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mfilip62
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You neutralize acids like before but then dump white NG/water emulsion in toluene and stirr a bit.
All water shuld sink.
How do you extract it from toluene.
Well,it is simple. Evaporate it at room temp. or under vacuum
of some kind!
Just don't heat it for Christ sake!
Or you can add NC directly in the toluene to make
gelignite,store it that way and evaporate it prior the use!
I recomend Celulose hexanitrate method from SamBarros page.
Will try it ASAP when I obtain chemicals.
That sounds one of the safest methods for making anything
related with NG in big batches and for long period storage.
Just make sure you neutralize it completly and suck up NOx with urea.
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hissingnoise
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| Quote: | | I got some idea about NG that may be crazy or great and simple... |
Forget the great; it's more likely to be simply crazy!
You could end up with a very sensitive mixture.
Then you'd have to evaporate the toluene to recover the nitro.
That'd require some heat or a lot of time!
And any non-volatile toluene contaminents would remain in the nitro.
It's way too dangerous to try!
At least with the tried and tested procedure you know where you are.
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nitro-genes
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small detail...
Fully nitrated NC won't gel NG IIRC
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Lambda
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I personally find the swirling method used for very exothermic reactions close to the critical temperature, and in small liquid volumes, to be quit
dangerous. Small volumes give faster temperature rise, and thus are harder to control. Unless the glycerin is added very slowly, by drop wise
addition, and given plenty of time to fully react with the nitrating mixture, thus diminishing hot spot formation. Stirring one way with a mixing rod,
is also a relatively inefficient way to mix fluids, unless used in the pattern of an 8. The stirring rod, is often the thermometer itself, and an
accident/stupidity is lurking around the corner like tickling the tale of the devil. @DetaDude's air mixing method is my favorite, and by far the
safest way to go. Multiple air outlets will also give more efficient mixing turbulences in the nitrating mixture.
Lambda
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hissingnoise
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| Quote: | | Fully nitrated NC won't gel NG IIRC |
Are you sure, nitro-genes?
I thought it would dissolve - just more slowly. . .
And produce a stiffer gel!
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Lambda
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Highly nitrated guncotton contain ca. 13 % by weight nitrogen, while low-nitrated collodion wool contain ca. 11 % N
It's the collodion that is used for blasting gelatine. Probably the higher 13 % N will only swell, but you won't get the gelatin under normal
conditions (pressure and temperature).
Lambda
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Uhm @ mfilip62
You think evaporating the toluene of the ng is going to cut it without evapping a load of NG, any idea how volatile it is ?
Even at lower temps and normal pressure the NG wil probably enjoy itself at evaporating along with the toluene.
Thats why I asked u this, I'd thought you figured this yourself.
What a fine day for chemistry this is.
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mfilip62
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Glycerine was added REALLY slowly in ice bath and constantly stirred,allmost no heat to be measured.
When I used to make bigger batches long ago I use altered blender with really slow stirring spead and teflon coated blade,biurete full of glycerine
and all that in really cold ice bath.
I really didn't know that fully nitrated NC won't disolve in acetone!
Thanks for the tip but why is that!?
Made it just one time but found it not too much interesting.
I didn't wanted to dilute NG with toluene too much but add it just enought to separate it from water in emulsion.
That is why I aksed you abbout this!
Why is NG/acetone mix considered safe and you say that NG/toluene
mix wuld be dangerous?
They are both non-polar solvents.
My NG is in oppen bottle for weeks and allmost no reduction in volume can be observed,it is not that volatile.
Previously I stored it in acetone,evaporising aceton day or two prior the use,leaving NG with a bit of acetone behind.
It is powerfull and blasting cap sensitie explosive.
That or freezing it,both is good,but impatience will kill you,REALLY!
Everiting abbut NG must be slow,expecially final preparatio if
stored long time.
I preffer it ower AN/NG and TNT/NG dynamite becouse it is liquid!
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nitro-genes
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Who said anything about acetone? Correctly speaking, the process cannot be termed solubility anyway, hence "colloidal" or "collodion" NC, as Lambda
pointed out...
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Deceitful_Frank
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I personally have never been able to (or taken the trouble to) to make NC with the ideal 11.5% nitrogen need to to set NG without the use of solvents
but find the most straight forward method is to make up your nitration bath for your glycerin (or better 50:50 EG/glycerin) take your cotton wool and
dip to soak with acids and set aside while you nitrate your polyols.
I think using acetone greatly speeds up gellation and saves time giving a more homogenous product. Just spread it out in a thin later on a dark
coloured non stick baking sheet and leave out in the sun for an hour and the acetone will be gone. 50:50 NG EGDN is MUCH less volatile and probably
safer to handle than NG and FAR less hassle and quicker to make and purify than pure NG.
Shoot for around 2.5% NC and it will just about hold its own shape but allow you to blend in some energetic dope or even 600 mesh flake Al if that
tents your trousers!
[Edited on 27-1-2010 by Deceitful_Frank]
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mfilip62
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Thanks nitro,didnt know that word in english so I didn't want to
sound like smartass!
You did not understood my question.
I didn't said you or someone else here said anything abbout acetone on this thread(doesn't matter),but I know that his mix
(NG/acetone) is widely accepted as safe method for storing NG,
why then you think it will be bad idea to stor it with toluene.
Chemically,there is no much difference between toluene and acetone
in this case,they are both oxygen pure volatile non-polar solvents,acetone being slightly less reactive.(I think...)
Why do YOU think it is bad idea to mix NG and toluene
if time needed for evap. is not crytical?
I ask you becouse I don't know and want to learn from someone who knows beter,not to make my point.
Frank,
I used EG much more than NG until cheap source of ethylen glycol
was withdra in my country becouse retarded children and old people
drank it,at least once...:
Now it can be found only in pharmacies (that "...won't sell you a poison for children!") or very diluted and contaminated in some brands of antifreez.
I never tried to nitrate glycerine and erythritol glycole in same batch,that sounds interesting,but don't really know what measures
shuld I take.Do you!?
We here have great explosive named "Vitezit" (made in neighbour Bosina,banana country with allmost no regulations at all.)
Friend of mine worked in factory,giving me a lot of precious info.
It is made of 60/40 EG/NG mix(depending on type 10-80%) and ammonuim nitrate with a bit of stabilizer FeO2 that gives him a nice red color.That is one
great booster explosive that never let me down!
They allso newer mix-nitrated EG and NG,but combined it afterward.
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hissingnoise
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A colloid is a type of emulsion and collodion is a partially nitrated cotton!
They're not related in any way.
IIRC, toluene mixed with oxidisers like HNO3, TNM and NO2 forms very shock-sensitive and powerful HEs which are difficult to handle safely.
Separating nitro from water is simple, relatively safe and very effective!
Why take chances with life and limb?
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mfilip62
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As I can remember, toluene forms nitrates only with highly concentrated HNO3 and H2SO4,and they are, under no mean unstable, most of them not even
real explosives.
You think that leftower NO2 or even ONO2 groups in NG can react with toluene to form,what; MNT,DNT,TNT...all of them much less sensitive than NG,or
did I overlooked something...
I don't,under any mean say I know more than you,it is interesting topic,thought...
And what about other water insoluble solvents like ether,how they may react!?
Ethers seems interesting,because they are most similar to the acetone,but don't mix with water!
And what about ethanol and methanol?!
They both mix with water and but not with NG!?
So you do it other way, put NG emulsion in some concentrated simple low alcohol like methanol/ethanol/propanol and mix it,
water from emulsion should be sucked up, leaving pure NG on the bottom. Only leftover may be some poppers that evaporate almost instantly!
Yes, it may be more expensive to use almost pure alcohol but
I don't care, just is it plausible!?
So, what are you bets;
toluene
ethers
simple alcohols
poppers
Who knows,we may found safer method for NG production?!
I found this step,the most dangerous of all.(handling emulsion)
Once it exploded in my garage, without any stimuli I know about,
obliterating table and blowing out windos!
No mices seen since then
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Lambda
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Collodion is a flammable, syrupy solution of pyroxylin (low nitrated cellulose) in ether and alcohol, and with Nitroglycerin it forms a Gel when all
the solvents (ether and alcohol) have been evaporated out.
Quote: Originally posted by hissingnoise  |
IIRC, toluene mixed with oxidisers like HNO3, TNM and NO2 forms very shock-sensitive and powerful HEs which are difficult to handle safely....
|
This citation is from:
Bretherick's Handbook of Reactive Chemical Hazards - Volume 1 - 6th Edition - Edited by P.G. Urben
(Butterworth-Heinemann - 1999)
Page 208 (scan page 235)
Tetranitromethane
Hydrocarbons
1.Stettbacher,A., Z.Ges.Schiess.Sprengstoffw.,1930, 25,439
2.Hager,K.F., Ind.Eng.Chem.,1949, 41,2168
3.Tschinkel,J.G., Ind.Eng.Chem.,1956, 48,732
4.Stettbacher,A., Tech.Ind.Schweiz.Chem.Ztg.,1941, 24,265–271
5.Anon., Chem.Ztg.,1920, 44,497
6.Zotov,E.V. etal,.,Chem.Abs.,1980, 93,49732,49734
When mixed with hydrocarbons in approximately stoicheiometric proportions, a sensitive highly explosive mixture is produced which needs careful
handling [1,2]. The use of such mixtures as rocket propellants has also been investigated [3]. Explosion of only 10g of a mixture with toluene caused
10 deaths and 20 severe injuries[4]. The mixture contained excess toluene in error[5]. Detonation characteristics of mixtures with benzene, toluene
(and nitrobenzene) were studied[6].
Bretherick's Handbook of Reactive Chemical Hazards - Volume
1&2
Bretherick's Handbook of Reactive Chemical Hazards - Volume 1 - 6th Edition - Edited by P.G. Urben (Butterworth-Heinemann - 1999) 2129s.pdf
(6.27 MB)
&
Bretherick's Handbook of Reactive Chemical Hazards - Volume 2 - 6th Edition - Edited by P.G. Urben (Butterworth-Heinemann - 1999) 433s.pdf
(1.41 MB)
as
Volume 1&2
iFile.it Download Link (5.9 MB):
http://ifile.it/cfqpkh6
Password: Gonorrhea ... and I just don't seem to get rid of it, ... or maybe I should just stop
visiting all those Hookers at night, ... for it's becoming exhausting ! 
I love Holland, and Amsterdam in the evening !
Enjoy !
Lambda
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mfilip62
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| Quote: |
Explosion of only 10g of a mixture with toluene caused 10 deaths and 20 severe injuries[4].
|
Yeah,right!
That sounds like someting that crazy Japanese guy said abbout AP
and "DPPP".
"30 people were killed while stearing in the 1g of unobtanium meganitrate!!!"
That only has sense if detonation started fire and they all burned in building.
Your last post lacks sense,don't get what Amsterdam and you being kinky has to do with NG extraction methods!?!?
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Lambda
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| Quote: Originally posted by mfilip62 |
Your last post lacks sense,don't get what Amsterdam and you being kinky has to do with NG extraction methods!?!? |
Mens Confessions
Explosive Sex
One night at the club with my friends, I saw this very sexy girl. I noticed she was eyeing me for a bit. So, I walked up to her. I wanted to start
with small talk but instead she pulled me into the bathroom and started stripping. I said, "Wow!" She had the biggest breasts ever and a tiny butt.
Then I stripped. She started rubbing me, and I gave her oral. All I can say is that we had explosive sex. We went to her house and started having
explosive sex again!
http://webcenters.netscape.compuserve.com/men/confession.jsp...
Enjoy Bretherick's Book, there is more Bang Bang to this Book than any other Book
in this field !, and it may save your life one day ! 
Lambda
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hissingnoise
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So, you've finally lost your virginity Lambda?
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mfilip62
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...or it may kill you in the very slow and paintfull manner!
Hate STD-s and dirty women!
NG on the other hand,if you don't drink it,it is relatively painless!
No really,has anyone any other idea on NG extraction/dehidration
with solvent!?
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Deceitful_Frank
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| Quote: Originally posted by mfilip62 |
I never tried to nitrate glycerine and erythritol glycole in same batch,that sounds interesting,but don't really know what measures
shuld I take.Do you!?
|
What measures? Well you either mean safety measures or more likely you are asking amounts... I'll go with the latter.
I just go with an equal mass or glycerin and EG. This will be slightly more EG by volume as glycerin is more dense but the mix is just nitrated as if
it was straight EG.
This makes nitration much more easy than using just glycerin. I squirt in 5ml at a time, mix with stirring rod (PTFE is good) wait for 3-4 minutes for
temperature to come back to 12-13C and repeat. Towards the end you can reduces the waiting time between additions greatly. Adding the equivalent mass
of glycerin to a nitration bath takes twice the time and stirring effort.
Your blasting oil has nearly identical power to NG or EGDN but is thinner so under a layer of saturated salt/NaHCO3 can be swirled and neutralized dry
and clear within a few days.
The blasting oil won't be nearly as volatile and headachy as pure EGDN and with the NG it contains will be more energy dense if maybe a little less
safe to handle but thats all relative.
Just don't go accidently throwing a litre bottle of it against a concrete wall!
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mfilip62
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Nice,thanks!
I preffer my method with bledner/biurete/icebth/thermometar.
With your formula I can speed up the process and do it safer!
I will probably work with my frend that is electronic freak to make
something that adds AN to the icebath or cuts of glycerin if themp rises ower 30° and dumps mix in the cold water if ti goes ower 45°.
That will be interesting project!
I didn't understand this part;
| Quote: |
The blasting oil won't be nearly as volatile and headachy as pure EGDN and with the NG it contains will be more energy dense if maybe a little less
safe to handle but thats all relative.
|
You mean a little bit less safethan pure EGDN or what!?
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Deceitful_Frank
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As far as impact sensitivity I would say safer than NG but not as safe as EGDN to handle but unless you are unlucky enough to have parkinson's AND
tourettes I would not worry too much!
EDIT: Damn if you think you can let temperatures even APPROACH 30C you are gonna LOSE!
I suggest you read more!
[Edited on 27-1-2010 by Deceitful_Frank]
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mfilip62
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That was kind of first experimental calibration.
No sinthesis done,where completed rig wasn't even finished in plans.
My synth never. goes over 20°C,it is usually arround 5-10°C
I once let intentionally small batch to go over 40 to see what will happen and what I need to care abbout.
Runnaway accours at arround 45°C,ad it is pretty nasty,but nothing
to worry abbout if you do it under 10ml and with complete safety gear,including gas-mask.
Biger batch,lower temp.
Actually I had industrila chart with temp/kilo ratio once!
I still preffer EGDN,much safer,and you allmost can't tell difference
in power.Need to find more good ol' antifreez!
[Edited on 27-1-2010 by mfilip62]
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hissingnoise
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| Quote: | | I once let intentionally small batch to go over 40 to see what will happen and what I need to care abbout. |
Your nonchalance is going to be a real liability at some time in the future if you don't slow down and think more seriously about the inherent dangers
of playing with high explosives.
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mfilip62
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Hehehe,don't worry abbout me,I survivem more than you can imagine,99% not by my guilt!
Quite oposite!
You don't read what I write!
I left SMALL batch in SAFE enviroment to go nasty,to
see what can I expect in worst case scenario when I do it in larger batches,capish!?
I was 20m+ away observing it behing plexiglass with
high power binocular,batch contained 10ml of glycerine that was added in nitration mix withou stirring and cooling.
It gave me some pretty valuable information to predict
when the batch my go nasty!
(For example when NG/glycerine starts to act like lava lamp
it is quite critical but still menegable,and when it turns red/brown,bubbles are abbout to form,the big brown cloud and everything goes
"Wuussssshhhhhh" with small det that blew glass.
That is something that reasonable and cautious person shuld do
before making bigger batches of any nitrate.
I made and detonate over 5kg of NG and EGDN,without any problem
exept mentioned incident in the garage.
it was 100% controled experiment,not something you do for fun
when you are drunk.
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Still charges of 5kg EGDN/NG , sorry to say but your really out of your mind.
And yes nonchalance really fits the profile your are sketching right now.
On the other hand why not blow yourself up , as long as you don't hurt the neighbors.
If your handling chemicals is as correct as your grammar you should be just fine.
Amateur experimentalism.. right.
What a fine day for chemistry this is.
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