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Rosco Bodine
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[*] posted on 16-12-2010 at 08:42
safer NG alternatives


There has been some limited mention and discussion of ethylene glycol dinitrate in the past, and there are a couple of related materials which would seem to be of interest also as possible safer alternatives for uses that nitroglycerin may have similar value.

Propylene glycol dinitrate ( 1,2-Propanediol Dinitrate ) Methyl Glycol Dinitrate
is one of these alternatives

Diglycerol Tetranitrate is another of these alternatives

There is a potential usefulness for the negative oxygen balance of these materials in combination with energetic oxidizers or combinations with other energetic materials
which have an oxygen surplus.

I have done no experiments with these materials so I have no direct observations or experiments to share, but can share some of the references.

Attachment: Diglycerol Tetranitrate page PATR Vol. 5 D(cont.)-E.pdf (88kB)
This file has been downloaded 910 times

Attachment: US1307033_EGDN - PGDN 50-50 composition.pdf (174kB)
This file has been downloaded 774 times

Attachment: US1371215_propyleneglycol_dinitrate_AND_PROCESS_OF_MAKING.pdf (262kB)
This file has been downloaded 850 times

Attachment: PGDN pages PATR Vol. 8 M-P.pdf (273kB)
This file has been downloaded 1058 times

[Edited on 16-12-2010 by Rosco Bodine]
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pjig
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[*] posted on 16-12-2010 at 08:55


Thank you Rosco... For the great pdf's, Im in the process of checking them out right now.. :)
Which of these are the safest in comparison to NG, or less sensitive to mechanical stimulation.
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Rosco Bodine
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[*] posted on 16-12-2010 at 08:58


PGDN, and it makes an interesting blasting gelatin too.
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pjig
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[*] posted on 16-12-2010 at 09:53


Now after reading the patent, I am intrigued on the mixing for the two glycols.Combined they show a remarkable improvement over each individually.

I am curious about cheap antifreeze having pure enough ethylene glycol to be used in the manufacture of this exp. I 'm sure one could extract any water left in solution by calcium salts or mag. sulfate etc. ( a descanter of sorts). What is your take on this?
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Rosco Bodine
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[*] posted on 16-12-2010 at 10:14


Propylene glycol is unrestricted available pure as cosmetic or food grade but you could probably distill it from the non toxic antifreeze which has dyes and anti-corrosion additives, similarly as can be done with ethylene glycol. I have distilled the ethylene glycol from antifreeze but found it has some water content not stated on the label. Ha they thought nobody would know !
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[*] posted on 16-12-2010 at 10:41


You probably already know this. cue Michael Caine moment ;), but the propylene glycol commonly available is the 1,2 isomer.
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Rosco Bodine
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[*] posted on 16-12-2010 at 11:08


Yeah thanks for keeping me honest. I extracted one page short on that PGDN pages PATR reference so I replaced the incomplete file and edited the isomer designation to correct the oversight.


[Edited on 16-12-2010 by Rosco Bodine]
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gnitseretni
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[*] posted on 16-12-2010 at 12:12


You can also get propylene glycol (lubricant) from livestock veterinarians.
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pjig
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[*] posted on 16-12-2010 at 16:00


Nice find... Thanks for sharing that valuable source ...:)
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franklyn
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[*] posted on 16-12-2010 at 16:04



Polyvinyl nitrate the ester of polyvinyl alcohol has been investigated as a
propellant alternative to nitrocellulose. It is a low melting thermoplastic used
as a binder with a density of ~ 1.6 and performance comparable to TNT.
Certainly from it's properties it appears that something similar to Amatol
could readily be formulated with it. See Urbanski vol IV pg 413-419

High Energy Materials: Propellants, Explosives and Pyrotechnics
http://books.google.com/books?id=rqZROysoS7QC&pg=PA75&am...

Attachment: Investigations on Polyvinyl Nitrate as a High Energetic Material.pdf (533kB)
This file has been downloaded 1046 times

Patent on how to make it US2118487 http://tinyurl.com/339p8pz , Type in code to download

Attachment: A Low Hazard Laboratory Procedure for the Preparation of Polynitrate Esters .pdf (93kB)
This file has been downloaded 929 times

Around six times more expensive than proplyne glycol
http://www.soapgoods.com/Polyvinyl-Alcohol-p-713.html
http://www.soapgoods.com/Propylene-Glycol-p-673.html


[Edited on 17-12-2010 by franklyn]
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bbartlog
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[*] posted on 16-12-2010 at 17:00


Quote:
I am curious about cheap antifreeze having pure enough ethylene glycol to be used in the manufacture of this exp.


The main contaminant is water (as you are aware) but there is other stuff in there, at the least a colorant and some diethylene glycol (speaking here of Prestone antifreeze specifically; maybe some other mfr doesn't add dye but I suspect for safety reasons they all use it). It's fairly easy to distill, though.
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Rosco Bodine
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[*] posted on 16-12-2010 at 18:38


@franklyn

Those Thiokol boys in Utah need to get their math straight
when it comes to ETN so that they can put the mole weight down right instead of being missing a cabon and couple of hydrogens like they have in error shown it in their paper.

@ScienceSquirrel .....wake up, you let me beat you to it! :D

[Edited on 17-12-2010 by Rosco Bodine]
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[*] posted on 17-12-2010 at 03:25


I have used PGDN lots of times. Synthesized it using 65% and more concentrated HNO3 and 98% H2SO4. I used it for :
1. Blasting gelatine, also a blasting gel from mixture of NG and PGDN. Used for ammonium nitrate explosives booster.
2. Aluminized and Mg added blasting gelatine - thermobaric mixtures.
3. Liquid mixture with nitroglycerine. I just nitrate a mix of glycerol and prop.glycol.(the mix is really powerful, don't know about how safe it is). Once I nitrated a mix of ethylene glycol, glycerol and propane glycol. 200 ml mixed esters. Same good results. The overpressure wave from this was visible in the field I shot it. As it travelled through the grass.
4. Once I tried ammonium perchlorate, Al powder and PGDN : 40% 20% 40%. 20% is Al powder. 100 grams - set off with 3-4 grams HMTD cap. Full detonation.

Still do not know about exactly how safe it is? Obviously, I never had any problems with it, or I would be blown to pieces. PGDN is very powerful, about 120-130% TNT equivalent.


[Edited on 17-12-2010 by simply RED]




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Rosco Bodine
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[*] posted on 17-12-2010 at 03:54


There are some reported experiments with PGDN in the archive of the E&W Forum.
I have been doing a little reading about PGDN, and it appears it definitely could have usefulness as a material whose precursor would have ready availability.
Having good performance combined with good stability and not being unduly sensitive, and being economical are all things which commend it. Having seen
the reckless abandon of caution that some "experimenters" have shown for ETN has made me look for safer alternative energetic materials for curious but inexperienced experimenters to consider for the larger scale syntheses. ETN
is a lot more likely to take its toll on the careless, so maybe PGDN is a saner
alternative and actually having greater utility for its varied compositions.
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[*] posted on 17-12-2010 at 07:09


One source for this (Propylene Glycol) are large veterinary supply places that cater to horses, cattle, etc. Additionally Bolices (large aspirin "tablets" may also be obtained at an extremely lower price per pound, etc.



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pjig
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[*] posted on 17-12-2010 at 21:01


Great find....
What would be the best way to purify the ethylene glycol ( distillation or descanting)?
Im assuming that the 70+% azeotrope N-acid should be enough with 98% S-acid as a mother liqueur to nitrate the two glycols.
Correct me if I'm wrong, but I dont believe that these need a strong N-acid above 70% by what the patents say.... Is this adventitious...?
This makes the otc materials easier to obtain, and can be made on a slightly larger scale with some safety V.S. NG.
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[*] posted on 18-12-2010 at 07:51


When I bought my distillation kit that was one of my first distillations from anti-freeze (remember to use the cheapest one possible for sake of purity). The Merck index will have the figures needed to do it efficiently - but a simple distillation is fine....however, there IS (I heard this 2nd hand but I believe it) an OTC source; obtainable at places that sell airplane parts for private prop planes.



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[*] posted on 18-12-2010 at 11:36


Awesome! Im assuming that your saying this "2nd hand info" is referring to a purer source than the antifreeze described here. Any finds there, any luck sourcing this?
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[*] posted on 18-12-2010 at 12:29


Since I have no idea where you live I might suggest looking to see if there is an air-park with active servicing, parts equipment (& of course) associated chemicals. Because of the depth of quality in certain areas of air-travel; often the items used are of a caliber not common with automobiles, etc. Unfortunately this is going to swing me off topic so I'm happy if you send me a PM as there may be other areas you could explore as well.

Once you have the glassware; the world is your laboratory!




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[*] posted on 18-12-2010 at 14:27


I think that most of the accidents that have occurred have been
during the nitrations due to run-aways. So the best choice for
safety may be an alcohol that is more resistant to oxidation.
I seem to remember that the ease of oxidation for alcohol
groups was -HCOH- > -H2COH > H3COH
So Methyl Nitrate, EGDN, 1,3PGDN and PETN may be the best choices
for powerful nitric esters.
The first 2 are easy to make with the alcohols easily available but
they are thin and volatile liquids.

All the propylene glycol that I have seen is 1,2 not 1,3
I have not seen many threads where people made their own PE,
and it seems difficult to find. There is a very long thread on
synthesis of acetaldhyde but it is mostly full of things that don't work.
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[*] posted on 18-12-2010 at 21:11



Quote: Originally posted by Rosco Bodine  
@franklyn
Those Thiokol boys in Utah need to get their math straight when it comes to ETN
so that they can put the mole weight down right instead of being missing a cabon
and couple of hydrogens like they have it shown in error in their paper.

Just six more shopping days - Seasons greetings -

Regarding the paper : A Low Hazard Laboratory Procedure for the Preparation of Polynitrate Esters
which I posted above , I got it from this forum the middle of last month, I have not been able to find the
link to it. Speaking of links, a minor mention of what was being refered to would have been considerate.

ETN MHN.gif - 9kB
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franklyn
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[*] posted on 22-12-2010 at 00:43


http://www.physorg.com/news142839189.html
download here _
http://www.sciencemadness.org/talk/files.php?pid=141343&...

.
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pjig
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[*] posted on 24-12-2010 at 14:22


Hey that is pretty cool..."Pent's cousin " 85% is not a bad return. Acetyl nitrate in acetic acid sounds like a much smother process and the high yield makes it very attractive . Having the power of the HMX , with a low cast-able temp is amazing as well. Could this be true !!! It seems like a pretty straight forward process.... Any feedback or attempts of manufacture?
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[*] posted on 25-12-2010 at 09:02


I have made this. As I explained in the dedicated thread (which wasn't authored by me), I chose the acronym NDBD to refer to this material since the article simply refers to it as 1.
I synthesized it in the context of my masters thesis, and explored some alternate nitration systems in addition to the one given in the article (Ac2O/HNO3).

It is indeed a fairly straight forward process except for two minor things; the acetal used for the protecting step, 2,2-diethoxypropane is difficult to make, and the deprotecting step with methanolic HCl is a mess.
In the original thread, a patent was referenced that described an easy way of using anhydrous CaSO4 to drive the reaction of acetone with ethanol to produce DEP, but despite numerous attempts with many variations, I just couldn't get it to work. In the end I had to order some.

Anyway, nitration proceeds nicely using Ac2O/HNO3, H2SO4/HNO3 and P2O5/HNO3. I also tried N2O5 in DCM but got negligible yield.
Recrystallized products were examined using Raman spectroscopy and were found to be identical and give spectra that were consistent with my simulations of NDBD.
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pjig
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[*] posted on 25-12-2010 at 09:29


Nice, what was your yield for the hno3 and h2so4? Was it as good or close to the acetyl nitrate in acetic acid? Out of the nitrating acids ,what seemed to be most available and straight forward for this synth?
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