P2O5 to bind excess of water. If you wanna get concentrated HNO3, use some nitrate (K or Na) and
sulfur acid. You may use some simple apparatus like a coffee pot- steel doesn't react with conc HNO3. Use diluted HNO3 to make styphnic acid of
hexamine dinitrate or urea nitrate. Last ones are useful precursors to something more interesting.
Women are more perilous sometimes, than any hi explosive.
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twelti
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| Quote: Originally posted by caterpillar | | Quote: Originally posted by twelti | I thought the lower nitrates of PETN were soluble in water, thus would not survive recrystalization?
As for P2O5, I thought that was used in distillation of NA, not direct nitration. If you still have to distill it, is there any advantage of the P2O5
over other approaches? |
No, you do not need to perform distillation- only add P2O5 to bind excess of water. If you wanna get concentrated HNO3, use some nitrate (K or Na) and
sulfur acid. You may use some simple apparatus like a coffee pot- steel doesn't react with conc HNO3. Use diluted HNO3 to make styphnic acid of
hexamine dinitrate or urea nitrate. Last ones are useful precursors to something more interesting. |
I don't mean to be dense, but can you point me to a synthesis where I can just add P2O5 to 70% HNO3 and nitrate to RDX? I would much rather do that
than make WFNA, but I have not been able to find such a procedure.
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Simoski
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Make ETN, just need erythritol, nitric, sulphuric and ethanol.
I made mine with 50% nitric no problem.
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caterpillar
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| Quote: Originally posted by twelti | | Quote: Originally posted by caterpillar | | Quote: Originally posted by twelti | I thought the lower nitrates of PETN were soluble in water, thus would not survive recrystalization?
As for P2O5, I thought that was used in distillation of NA, not direct nitration. If you still have to distill it, is there any advantage of the P2O5
over other approaches? |
No, you do not need to perform distillation- only add P2O5 to bind excess of water. If you wanna get concentrated HNO3, use some nitrate (K or Na) and
sulfur acid. You may use some simple apparatus like a coffee pot- steel doesn't react with conc HNO3. Use diluted HNO3 to make styphnic acid of
hexamine dinitrate or urea nitrate. Last ones are useful precursors to something more interesting. |
I don't mean to be dense, but can you point me to a synthesis where I can just add P2O5 to 70% HNO3 and nitrate to RDX? I would much rather do that
than make WFNA, but I have not been able to find such a procedure. |
Try yourself. Add P2O5 to your HNO3 and cool the mix. make hexamine dinitrate, using diluted HNO3. Normally to perform nitrolysis of hexamine one has
to use a large amount of nitric acid- 1: 10. If you use dinitrate, you may calculate the equivalent amount of dinitrate. Read Agrawal and Hodgson.
Women are more perilous sometimes, than any hi explosive.
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twelti
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Which method are you talking about?
From Agrawal and Hodgson:
The extreme sensitivity of (238) to
hydrolysis means that nitrolysis has to be conducted under anhydrous conditions using sulfur
trioxide or phosphorous pentoxide dissolved in fuming nitric acid.
Still fuming nitric acid.
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jessjabb
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| Quote: Originally posted by twelti | Which method are you talking about?
From Agrawal and Hodgson:
The extreme sensitivity of (238) to
hydrolysis means that nitrolysis has to be conducted under anhydrous conditions using sulfur
trioxide or phosphorous pentoxide dissolved in fuming nitric acid.
Still fuming nitric acid. |
I am doing it in this method http://www.powerlabs.org/chemlabs/petn.html
I will do smaller scale, like a half batch with only 5g or 2.5g to get to know the reaction a little better.
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twelti
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That is basically the same method I used. I'm going to just bit the bullet and make some fuming nitric acid. After the last couple of experiments,
I'm not really convinced I did get PETN after all. I'm going to make it with fuming nitric acid and compare.
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caterpillar
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| Quote: Originally posted by twelti | Which method are you talking about?
From Agrawal and Hodgson:
The extreme sensitivity of (238) to
hydrolysis means that nitrolysis has to be conducted under anhydrous conditions using sulfur
trioxide or phosphorous pentoxide dissolved in fuming nitric acid.
Still fuming nitric acid. |
Not this. Or you have (238- known as White Salt)? In such a case, you may try it. But if you have not (238), use the first method- hexamine + fuming
nitric acid. I only recommend to use not the pure hexamine but its dinitrate. Again- make conc nitric acid, adding P2O5 to diluted nitric acid. Add
slowly hexamine dinitrate. Any problem with calculations of necessary amounts of chems?
Women are more perilous sometimes, than any hi explosive.
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twelti
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I think we are going around in a circle. Regarding the use of 70% NA, you said:
"Or add some phosphorous pentoxide to your weak acid"
It sounded as if you were saying the synth could be done using the weaker acid, by adding the P2O5. From your other comments and from the source you
cited, it looks like the weaker acid won't work.
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caterpillar
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| Quote: Originally posted by twelti | I think we are going around in a circle. Regarding the use of 70% NA, you said:
"Or add some phosphorous pentoxide to your weak acid"
It sounded as if you were saying the synth could be done using the weaker acid, by adding the P2O5. From your other comments and from the source you
cited, it looks like the weaker acid won't work.
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??? Sorry? When the appropriate amount of P2O5 has been added to weal (63-67%) HNO3, it becomes STRONG. Excess of water is bind and you have HNO3 +
H3PO4. So simple.
Women are more perilous sometimes, than any hi explosive.
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MineMan
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I have two dueling pistols. The only catch is they must be filled with an energetic you made.
Catapiller. I personally would fill it with NiAGP and AP for gas generation.
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jessjabb
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| Quote: Originally posted by jessjabb | | Quote: Originally posted by caterpillar | | Quote: Originally posted by jessjabb | | Quote: Originally posted by caterpillar | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
Ok do you think I could dissolve Ammonium Nitrate into the acid? I also have potassium nitrate. When I attempted to synth PETN the first couple times
the PE would dissolve completely into the NA ( I didn't use sulfuric acid) creating a crystal clear fluid that would just decompose into nitrogen
dioxide and smoke up my garage with orange vapor. Do I need sulfuric or can I synth PETN without it? |
Of course, I ment solution of some nitrate in sulfur acid. maybe, NH4NO3 is better due to its better solubility in sulfuric acid. And keep temp below
20 Celsius. I could recommend this: Jai_Prakash_Agrawal,_Robert_Hodgson-Organic_Chemistry_of_Explosives-Wiley(2007) The last part described nitration
with N2O5- you may try some methods, dissolving P2O5 in nitric acid. |
Ok Ill pick up a bit of sulfuric acid, because I have done the flask in cooling water method with just nitric acid and it does not work.
|
Alright I synthesized something that I believe is PETN. I did a small test run and ended up with a fine powder, then I did full scale with 10g of PE,
I filtered off the precipitate and dissolved the powder in acetone after it dried, I diluted the acetone and sand like crystals precipitated out. I am
currently in the process of drying said crystals. How would you recommend I test it?
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caterpillar
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| Quote: Originally posted by jessjabb | | Quote: Originally posted by jessjabb | | Quote: Originally posted by caterpillar | | Quote: Originally posted by jessjabb | | Quote: Originally posted by caterpillar | | Your acid is definitely too weak. Make conc acid- it is not a great problem. Stainless steel vessel is good for distillation. Or try to use some
nitrate, dissolved in H2SO4. Or add some phosphorous pentoxide to your weak acid. |
Ok do you think I could dissolve Ammonium Nitrate into the acid? I also have potassium nitrate. When I attempted to synth PETN the first couple times
the PE would dissolve completely into the NA ( I didn't use sulfuric acid) creating a crystal clear fluid that would just decompose into nitrogen
dioxide and smoke up my garage with orange vapor. Do I need sulfuric or can I synth PETN without it? |
Of course, I ment solution of some nitrate in sulfur acid. maybe, NH4NO3 is better due to its better solubility in sulfuric acid. And keep temp below
20 Celsius. I could recommend this: Jai_Prakash_Agrawal,_Robert_Hodgson-Organic_Chemistry_of_Explosives-Wiley(2007) The last part described nitration
with N2O5- you may try some methods, dissolving P2O5 in nitric acid. |
Ok Ill pick up a bit of sulfuric acid, because I have done the flask in cooling water method with just nitric acid and it does not work.
|
Alright I synthesized something that I believe is PETN. I did a small test run and ended up with a fine powder, then I did full scale with 10g of PE,
I filtered off the precipitate and dissolved the powder in acetone after it dried, I diluted the acetone and sand like crystals precipitated out. I am
currently in the process of drying said crystals. How would you recommend I test it? |
Wrap small amount ( 0.2-0.5 gr ) in tinfoil, put it onto a steel plate and strike with a hammer.
Women are more perilous sometimes, than any hi explosive.
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