| Pages:
1
2
3 |
Nevermore
Hazard to Others
Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline
Mood: shopping businessman
|
|
Playing with EGDN
Like every year for new year eve SWINM prepares his experiment
this is the only period of the day when He can test energetic matherials outside in quantities bigger than 1ml, and ppl won't even complain!
so let's see what do we have here:
14,6 ml of "paraflu" antifreeze fluid of unknown composition "for alu radiator".
40 grams of ammonium nitrate fertilizer grade, dried and crushed in powder.
60 ml of Sulfuric Acid, drain cleaner quality, 96%.
a kg of ice
thermomether
pipette and some glassware.
First of all, let's try to identify the antifreeze fluid:
it is blue, doesn't smell, is a thick syrupy fluid, and they say contains EG.
test: trying to boil it to check the boiling point.
result: it boils far over 140°C which is SWINM thermometer limit, and never boils actually just evap off, the condense is a clear oily liquid.
so let's start the synth.
SWINM puts 60ml of acid and AN into the freezer until they reach 0°C (don't let the acid freeze..)
then they get mixed into a clean becker surrounded with the melting ice.
The temp pops up to 20°C and little fumes get off, then cools down to 3°C again making it a thick slurry.
In the meanwhile the antifreeze lays in the freezer.
At this point the antifreeze gets added with a pipette, while the nitrating slurry is being mixed with the thermometer, the total addition of 14.6 ml
takes around 20 minutes keeping the temp at 10°C (yes i know, SWINM is damn cautious with things he doesn't know),which are followed by another 25
minutes of "le the stuff do their job".
After this time the slurry is dumped in approx 600ml of ice cold water, which is continuosly stirred for 2 minutes then allowed to sit, in the next 5
minutes the EGDN collects on the bottom as a white oily blog, in quantity FAR over what was espected (considering the unknown composition and the
normal loss).
SWINM uses a pipette to suck the EGDN out and dumps into a NaHCO3 saturated solution, some bubbles evolves then the EGDN sets on the bottom again, it
gets sucked by the pipette and again into a fresh NaHCO3 solution until NEUTRAL.
The EGDN is pipetted again into a shallow dish in order to lose the water and become a clear fluid with a yellow highlight (okok, should be clear
only, but damn it is neutral, maybe some dyes got nitrated too giving the yellow tone?)
Now SWINM has a burping vial of neutral EGDN, approx 15ml, laying into a becker filled with water.
Interesting stuff is that the blue color is lost during nitration, and the result is perfectly clear.
SWINM plans to set off the EGDN in batches of 5ml absorbed in dry AN in order not to attract too much interest, around midnight of tonite, so that it
will be confused with the other fireworks, set off will be insured by a straw filled with SP, around 200mg of Silver Nitrate/Acetylide, and 300-500mg
of MHN.
i think i found why the EGDN is yellowish, it shows a ph of 5 now, i think is still fine, since will be set off in a few hours, and i dun have enough
time to dry it after a new neutralization..
Happy new year to everyone!
Nevermore!
|
|
|
h0lx
Hazard to Self
Posts: 69
Registered: 31-12-2005
Member Is Offline
|
|
No, this can't be the pH, what makes it yellow. Mine is the exact same color always and it is always neutral or slightly basic.
EDIT: fixed grammar
[Edited on 31-12-2005 by h0lx]
|
|
|
chemoleo
Biochemicus Energeticus
Posts: 3005
Registered: 23-7-2003
Location: England Germany
Member Is Offline
Mood: crystalline
|
|
Nice. YOur picture is sideways I guess.
How sensitive is it, as bad as NG? Letting a drop fall onto the ground, will it make a bang?
ON the note of the dyes - yes it's probably just some triphenyl derivative, which gets nitrated to nitrobenzenes and TNP. Maybe that's where you get
part of your colour from.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
|
|
|
kABOOM!
Harmless
Posts: 40
Registered: 19-12-2005
Location: Pacific side of Canada
Member Is Offline
Mood: No Mood
|
|
How powerful is EGDN? Is it as powerful as NC?
Anyway, have a happy new year everyone!!!
play safe, play hard...get your lumps...pick yourself up and try again. It will only make you stronger.
|
|
|
Nevermore
Hazard to Others
Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline
Mood: shopping businessman
|
|
hello
is far less sensitive than NG
no, letting a drop fall won't set it off, it doesn't even with NG.
not even from a tall building.
i've been able to set off NG only by hammering it really bad on a steel plate..
no other ways..
drop it and set it off is a legend i suppose, or just could happen with NG at PH 1 or semifrozen...
and has about the same power of NG from what i read, NC can't be compared to any of them..
just easier to set off and less sensitive..
BUT volatile.
[Modificato il 31/12/2005 da Nevermore]
Nevermore!
|
|
|
kABOOM!
Harmless
Posts: 40
Registered: 19-12-2005
Location: Pacific side of Canada
Member Is Offline
Mood: No Mood
|
|
could it be added to Nitromethane to become more shock sensitive? I'm thinking of a supercharged form of PLX, which really doesn't need any real
supercharging 
...just thinking.
play safe, play hard...get your lumps...pick yourself up and try again. It will only make you stronger.
|
|
|
Nevermore
Hazard to Others
Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline
Mood: shopping businessman
|
|
actually i think is a little wasting to sensitive NM with EGDN, being NM effectively sensitized by H2SO4 or epoxy hardener...
but i don't know if the two liquids are miscible, i suppose yes.
Nevermore!
|
|
|
Chris The Great
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
EGDN is more powerful than nitro.
Lead block 650cm3, brisance 185% TNT, perfect O balance:
C2H4N2O6 -> 2CO2 + 2H2O + N2
|
|
|
Nevermore
Hazard to Others
Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline
Mood: shopping businessman
|
|
7ml of EGDN absorbed on 20g of AN into a coffee plastic glass
ignited by a cap made with 500mg MHN + 200mg Double salts
made a loud sharp boom and an orange fireball
the result were a round hole on the concrete
approx 8cm radius parabolic shaped with the center deep around 3cm.
pretty powerful considering that the boom was much less than i expected!
Nevermore!
|
|
|
Deceitful_Frank
Hazard to Self
Posts: 82
Registered: 5-11-2005
Member Is Offline
Mood: Pensive
|
|
| Quote: | Originally posted by Chris The Great
EGDN is more powerful than nitro.
Lead block 650cm3, brisance 185% TNT, perfect O balance:
C2H4N2O6 -> 2CO2 + 2H2O + N2 |
I think it all depends on how you define power and we all know theres alot more to it than lead block expansion (I dont know where you got 650cm3 from
but sounds a little exaggerated to me... 600 is more the figure) and perfect oxygen balance.
Plus "185% TNT" means nothing as far as I can see unless you would like to elaborate on wether you mean by mass or by bulk, velocity or gas expansion?
If you offered me a 10Kg of TNT or the same mass/volume of EGDN to do a blasting job I'd go for the TNT pretty much every time. Although EGDN may be
more "powerful", TNT is ALOT more usable.
EGDN does interest me and after sourcing all the necessary chems, I have yet to make it. I have synthesised NG many times and have perfected my
process to get 1.82g dry neutral NG from every gram of glycerol. I'd probably use a very similar process whilst minimizing loss of yeild through acid
and water dissolution wherever possible but its what I would do with it when made thats been putting me off.
Due to its volatilty the same process that I use to make blasting gelatine (no loss of velocity over the pure nitric ester and incorporation of
microbubbles to lower the density and ensure high velocity detonation) using distilled acetone as a solvent would result in MAJOR losses in the drying
process that you just dont get when using NG.
I dont want to just absorb it into something shit like AN as then i may as well just stick to kinepack! Plus to fire it pure as a liquid and at
>7000m/s you need confinement in steel and/or a HUGE blasting cap... (80g TNP) according to urbanski/federoff though they did state 8400m/s IIRC!
Ant ideas on how to make this no doubt excellent explosive usable and easy to initiate fully?
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
It could be worthwhile to experiment to see what
sort of potential solvent / plasticizing / densifying
properties the EGDN may have with things like
R-salt or RDX , or the nitrated polyols like MHN or
inositol hexanitrate or even PETN or ETN . Some
interesting mixtures might result which could have
the property of partially melting upon gentle heating
and then setting solid on cooling to a dense and
highly brisant composite having easy initiation .
|
|
|
ADP
Hazard to Others
Posts: 120
Registered: 4-4-2005
Location: USA
Member Is Offline
Mood: Productive
|
|
Nevermore I'm not sure what kind of antifreeze you may have used but I believe that many kinds of antifreeze not only contain ethylene glycol and a
dye but also diethylene glycol.
This means perhaps not only is your product ethylene glycol dinitrate, but it could also contain diethylene glycol dinitrate which has similar
properties and is misible with the former, while being insoluble in water.
Firstly is anyone aware of a method to separate the two via solubilites and chemically? (not distillation). I will soon obtain samples of both
diethylene g. and ethylene g, in which I plan to nitrate both and examine similaries and differences.
FYI: Ethylene Glycol: BP: 197dC with formula C2H6O2 or HO-CH2-CH2-OH, while
Diethylene Glycol: BP: 245dC with formula C4H10O3 or HO-CH2-CH2-O-CH2-CH2-OH (to better reflect structure).
|
|
|
12AX7
Post Harlot
Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline
Mood: informative
|
|
Possibly DG is more lipophilic so a light solvent such as mineral spirits could be shaken to dissolve it? If it takes some EG with, an addition of
water might break that.
Just guessing...
Tim
|
|
|
Chris The Great
Hazard to Others
Posts: 463
Registered: 29-10-2004
Location: Canada
Member Is Offline
Mood: No Mood
|
|
| Quote: | Originally posted by Deceitful_Frank
I think it all depends on how you define power and we all know theres alot more to it than lead block expansion (I dont know where you got 650cm3 from
but sounds a little exaggerated to me... 600 is more the figure) and perfect oxygen balance.
Plus "185% TNT" means nothing as far as I can see unless you would like to elaborate on wether you mean by mass or by bulk, velocity or gas expansion?
|
Chemistry and Technology of Explosives, vol 2 for the lead block.
The 185% TNT is for the brisance, which is a measure of the shattering effect and so velocity, gas expansion etc has nothing to do with it. It's
measured by mass, like most tests. I beleive the 185% of TNT was determined by firing 100g EGDN on top of a lead cylinder and measuring the
compression.
|
|
|
Nevermore
Hazard to Others
Posts: 140
Registered: 3-5-2003
Location: China at the moment
Member Is Offline
Mood: shopping businessman
|
|
then being EGDN far less dense than NG could in part explain the effect...
Nevermore!
|
|
|
ADP
Hazard to Others
Posts: 120
Registered: 4-4-2005
Location: USA
Member Is Offline
Mood: Productive
|
|
Distillation of Ethylene Glycol from Antifreeze
I performed a distillation of antifreeze at 197dC (Ethylene Glycol's BP) and had wonderful results. The antfreeze had EG and DEG (a small amount I
believe) in it.
I used a retort as it is easy to use and works great for the job.
Boiling at 197 degrees
After 2 hours or so, the final yield was 110ml (this pic shows after about 1.5hours)
Here is the final look at a bottle of antifreeze and a bottle of EG
In conclusion, distillation is very simple and easy and good to do if purity is of importance. The resultant product is very pure.
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
The distilled product from antifreeze may have some
water in it , and may need to be dried before nitration .
A density measurement can be done and the results
compared with the chart attached , to get an idea of
the purity .
Attachment: glycol solutions density chart.pdf (348kB)
This file has been downloaded 1686 times
|
|
|
oneup
Harmless
Posts: 47
Registered: 17-12-2005
Member Is Offline
Mood: No Mood
|
|
I just did the synthesis of EGDN, and my experience differs somewhat from yours, nevermore.
Everything is the same UNTIL i drop the still white EGDN in carbonate solution, it loses it's white color and becomes almost invisible as a colorless
blob on the bottom of my vessle. I used 10mL EG and got 9mL EGDN, but some got lost becouse I didn't wait long enough for all the EGDN to settle to
the bottom. I haven't tested it yet becouse I ran out of acetone peroxide to detonate it but I will compare it to nitroglycerin and post the results.
|
|
|
ordenblitz
Hazard to Others
Posts: 259
Registered: 18-7-2004
Location: Northwest
Member Is Offline
Mood: Bohr'd
|
|
Say... how did "someone who is not you", get a picture of something you did not make right after you didn't make it?
I'll bet the man won't ever figure out this type of clever subterfuge!
|
|
|
h0lx
Hazard to Self
Posts: 69
Registered: 31-12-2005
Member Is Offline
|
|
I ran out of AN and I want to make some more of EGDN. Using KNO3. So I calculated the ractants to use and the numbers didn't seem correct. I
calculated as 1 mol of MEG, 2 mol of KNO3, 4 mol of H2SO4(2 mol for forming nitric acid and 2 for absorbing 2 moles of water)
I got (rounded, decimoles)
13,2 mls of MEG(15,2g)
20g of KNO3
23,1 ml of H2SO4(39,8g)
Could someone correct me?
[Edited on 24-1-2006 by h0lx]
|
|
|
Boomer
Hazard to Others
Posts: 190
Registered: 11-11-2005
Member Is Offline
Mood: No Mood
|
|
C = 12, H = 1, N = 14, O = 16, K=101. Therefore 1 mol EG ( C2H4(OH)2) = 62g, KNO3 weighs 101g, sulfuric 98g.
15.2 g = 0.245 mol EG needs 0.49 mol = 49.5g KNO3. Use 40-50% excess for a nitrate/acid nitration.
Plus 4 x 0.245 = 0.98 mol (96g) SA of 100%. More to absorb its own water if it is only 96%.
Plus some excess again perhaps, but it absorbs more than a mol of water.
Try 15ml + 30g + 50ml for a start. This is the minimum amount of sulfuric, but too much dissolves the product.
|
|
|
h0lx
Hazard to Self
Posts: 69
Registered: 31-12-2005
Member Is Offline
|
|
I will try with 30ml + 60g + 120ml today as my SA is only 94% and KN will dissolve more easily. I had calculated the MEG mass wron, I Calculated
EGDN's
|
|
|
rot
Hazard to Self
Posts: 62
Registered: 26-1-2006
Member Is Offline
Mood: No Mood
|
|
Is EGDN more powerfull than Nitroglycerin or not? nitroglycerin has a VoD of 7700m/s i know but some say EGDN vod is <7300, some say it's 8000.
|
|
|
Boomer
Hazard to Others
Posts: 190
Registered: 11-11-2005
Member Is Offline
Mood: No Mood
|
|
It has slightly more energy content due to perfect OB, but less brisance and VoD due to lower density. It is 'thinner' than NG and therefore transmits
detonation easier.
That is why some people found higher brisance/speed values for it. If you manage to get NG going full steam, it beats EGDN (except for energy as said,
but a few percent theoretical heaving power are of no concern for someone using these comps pure).
|
|
|
blank
Harmless
Posts: 2
Registered: 13-3-2006
Member Is Offline
Mood: No Mood
|
|
Last week I came across over 7L of industrial grade EG. Of course I then decided to make some EGDN.
I used:
300g H2SO4
100g NH4NO3
20G Ethylene Glycol
I premixed acid and AN and heated a bit to get some good thin acids. I cooled all chems in my freezer to 10ºC or under. I thin placed that acids in
my ice bath and added the EG while stirring over a period of 20 min. I then let it sit for 20 more minutes with occasional stirring. During the
nitration, the temp of the nitration bath stayed well under 20ºC. After nitration, I poured it into 1 L of cold water and stirred. The problem is
that I had no bottom layer of EGDN. Instead I have some kind of yellowish precipitate. Some of it floats, some sinks. I poured a few ml into a
seperate container and some droplets of EGDN formed. The droplets are reddish due to dyes in my sulfuric acid. I neutralized what I had and I am
drying it in my dessicator right now. I will test it once dry. Does anyone know how to get the rest of my EGDN to seperate from the water and acid?
It is sitting in an ice bath right now, I notice that droplets are slowly forming. Hopefully tomorrow I will be able to decant off the acid waste
and have some good EGDN. If not, does anyone know what I could do? Help is appreciated
|
|
|
| Pages:
1
2
3 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
