Grantr
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looking for advise
I want to make a high explosive. I am looking for advise on the best compounds to start with. I want something easy to make that does not have to
have nitric acid to synthesize. I want it to have a high vod and be safe to handle. No peroxides for me!
I know nitric acid is the best way to nitrate chemicals however the stuff is very expensive online and probably expensive to ship. I can get farm
grade AN 34-0-0 really cheap. i have seen reference to using this in place of nitric acid for some synthesis.
The compounds I am interested in are ETN, MHN, and EGDN.
ETN is my favorite so far. I have seen a few videos on how to make it and various test videos. i also like that it is stable in storage. It seems to
be easy to make and not to sensitive. I have seen videos of it being used as blasting caps. The videos had it wrapped in aluminum foil then lit with a
fuse. If that works well that would make the whole process easier since i would not have to make another substance for a primary.
As far as primarys go I have no idea which compound would be easy to make and be relatively safe. I want it fuse sensitive and able to set off the
secondarys i mentioned above or ones you may suggest.
Silver acetylide seems to be about as easy as it gets however Silver nitrate is very expensive.
Any information and or advise would be great.
Thanks
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Detonationology
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You've pretty much eliminated the safer end of spectrum of explosives by not working with HNO3. ETN is probably the most stable, shock and friction
insensitive compound listed here; however, you mentioned that you didn't want to have to use HNO3, which would be necessary to nitrate the erythritol.
I am very happy to hear that you do not wish to work with organic peroxides, because rarely are those compounds treated with the respect they
deserve. You say a high vod: how high? If 2200m/s is good, stick with Tannerite. Anything with a much higher velocity is probably either a nitrate
or a peroxide. When it comes to explosives, one must decide whether safety or accessibility is valued more, IMO.
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Grantr
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So is HNO3 basically needed to nitrate chemicals? I want a VOD in the TNT and up range. That was one reason I like the ETN. What is the safer end of
the spectrum? I though ETN could be made without HNO3. I saw this post on this forum:
| Quote: |
The synthesis I use:
1). 240 grams of Ammonium Nitrate is slowly added to 175 mL Conc. Sulfuric Acid while keeping
the temp below 25 Celsius. (Note: I use a LOT of ice around the reaction beaker sides and bottom, with only a little water to fill.)
2). 75 grams of Erythritol is slowly added to the acid/nitrate mix while keeping the temp
10-15. This is stirred vigorously.
3). While still keeping the temp between 10 and 15 degrees Celsius, 330 mL Sulfuric Acid
is added while stirring vigorously
4). This is allowed to react for 30 minutes, then crashed into 4 liters of ice water and
filtered
(IF the synth works, I then recrystallize the ETN via Ethanol)
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I also saw this:
| Quote: |
I made a research here on this forum and i found somebody that had a very good yields of ~45-50g of ETN for every 35g of Erythritol
200 ml sulfuric acid
110g Ammonium Nitrate
35g Erythritol
So you can give it a try...
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Is there a reason not to use the nitrate salt method?
Does the HNO3 have to be highly concentrated to work? I saw a 2.5 liter bottle of 70% for $110 on Amazon plus $27 shipping.
I saw a few videos how to make HNO3 with a nitrate salt, water, hydrochloric acid and copper. Would this weak form work ok to make ETN?
Thanks,
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Bert
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Detonationology said:
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you mentioned that you didn't want to have to use HNO3, which would be necessary to nitrate the erythritol.
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I never bothered to use nitric acid when making ETN. Quite a few others here also used the various nitrate salts & sulfuric acid method.
This goes into beginnings until and unless OP cares to post his list of references. Then it possibly might get merged into an existing ETN thread...
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Bert
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Thread Moved
20-9-2015 at 17:10 |
Detonationology
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Sorry for not understanding in the beginning, sometimes I read things too quickly and I was under that impression that any nitric acid (concentrated
or crude) was out of the question. I prefer purer reagents when nitrating to avoid the formation of metal sulfate chunks, which can be difficult to
differentiate from the desired product. I'm not too keen on filtering acid because it will more than likely to make a mess. It really isn't
difficult to go the extra step and make fairly concentrated HNO3. ETN make great salutes; it gives a very sharp and loud report, which seems very desirable. There
is always PETN, which I have never tried, but is similar to ETN. I know it's harder to acquire than erythritol (which can be found in Truvia brand
sweetener). RDX is always a possibility; however, lately I hear of many on the forum experiencing issues with carrying the nitration to completion
using crude nitrating mix.
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Bot0nist
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Using a nitrate salt and concentrated sulfuric acid mix works just fine to prepare ETN. Follow an established procedure (quicksilver posted a great
pdf a while back, using ammonium nitrate), work in small qauntities, and before you do anything, read everything you can find on the subject.
Even when using a "crude" nitration mix, after a simple work up, nutralizations, and a few recrystallizations, a very pure product can be had, and
with consistant and desirable crystal structure. Make sure your read up on how to properly eliminate any remaining acids completely and to incorporate
a stabilizer into your recrystallizations if you plan to keep any of your ETN around for any time.
Also, ETN is very sensitive for a secondary even when made perfectly, and it is much more sensitive and dangerous when heated to melting, like for
casting. I strongly advise agianst that. I stress agian, if you decide to give this a try, READ everything you can find, cross check sources, read
accident accounts with it (several exist on this forum, some with graphic pictures, and in general, U.T.F.S.E.
Good luck, happy reading, and be safe.
[Edited on 21-9-2015 by Bot0nist]
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Bert
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Detonationology wrote:
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ETN make great salutes; it gives a very sharp and loud report, which seems very desirable.
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Could you explain that a bit further? You are making ETN for use in reports.
Are you making salutes with a primary, and/or blasting cap?
"Cooking off" the ETN in contact with Aluminum using a fuse/pyrogen?
Or adding ETN to a more traditional flash powder to increase gas output and sharpen the sound...
I knew of old time fireworks people who were said to add 50% Bullseye pistol powder to 70:30 perchlorate:dark Aluminum flash powder to this- Allegedly
did not increase shock and friction sensitivity as much as Sulfur or Antimony sulfide might, had an even better effect on "sharpening" the sound. Down
side: VERY expensive now, and a scarce material during the various ammunition/reloading supply shortages in USA.
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
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2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Detonationology
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Last New Years, I made up some ETN using H2SO4 and HNO3 concentrated from hardware store chemicals. Since firecrackers (salutes) cannot be purchased
in my area, I decided to make my version of an M-80 using some craft paper to tightly wrap the ETN into explosive capsules (of no more than .5 grams
each I believe). Attach a bit of fuse and you've got a firecracker. The report was a very loud crack when confined tightly. It's obviously wasn't
the best substance to use in my situation, but it was safer than TATP, that's for sure.
“There are no differences but differences of degree between different degrees of difference and no difference.” ― William James
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Bot0nist
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A half of a gram of pressed ETN detonated from contact with a black powder fuse? With no primary incorporated? I would have to see that to believe it.
ETN can be thermally shocked into detonation, and several members have employed this while attempting to design non primary caps. If it was as easy as
you described, then ETN would be a flame sensitive primary explosive.
[Edited on 22-9-2015 by Bot0nist]
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Detonationology
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I neutralized the product with a bicarb solution, so I don't think it would have been sensitized by any remaining acid. I compacted it, and made sure
that the ETN was in direct contact with the fuse in the end and it definitely detonated. I used Truvia sweetener because it was cheap, there were
other impurities present, but I haven't figured out how to purify the erythritol. Maybe if I UTFSE before I made it, I would have found this thread about it. I wish the OP would interject their thoughts and opinions a little more.
[Edited on 9-22-2015 by Detonationology]
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Grantr
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Sorry for no reply yet. I think ETN is what I am after. I want a loud sharp boom vs the low bass boom of ammonal. I believe the high VOD accomplishes
this.
I have been reading a lot on ETN and trying to find the PDF Quicksliver posted.
I found these two:
www.sciencemadness.org/talk/files.php?pid=29497&aid=380
www.sciencemadness.org/talk/files.php?pid=82615&aid=2150
I am not sure if these are the ones you referred to.
| Quote: |
Even when using a "crude" nitration mix, after a simple work up, nutralizations, and a few recrystallizations, a very pure product can be had, and
with consistant and desirable crystal structure. Make sure your read up on how to properly eliminate any remaining acids completely and to incorporate
a stabilizer into your recrystallizations if you plan to keep any of your ETN around for any time. |
How do you tell when you have the desired crystal shape? What works as a stabilizer?
I take it that the ETN needs to be neutralized with a bicarbonate solution or ammonia?
Is recrystallization necessary? It seems that Ethanol is the alcohol to use and using a mix of 25% acetone to 75% alcohol works as a better solvent to
recrystallize. Would 90% rubbing alcohol be ok to use?
So I think recrystallization removes impurities since the yield is almost always less after the 1st recrystallization. What affect do these impurities
have on the product? Can it be stored without recrystallization?
I am not going to heat it for casting. I do want to press it to make a denser charge for a higher VOD vs just having it loose in a bag.
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Bert
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Quote: Originally posted by Bot0nist  | A half of a gram of pressed ETN detonated from contact with a black powder fuse? With no primary incorporated? I would have to see that to believe it.
ETN can be thermally shocked into detonation, and several members have employed this while attempting to design non primary caps. If it was as easy as
you described, then ETN would be a flame sensitive primary explosive.
[Edited on 22-9-2015 by Bot0nist] |
There is no need to DETONATE highly flammable and finely powdered HE if all you want is a firecracker- It's a bit of a waste, but a couple of grams of
powdered ETN ignited by a BP core fuse will certainly rupture a strongly made firecracker case and make a decent report, even if only deflagrating.
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Bot0nist
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Thank you for the clarity, Bert. I guess when I read "tightly wrapped" and "capsule" I erroneously took it to mean compressed into a dense solid mass,
and not a confined loose powder, and couldn't imagine it bursting the casing. I apologize, detonationology.
Grantr, those arn't the ones I had in mind. IIRC, it was titled "2005.pdf" or something along those lines. I've had trouble re-finding it in the past,
but will give it another look. He discussed neutralizations, stabilization, and recrystallizations in depth.
95% ethanol (everclear, goldengrain) works well for recrystallization, and, in quicksilver's words, the 5% included water allowed some of his sodium
carbonate(which he preferred to bicarbonate due to solubility) to help ensure neutralization during recrystallization. As far as crystal structure, a
microscope helps, but just observing the material and the way pours can be usefull. Keep searching. There are so many ETN jems hidden on this board,
some buried in other, unrelated threads.
Oh, and no, in my opinion it can NOT be stored without proper neutralization and at least a couple recrystallizations. The initially formed crystals
can not be washed or neutralized of acid properly, as it gets trapped in their structures. It will turn yellow and decompose in storage.
[Edited on 23-9-2015 by Bot0nist]
[Edited on 23-9-2015 by Bot0nist]
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Bert
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I have observed yellowing after 6 months of storage, even after a single neutralization/re-crystallization from ethanol. My solution: Burned that
sample off and I won't try to store this in the future. How many receustalizations has anyone else found to be needed... I never bothered to repeat
that experiment, too many other fun things to explore.
PETN similarly given a single neutralization/re-crystallization from acetone was observed to store happily, remaining snow white and odorless for
YEARS.
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4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Detonationology
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According to the Wikipedia page, ETN melts at 61 °C (142 °F). I can't say I have much experience in casting or recrystalization of ETN (main reason
being that I only make it when I need it, and I do not plan to store for long periods), yet I am familiar with my food dehydrator which has a heat
range between 120˚-180˚F, and I typically opt to use the dehydrator when drying/ recrystalizing anything flammable or explosive. Think it would
work?
“There are no differences but differences of degree between different degrees of difference and no difference.” ― William James
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Grantr
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Is this the PDF in this thread? http://www.sciencemadness.org/talk/viewthread.php?tid=7209
Page one a few posted down by Quicksilver
[Edited on 23-9-2015 by Grantr]
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Bert
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| Quote: Originally posted by Detonationology | | According to the Wikipedia page, ETN melts at 61 °C (142 °F). I can't say I have much experience in casting or recrystalization of ETN (main reason
being that I only make it when I need it, and I do not plan to store for long periods), yet I am familiar with my food dehydrator which has a heat
range between 120˚-180˚F, and I typically opt to use the dehydrator when drying/ recrystalizing anything flammable or explosive. Think it would
work? |
THINK it will work?
How about you go read up on "heat stability test" as it relates to such things as industrial manufacture and storage of nitrocellulose, nitroglycerin
& etc., then perform some stability tests on small amounts of your actual materials!
Come back and report your findings, all you need to know to get started on this project is in the Davis and Naoum books in the library here-
Afterwards, you will know something well worth knowing, and we will know you're not a kewl looking for spoon feeding.
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
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3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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Bot0nist
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Yes.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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Detonationology
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Thanks for those resources, Bert. Allow me to correct myself: ETN would be capable of melting in a food hydrator between the temperature range
specified. I should have phrased my question "What is the most controlled way to recrystalize/dry/or cast ETN tested?" My apologies for posting a
potentially life-threatening, untested method.
“There are no differences but differences of degree between different degrees of difference and no difference.” ― William James
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Grantr
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After I buy a good thermometer and some glass I am going to try this 1st method in Quicksilver's synthesis which yields 85%.
IS this thermo ok? Thermo
I have a few more questions. Is the fertilizer grade AN 34-0-0 pure enough from the bag?
The method only mentions one temperature of 20C. I assume it is ok to be a bit lower than that when adding the Erythritol (E) to the solution?
It says to add all of the E while stirring then put in the fridge for an hour. So how long do you wait after stirring to put in the fridge? Do I just
set it and forget it for an hour? Seems strange being the 2nd method calls for stirring every 5 mins.
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aga
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Have you actually Done anything yet Grantr ?
Lots of Advice has been offered already.
Do some gunpowder or something easy like that.
Bert was born with a Silver Spoon in his mouth.
Aged < 1 day he added some other ingredients, then literally Blew it out.
(i think the spoon is still embedded in the timbers of that house).
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Grantr
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aga,
Not with the ETN synthesis. I have played with black powder for a long time., Sugar Kno3 rocket fuel and smoke bombs. I also make ammonal and shoot
it. I mainly play with the ammonal now since it cost me less than a dollar a pound to make. Much cheaper than BP and a whole lot more powerful.
Not sure I follow your post about Bert and the spoon.
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Grantr
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After you recrystallize the ETN with methanol or ethanol, What do you do with the used alcohol after dumping it in water?
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