megalomania
June 17th, 2003, 08:00 PM
mav
New Member
Posts: 5
From: Czech republik
Registered: MAY 2001
posted 05-17-2001 02:08 AM
--------------------------------------------------------------------------------
I need precise instruction on production IPN, mixture IPA+HNO3 saturation urea me inject from flask mfuego@mail.ru
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-17-2001 07:22 AM
--------------------------------------------------------------------------------
Take 5 ml of 50%-65% nitric acid, add about 100 mg Urea, cool and add 5 ml IPA, NOT LESS!!! [Using the stoichiometric best amount of IPA, here about 2,5 ml, may cause too much heat generating and decomposion of the mixture.] When you cool the solution you prepared after 1-2 hours a IPN-Phase on the acidic solution should have formed.
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 05-20-2001 04:48 PM
--------------------------------------------------------------------------------
That sounds really great! Can you tell me another way of purifying that doesn't deal with distilling. For example decanting and mixing with water solution of sodium bicarbonate(is IPN(isopropyl nitrate) soluble in water?).
How dangerous not totally purified IPN is?
BoB-
Frequent Poster
Posts: 679
From:
Registered: SEP 2000
posted 05-20-2001 05:05 PM
--------------------------------------------------------------------------------
Dude, you could at least make your question a bit longer than 2 lines, I just checked with my own eyes and Mega's site has information about IPN.
[This message has been edited by BoB- (edited May 20, 2001).]
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-20-2001 05:19 PM
--------------------------------------------------------------------------------
Ehm, I'm confused by simplys post. I believe that IPN is completely not or very little water soluable. And purifying, well, shake an mixture of IPN and carbonate solution, that will bring you acid free IPN and a red carbonate solution. I don't know why it turns red but it does. And mixing acidic IPN with HMTD caused a giant detonation in my laboratory. Thank god there was a plank between me and the BOOOOM........
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-21-2001 07:10 AM
--------------------------------------------------------------------------------
I think that HNO3 + HMTD does generate enough heat to detonate the stuff!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-21-2001 07:32 AM
--------------------------------------------------------------------------------
Of course it does. If not I wouldn't have a crater in my cupboard.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-21-2001 10:01 AM
--------------------------------------------------------------------------------
I think it is a good lesson for you!And for others who read this!
Now you will never manipulate HMTD nor nitric ester without care as if it was suggar!
Mixing explosives can have very anoying side reactions always keep that in mind!One ingredient can make the difference and BOOM!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-21-2001 11:20 AM
--------------------------------------------------------------------------------
If I would tell you what happened in my laboratory beside you wouldn't mention this ridiculous explosion to be lesson.
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 05-22-2001 04:40 AM
--------------------------------------------------------------------------------
I read in "Organic Chemistry" book:
"the speed of esterification decreases with the increase of the molecular weight of the alcohols". It was not described why this happens. What is the real chemical explanation of this? The only explanation I can find(for the nitration) is that the O--H bond in the alcohols with low molecular weight is more polar because of the lower +I of the carbon radical.
for examle: o2n-OH + H--och3---}CH3ONO2 + H2O
If the O--H is more polar the water will form easier.
But on the other hand i doubt is the O atom in the alcohols with higher carbon chain more electronegative because of the higher +I of the radical.
I'm confused....
[This message has been edited by simply RED (edited May 22, 2001).]
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-22-2001 05:13 AM
--------------------------------------------------------------------------------
Yes lesson is a bit severe, but a good warning then if you prefer!
Everybody here (wel most of us) have had our lot of accidents-me included!Some have had only material accidents others have been injuried!Hopefully we are stil alive, but now we take more care about what we do!
In french we say:
A cat that has got boiling water on it, is scared about cold water!
I find it too bad that we have to pass trough that to learn to work safely and with safe quantities!
The speed of nitration decreases simply because the viscosity increases (allowing a much less efficient mix), the solubility decreases (since the organic part grows the alcool tends to become hydrophobic-you don't have a proper contact between the reactants!).
Those problems are less effective whith polyols like glycol, glycerol, erythritol, pentaerythritol, sorbitol, suggar, mannitol, cyclohexanhexol,... since then solubility is higher (but the viscosity is stil increasing!).
A good way to diminish viscosity is to heat up the stuff, but unfortunately it is a very bad idea with nitrations since heat has to be low to avoid runaway!!!!!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
mav
New Member
Posts: 5
From: Czech republik
Registered: MAY 2001
posted 06-07-2001 03:10 AM
--------------------------------------------------------------------------------
Hi. I'm found something about make IPN with refer to british patent Have not you is ?
T. Urbanski: Chemistry and Technology of Explosives volume 4 (1984) pg.309
IPN
Direct nitration was found to yield mainly acetone due to the oxidation of the secondary alcoholic group.
However a process of continuous nitration of iso-propyl alcohol in the presence of urea has been described
by Imperial Chemical Industries patents(W.G.Allen and T.J. Tobin-British Patent 696489-1953;749734,749844-1956)
iso-propyl alcohol and urea were introduced into nitric acid (over 40 % HNO3) at its boiling temperature
and a current of air stirred and removed unstable products.
According to Desseige (G.Desseigne, Mém.podres 37,97;1955) the method gave ca. 80% yield. He used nitric acid of over 50 % HNO3 at 108-110 C.
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 06-07-2001 06:11 AM
--------------------------------------------------------------------------------
Yes, I've got the book, too, but that's an industrial procedure. It's difficult to remove the unstable products in this way, also it's not needed to carry out the reaction at elevated temperatures, it works good at room temperature. This way to obtain IPN may work good for industry but not for home labs....
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-18-2001 02:33 PM
--------------------------------------------------------------------------------
I bought 1 litre of IPA and tried to make IPN. The first two attempts failed. The first attempt I mixed 5 ml 60%HNO3 with 4ml Isopropanol and 100mg urea(fine chrystals which did not dissolved). The ingredients were cooled before mixing to 0 degrees celsius. After mixing it was left at 10 gegrees celsius atmosphere(in my fridge). I checked it after 5 minutes.....It has started to bubble and release red fumes! FUCK, I said, and fast dumped it with water, immagine if I haven't checked it it could blast the fridge door abd poison the food .
The next time I tried with 5 ml 55% nitric acid, 5ml IPA and 150mg urea. I did everything at 0 degrees celsius. After 30 minutes it has become yellow, no layers, no nothing, just yellow slowly bulbing shit. I mixed it with 20ml water, and it just diluted, again no layers.
My question is where have I been wrong, Ciplla, you have have made it many times as you said, can you tell me the exact procedure you use(everyone else's help is of course also good).
[This message has been edited by simply RED (edited June 18, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-20-2001 05:12 AM
--------------------------------------------------------------------------------
This is the most uncontrolable reaction I've ever seen. It seems really difficult to make IPN.
I made some more tests with different quantities of urea, IPA, HNO3(60% and 55%). Or they don't react at all or the reaction gets out of control, red fumes,boil and finally a great splash...
Can it really be made without distilation and high temperature acid?
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 06-20-2001 08:48 AM
--------------------------------------------------------------------------------
Hmmmm I've made it about 40 times and that works. Of course I also have had a few explosion like reactions, but now .....
Ok, I put about 5 ml HNO3 55% in a test tube, then add urea until i find that it's enough.....you have to find out yourself....then I add about 5 ml IPA and then let the test tube swim in cold water....at first the urea bubbles, ´reacting with the HNO2, and then, after a while, a thick layer of IPN forms on the acid mix. If it doesn't work for you, keep the reaction principle in mind and try again and again.
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-20-2001 05:27 PM
--------------------------------------------------------------------------------
It is midnight now...
I tried the reaction again putting some more urea and not making it at 0 degrees celsius but actually at 4-5 or even more(it may have been 10-12, i don't use termometer).
IT WAS SUCCESFULL, the IPN formed an upper phase on the acidic solution! It looks very slightly yellow, the down solution looks white. While I was purifying it it formed always upper layers, never used pure distilled water but always with some salts. Have you tried it to form a down or upper layer with absolutely clear distilled water(as i read it's density is near 1(mega's site)Another questions : does it dissolve nitrocellulose(if it does I'm gonna make some plastique soon).
I'm happy i finally managed to make it! The yield seems 30-40%.
THANKS FOR THE GREAT HELP AND INFO!
[This message has been edited by simply RED (edited June 20, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-21-2001 05:42 PM
--------------------------------------------------------------------------------
Some more tests with it:
After purifying I tried to burn it. It bured with blue flame(pleasant light blue colour) faster than isopropyl aclohol.
I couldn't purify it 100%. There was always somthing that left unburned(actually really small ammount), but I didn't left it enough time in the separation funnel(improvised one).
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-22-2001 05:37 PM
--------------------------------------------------------------------------------
I made another test with the stuff. I mixed it with nitrocellulose to try will it dissolve. The nitrocellulose was really a highly nitrated one. I think it was almost clear pyroxiline. It totally gelled in acetone.
The nitrocellulose did not dissolve in the IPN. It become just wet with the IPN and cold in touching.
Must NC dissolve in IPN, have you got info on it or you just have tried it?
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-24-2001 11:10 AM
--------------------------------------------------------------------------------
Sorry everyone who still can't make it, I forgot I had this from FEMFEP which might help you (it doesn't say to distil it to purify it):
Preparation of Isopropyl Nitrite
A mixture of 45 ml concentrated sulfuric acid, 30 ml water and 110 ml
isopropyl alcohol, previously cooled to 0 centigrades, was added to an ice
cold solution of 114 grams of sodium nitrite (My edit: I assume they mean nitrate here, not nitrite. What they are calling isopropyl nitrite in this text has the formula of C3H7ONO2, they use it in the next step to make sodium azide. I've normally seen this called isopropyl nitrate though.) in 450 ml of H2O. Slow
addition required about two hours in order to maintain a temperature around
0 centigrades. The upper oily layer was separated and washed three times
with 30 ml portions of 5 gram 100 ml sodium bicarbonate solution and 22
grams NaCl 100 ml solution respectively.
[This message has been edited by Mr Cool (edited June 24, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-24-2001 04:18 PM
--------------------------------------------------------------------------------
What is the solubility of other explosives in IPN(nitrocellulose, TNT, urea nitrate ), it will be good to dissolve something in it to higher the viscosity and to make better oxigen balance.
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-24-2001 09:35 PM
--------------------------------------------------------------------------------
I don't get the point of adding H2O to the concentrated H2SO4, is it the alchohol that requires it or the reaction process?
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-25-2001 08:03 AM
--------------------------------------------------------------------------------
Mr Cool the typo error is in the chemical formula...it indeed is a nitrate ester! But nitrite is -ONO not -ONO2!
Nitrites ester are indeed involved in azide formation while nitrate are not!
The process you describe is for isopropyl nitrite, not for the isopropyl nitrate!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-25-2001 08:39 AM
--------------------------------------------------------------------------------
Oh, OK.
Jumala
Frequent Poster
Posts: 200
From: Germany
Registered: OCT 2000
posted 06-25-2001 08:52 PM
--------------------------------------------------------------------------------
NITROGLYCERINE AND NITROGLYCERINE EXPLOSIVES
ISOPROPYL NITRATE
CH3 x CHONO2 x CH3
Isopropyl alcohol has been made recently in large quantities by the catalytic reduction of acetone. The isopropyl nitrate obtained from it has hardly attained any importance as a commercial explosive component on account of its volatility and low explosive strength. Previously it had been made only by a double decomposition of isopropyl iodide and silver nitrate. It boils at 101 to 102°C. Its preparation by direct esterification with concentrated nitric acid, mixed acid, or even by nitric of a specific gravity of 1.4, with which ethyl alcohol or normal propyl alcohol can be easily esterified, is impossible, because in the secondary position the hydroxyl group is subject to oxidation very readily by the nitric acid.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 06-26-2001 05:44 AM
--------------------------------------------------------------------------------
That was Naoum 1924, but in 1955 DESSEIGNE managed the direct nitration of isopropy alcohol with 61% HNO3 in urea saturated solution. (Urbanski 1963)
btw, Jumala u should mail me, i still have something for you...
------------------
for best catfood visit:
kangaroooo.cjb.net
[This message has been edited by wantsomfet (edited June 26, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-26-2001 02:20 PM
--------------------------------------------------------------------------------
I made 5 ml of IPN and tested it to detonation. As i said the IPN looked slightly yellow, it has very low viscosity, high volatility and smells like ether.
I tried to detonate it with 4 grams of AP. I placed the first 2 grams in a detonator(electric) and the second on the top ot the IPN secured with nylon(the AP could have become wet with IPN in this test, I don't know).
The detonation was really nice! Very loud for this quantity of explosive, the plastic container was totally shattered. I think that the IPN detonated.
Jumala
Frequent Poster
Posts: 200
From: Germany
Registered: OCT 2000
posted 06-26-2001 09:08 PM
--------------------------------------------------------------------------------
Yes, I think I must get the Urbanski books somehow. The Naoum is nice but Urbanski is much more up to date.
New Member
Posts: 5
From: Czech republik
Registered: MAY 2001
posted 05-17-2001 02:08 AM
--------------------------------------------------------------------------------
I need precise instruction on production IPN, mixture IPA+HNO3 saturation urea me inject from flask mfuego@mail.ru
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-17-2001 07:22 AM
--------------------------------------------------------------------------------
Take 5 ml of 50%-65% nitric acid, add about 100 mg Urea, cool and add 5 ml IPA, NOT LESS!!! [Using the stoichiometric best amount of IPA, here about 2,5 ml, may cause too much heat generating and decomposion of the mixture.] When you cool the solution you prepared after 1-2 hours a IPN-Phase on the acidic solution should have formed.
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 05-20-2001 04:48 PM
--------------------------------------------------------------------------------
That sounds really great! Can you tell me another way of purifying that doesn't deal with distilling. For example decanting and mixing with water solution of sodium bicarbonate(is IPN(isopropyl nitrate) soluble in water?).
How dangerous not totally purified IPN is?
BoB-
Frequent Poster
Posts: 679
From:
Registered: SEP 2000
posted 05-20-2001 05:05 PM
--------------------------------------------------------------------------------
Dude, you could at least make your question a bit longer than 2 lines, I just checked with my own eyes and Mega's site has information about IPN.
[This message has been edited by BoB- (edited May 20, 2001).]
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-20-2001 05:19 PM
--------------------------------------------------------------------------------
Ehm, I'm confused by simplys post. I believe that IPN is completely not or very little water soluable. And purifying, well, shake an mixture of IPN and carbonate solution, that will bring you acid free IPN and a red carbonate solution. I don't know why it turns red but it does. And mixing acidic IPN with HMTD caused a giant detonation in my laboratory. Thank god there was a plank between me and the BOOOOM........
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-21-2001 07:10 AM
--------------------------------------------------------------------------------
I think that HNO3 + HMTD does generate enough heat to detonate the stuff!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-21-2001 07:32 AM
--------------------------------------------------------------------------------
Of course it does. If not I wouldn't have a crater in my cupboard.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-21-2001 10:01 AM
--------------------------------------------------------------------------------
I think it is a good lesson for you!And for others who read this!
Now you will never manipulate HMTD nor nitric ester without care as if it was suggar!
Mixing explosives can have very anoying side reactions always keep that in mind!One ingredient can make the difference and BOOM!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 05-21-2001 11:20 AM
--------------------------------------------------------------------------------
If I would tell you what happened in my laboratory beside you wouldn't mention this ridiculous explosion to be lesson.
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 05-22-2001 04:40 AM
--------------------------------------------------------------------------------
I read in "Organic Chemistry" book:
"the speed of esterification decreases with the increase of the molecular weight of the alcohols". It was not described why this happens. What is the real chemical explanation of this? The only explanation I can find(for the nitration) is that the O--H bond in the alcohols with low molecular weight is more polar because of the lower +I of the carbon radical.
for examle: o2n-OH + H--och3---}CH3ONO2 + H2O
If the O--H is more polar the water will form easier.
But on the other hand i doubt is the O atom in the alcohols with higher carbon chain more electronegative because of the higher +I of the radical.
I'm confused....
[This message has been edited by simply RED (edited May 22, 2001).]
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-22-2001 05:13 AM
--------------------------------------------------------------------------------
Yes lesson is a bit severe, but a good warning then if you prefer!
Everybody here (wel most of us) have had our lot of accidents-me included!Some have had only material accidents others have been injuried!Hopefully we are stil alive, but now we take more care about what we do!
In french we say:
A cat that has got boiling water on it, is scared about cold water!
I find it too bad that we have to pass trough that to learn to work safely and with safe quantities!
The speed of nitration decreases simply because the viscosity increases (allowing a much less efficient mix), the solubility decreases (since the organic part grows the alcool tends to become hydrophobic-you don't have a proper contact between the reactants!).
Those problems are less effective whith polyols like glycol, glycerol, erythritol, pentaerythritol, sorbitol, suggar, mannitol, cyclohexanhexol,... since then solubility is higher (but the viscosity is stil increasing!).
A good way to diminish viscosity is to heat up the stuff, but unfortunately it is a very bad idea with nitrations since heat has to be low to avoid runaway!!!!!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
mav
New Member
Posts: 5
From: Czech republik
Registered: MAY 2001
posted 06-07-2001 03:10 AM
--------------------------------------------------------------------------------
Hi. I'm found something about make IPN with refer to british patent Have not you is ?
T. Urbanski: Chemistry and Technology of Explosives volume 4 (1984) pg.309
IPN
Direct nitration was found to yield mainly acetone due to the oxidation of the secondary alcoholic group.
However a process of continuous nitration of iso-propyl alcohol in the presence of urea has been described
by Imperial Chemical Industries patents(W.G.Allen and T.J. Tobin-British Patent 696489-1953;749734,749844-1956)
iso-propyl alcohol and urea were introduced into nitric acid (over 40 % HNO3) at its boiling temperature
and a current of air stirred and removed unstable products.
According to Desseige (G.Desseigne, Mém.podres 37,97;1955) the method gave ca. 80% yield. He used nitric acid of over 50 % HNO3 at 108-110 C.
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 06-07-2001 06:11 AM
--------------------------------------------------------------------------------
Yes, I've got the book, too, but that's an industrial procedure. It's difficult to remove the unstable products in this way, also it's not needed to carry out the reaction at elevated temperatures, it works good at room temperature. This way to obtain IPN may work good for industry but not for home labs....
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-18-2001 02:33 PM
--------------------------------------------------------------------------------
I bought 1 litre of IPA and tried to make IPN. The first two attempts failed. The first attempt I mixed 5 ml 60%HNO3 with 4ml Isopropanol and 100mg urea(fine chrystals which did not dissolved). The ingredients were cooled before mixing to 0 degrees celsius. After mixing it was left at 10 gegrees celsius atmosphere(in my fridge). I checked it after 5 minutes.....It has started to bubble and release red fumes! FUCK, I said, and fast dumped it with water, immagine if I haven't checked it it could blast the fridge door abd poison the food .
The next time I tried with 5 ml 55% nitric acid, 5ml IPA and 150mg urea. I did everything at 0 degrees celsius. After 30 minutes it has become yellow, no layers, no nothing, just yellow slowly bulbing shit. I mixed it with 20ml water, and it just diluted, again no layers.
My question is where have I been wrong, Ciplla, you have have made it many times as you said, can you tell me the exact procedure you use(everyone else's help is of course also good).
[This message has been edited by simply RED (edited June 18, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-20-2001 05:12 AM
--------------------------------------------------------------------------------
This is the most uncontrolable reaction I've ever seen. It seems really difficult to make IPN.
I made some more tests with different quantities of urea, IPA, HNO3(60% and 55%). Or they don't react at all or the reaction gets out of control, red fumes,boil and finally a great splash...
Can it really be made without distilation and high temperature acid?
Cipolla
New Member
Posts: 37
From:
Registered: MAY 2001
posted 06-20-2001 08:48 AM
--------------------------------------------------------------------------------
Hmmmm I've made it about 40 times and that works. Of course I also have had a few explosion like reactions, but now .....
Ok, I put about 5 ml HNO3 55% in a test tube, then add urea until i find that it's enough.....you have to find out yourself....then I add about 5 ml IPA and then let the test tube swim in cold water....at first the urea bubbles, ´reacting with the HNO2, and then, after a while, a thick layer of IPN forms on the acid mix. If it doesn't work for you, keep the reaction principle in mind and try again and again.
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-20-2001 05:27 PM
--------------------------------------------------------------------------------
It is midnight now...
I tried the reaction again putting some more urea and not making it at 0 degrees celsius but actually at 4-5 or even more(it may have been 10-12, i don't use termometer).
IT WAS SUCCESFULL, the IPN formed an upper phase on the acidic solution! It looks very slightly yellow, the down solution looks white. While I was purifying it it formed always upper layers, never used pure distilled water but always with some salts. Have you tried it to form a down or upper layer with absolutely clear distilled water(as i read it's density is near 1(mega's site)Another questions : does it dissolve nitrocellulose(if it does I'm gonna make some plastique soon).
I'm happy i finally managed to make it! The yield seems 30-40%.
THANKS FOR THE GREAT HELP AND INFO!
[This message has been edited by simply RED (edited June 20, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-21-2001 05:42 PM
--------------------------------------------------------------------------------
Some more tests with it:
After purifying I tried to burn it. It bured with blue flame(pleasant light blue colour) faster than isopropyl aclohol.
I couldn't purify it 100%. There was always somthing that left unburned(actually really small ammount), but I didn't left it enough time in the separation funnel(improvised one).
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-22-2001 05:37 PM
--------------------------------------------------------------------------------
I made another test with the stuff. I mixed it with nitrocellulose to try will it dissolve. The nitrocellulose was really a highly nitrated one. I think it was almost clear pyroxiline. It totally gelled in acetone.
The nitrocellulose did not dissolve in the IPN. It become just wet with the IPN and cold in touching.
Must NC dissolve in IPN, have you got info on it or you just have tried it?
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-24-2001 11:10 AM
--------------------------------------------------------------------------------
Sorry everyone who still can't make it, I forgot I had this from FEMFEP which might help you (it doesn't say to distil it to purify it):
Preparation of Isopropyl Nitrite
A mixture of 45 ml concentrated sulfuric acid, 30 ml water and 110 ml
isopropyl alcohol, previously cooled to 0 centigrades, was added to an ice
cold solution of 114 grams of sodium nitrite (My edit: I assume they mean nitrate here, not nitrite. What they are calling isopropyl nitrite in this text has the formula of C3H7ONO2, they use it in the next step to make sodium azide. I've normally seen this called isopropyl nitrate though.) in 450 ml of H2O. Slow
addition required about two hours in order to maintain a temperature around
0 centigrades. The upper oily layer was separated and washed three times
with 30 ml portions of 5 gram 100 ml sodium bicarbonate solution and 22
grams NaCl 100 ml solution respectively.
[This message has been edited by Mr Cool (edited June 24, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-24-2001 04:18 PM
--------------------------------------------------------------------------------
What is the solubility of other explosives in IPN(nitrocellulose, TNT, urea nitrate ), it will be good to dissolve something in it to higher the viscosity and to make better oxigen balance.
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 06-24-2001 09:35 PM
--------------------------------------------------------------------------------
I don't get the point of adding H2O to the concentrated H2SO4, is it the alchohol that requires it or the reaction process?
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 06-25-2001 08:03 AM
--------------------------------------------------------------------------------
Mr Cool the typo error is in the chemical formula...it indeed is a nitrate ester! But nitrite is -ONO not -ONO2!
Nitrites ester are indeed involved in azide formation while nitrate are not!
The process you describe is for isopropyl nitrite, not for the isopropyl nitrate!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-25-2001 08:39 AM
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Oh, OK.
Jumala
Frequent Poster
Posts: 200
From: Germany
Registered: OCT 2000
posted 06-25-2001 08:52 PM
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NITROGLYCERINE AND NITROGLYCERINE EXPLOSIVES
ISOPROPYL NITRATE
CH3 x CHONO2 x CH3
Isopropyl alcohol has been made recently in large quantities by the catalytic reduction of acetone. The isopropyl nitrate obtained from it has hardly attained any importance as a commercial explosive component on account of its volatility and low explosive strength. Previously it had been made only by a double decomposition of isopropyl iodide and silver nitrate. It boils at 101 to 102°C. Its preparation by direct esterification with concentrated nitric acid, mixed acid, or even by nitric of a specific gravity of 1.4, with which ethyl alcohol or normal propyl alcohol can be easily esterified, is impossible, because in the secondary position the hydroxyl group is subject to oxidation very readily by the nitric acid.
wantsomfet
Frequent Poster
Posts: 236
From: EU
Registered: JAN 2001
posted 06-26-2001 05:44 AM
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That was Naoum 1924, but in 1955 DESSEIGNE managed the direct nitration of isopropy alcohol with 61% HNO3 in urea saturated solution. (Urbanski 1963)
btw, Jumala u should mail me, i still have something for you...
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[This message has been edited by wantsomfet (edited June 26, 2001).]
simply RED
Frequent Poster
Posts: 240
From: HELL
Registered: OCT 2000
posted 06-26-2001 02:20 PM
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I made 5 ml of IPN and tested it to detonation. As i said the IPN looked slightly yellow, it has very low viscosity, high volatility and smells like ether.
I tried to detonate it with 4 grams of AP. I placed the first 2 grams in a detonator(electric) and the second on the top ot the IPN secured with nylon(the AP could have become wet with IPN in this test, I don't know).
The detonation was really nice! Very loud for this quantity of explosive, the plastic container was totally shattered. I think that the IPN detonated.
Jumala
Frequent Poster
Posts: 200
From: Germany
Registered: OCT 2000
posted 06-26-2001 09:08 PM
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Yes, I think I must get the Urbanski books somehow. The Naoum is nice but Urbanski is much more up to date.