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plasma
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Organic peroxides
What is this and how can I make it.
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madscientist
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Organic peroxides are a type of chemical. Many are explosive in nature. They are organic compounds (compounds based off of a carbon structure) that
contain a peroxide group (a pair of oxygen atoms joined by a single bond). There are many explosive organic peroxides: tricylcoperoxyisopropanone
(CH3COOCH3)3 (commonly known as trimeric acetone peroxide) methyl ethyl ketone peroxide, HMTD... I am thinking that it would be possible to form
aceteldehyde peroxide and / or formaldehyde peroxide.
I weep at the sight of flaming acetic anhydride.
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plasma
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Is it possible to get a receipt on a organic peroxide ?
Bt the way, I found Methylketonperoxide in my garage, this sounds like a organic peroxide to me but I isn't exploding. It just burns vigoursly. Does
it have to be in a confined space to explode ?
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Polverone
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Methyl ethyl ketone peroxide is indeed an organic peroxide. It is a poisonous, irritating, explosive liquid. It is used to catalyze the hardening of
resins, as with fiberglass. I assume this is how you come to have some in your garage. However, the stuff sold as a catalyst it certainly NOT pure MEK
peroxide! Here's some information from Smith Fiberglass about their MEK peroxide catalyst:
Methyl ethyl ketone peroxide: 0-10%
Dimethyl phthalate: 10-60%
Hexylene glycol: 1-10%
Methyl ethyl ketone: 0-5%
Hydrogen peroxide: 0-5%
Not too long before the Forum went down, there was a thread on MEK peroxide. It can be prepared like acetone peroxide, substituting methyl ethyl
ketone for the acetone. It can be set off by shock and heat. Unlike many other organic peroxides, it is a liquid, so it can't form dangerous crystals.
However, the limited information available should discourage an inexperienced experimenter from preparing it.
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plasma
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The bottle I found was a catalyst. The label says that it contains 30-60% methyl ethyl keton peroxide. But it won't explode. It just burns vigoursly.
I need a explosion powerfull enough to set of AN, but it doesn't seem like organic peroxides will work. Do you now about any ways to make the AN more
sensitive (much more).
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madscientist
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I would forget trying to set off pure ammonium nitrate. I would make ANFO with it (about 96% prilled ammonium nitrate, 4% diesel or other liquid
hydrocarbon fuel). You will still need a relatively powerful detonator. If you do not have the resources to prepare common detonators (for example,
lead azide, mercury fulminate, etc.) you will need to make organic peroxides. Look here for more information on organic peroxide explosives like HMTD
and AP. http://wind.prohosting.com/megaback/megalomania/index.html
I weep at the sight of flaming acetic anhydride.
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plasma
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I found this information on :
ACETONE PEROXIDE - mix by volume 3 parts 6% peroxide to 2 parts acetone in a
glass jar, leave 30 min, add 2 parts hydrochloric acid and let sit overnight.
White crystals will form out of the mixture, these are the explosive which are filtered and dried.
HMTD - Dissolve 2 parts hexamine in 4 parts 6% peroxide, add 2 parts hydrochloric acid and let sit overnight. A white fluffy powder will form which is
HMTD, filter and dry as with acetone peroxide.
These are explosives that are usually underestimated in power and sensitivity.
4 grams of either of these will take off a hand of anyone careless enough to
make and misuse this material.
Many files recommend using them strait for detonation of ammonium nitrate, don't bother, it won't work.
This last sentence is very confusing. :/
Thanks for the wonderful link madscientist
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Polverone
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That's a pretty good writeup that you found. Note that the fireball picture on the page is certainly from a *deflagration* - quick burning - of
acetone peroxide rather than a detonation. When exploding, I have seen at most a dull orange flash with acetone peroxide. The last sentence on the
page may mean a couple of things: 1. Ammonium nitrate will not explode with initiation from organic peroxides. This is perfectly reasonable since pure
ammonium nitrate is *extremely* difficult to detonate, and there is in fact debate whether the pure compound will every experience a self-sustaining
explosion. 2. Ammonium nitrate blasting agents will not explode with initiation from organic peroxides. I would beg to differ with this. Success in
setting off ammonium nitrate blasting agents will vary with the composition of the agent, its manner of preparation, and choice, quantity, and
placement of the initiating agent.
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plasma
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I have successfully made AP but one thing is bothering me, the process needs very much acid when using 6% hydrogenperoxide, here are my ideas:
(CH3)2CHOH O2 -} (CH3)2CO H2O2
isopropyl dioxide -} Acetone Hydrogenperoxide
My problem is how to oxidize the isopropyl, can it can it be done by bubbling carbondioxide through it like this:
(CH3)2CHOH 2CO2 -} (CH3)2CO H2O2 2CO
Or like this:
(CH3)2CHOH CO2 -} (CH3)2CO H2O2 C
Are any of this reactions correct ?
I belive that these reactions would give relatively pure Acetone and Hydrogenperoxide, if they are correct.
Please correct me if I'm wrong 
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Polverone
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Your equations are confusing. Please consider using the + symbol. Carbon dioxide will not easily oxidize anything but the most powerful reducing
agents. If you hope to change isopropanol by bubbling CO2 through it you're out of luck. Please clarify if I've misinterpreted what you're saying.
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plasma
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I looks like the spell checker removes the + symbol after checking. It seems like you got the point, if not I will try to make it a bit clearer. I
read in a encyclopedia that if isopropanol is oxidized it will create acetone and hydrogenperoxide. My calculations said that this solution would
contain 64% acetone and 36 % hydrogenperoxide (by weight). With hydrogenperoxide as concentrated as this, the amount of acid used in AP processing
could be lowered very much. So my idea was to oxidize the isopropanol by bubbling CO2 trough it (which apparently won't work).
Do anyone know isopropanol can be oxidized
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madscientist
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I don't see why the oxidation of isopropanol would form hydrogen peroxide. Isopropanol would probably be oxidized by KMnO4. I find the following to be
more likely:
6(CH3)2HCOH + 2KMnO4 --> 5(CH3)2CO + (CH3)2HCOH + 4H2O + 2KOH + 2MnO
I weep at the sight of flaming acetic anhydride.
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plasma
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I found this equation in a encyclopedia at my school:
(CH3)2CHOH + O2 -} (CH3)2CO + H2O2
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Polverone
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You will notice that your encyclopedia equation is using oxygen, not carbon dioxide. Also, I do not believe that isopropanol deteriorates in ambient
conditions on exposure to atmospheric oxygen. In other words, if the reaction does take place as shown (which seems kind of dubious - H2O2 is not a
very stable molecule), it almost certainly takes place under extreme reaction conditions - high temperatures/pressures, or maybe with the aid of a
catalyst. What encyclopedia was this from, BTW?
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plasma
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I know the encyclopedia used oxygen not carbon dioxide, that was just my theory on oxidizing the isopropanol since I can't get pure oxygen.
I found the equation under "isopropanol" in a Norwegian encyclopedia which is called "Aschehoug".
The encyclopedia said nothing about pressure, temperature or catalysists.
BTW, I made AP today, and now just one hour after I added acid, a 5mm layer of crystals has appeared (tube dia. 5 cm). This is the ingredients that I
used :
36 ml Acetone
24 ml 1-5% Hydrogenperoxide
3 ml 50-60% Sulfuric acid
Considering that it just have been standing for one hour, is this a high yield ?
(Yes I'm Norwegian)
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madscientist
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Excerpt from one of my chemistry texts:
There are many organic peroxides and hydroperoxides.
Peroxo carboxylic acids, for example peracetic acid,
CH3C(O)OOH, can be obtained by the action of H2O2 on
acid anhydrides. The peroxo acids are useful oxidants
and sources of free radicals, for example by treatment
with Fe(2+) (aq). Benzoyl peroxide and cumyl
hydroperoxide are moderately stable and widely used
where free radical initiation is required, as in
polymerization reactions.
Organic peroxo compounds are also obtained by
autoxidation of ethers, alkenes, and the like, on
exposure to air. Autoxidation is a free radical chain
reaction initiated by radicals generated by
interaction of oxygen and traces of metals such as Cu,
Co, or Fe. The attack on specific reactive C-H bonds
by a radical (X*), first gives R* and then
hydroperoxides that can react further.
RH + X* --} R* + HX
R* + O2 --} RO2*
RO2* + RH --} ROOH + R*
Explosions can occur on distillation of oxidized
solvents. These solvents should be washed with
acidified FeSO4 solution or, for ethers and
hydrocarbons, passed through a column of activated
alumina. Peroxides are absent when the Fe(2+) + SCN-
reagent does not give a red color indicative of the
Fe(SCN)(2+) ion.
I weep at the sight of flaming acetic anhydride.
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plasma
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I have still not made HMTD succesfully, and I think it's because my fuel sticks isn't methamine. My fuel sticks are black, burn very slow and smells
and looks a bit like charcoal. They aren't soluble at all. The name of the fuel sticks are "Solid fuel sticks" and the brand is "Jimmy" (From America)
Where to get methamine fuel tablets ?
Thanks
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madscientist
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Hexamethylenetetramine (also called "hexamine" or "methanamine") is also sold as "Urotropine", a urinary antiseptic.
I weep at the sight of flaming acetic anhydride.
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plasma
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This is ment for reodor felgen, if he has found his way into the new forum.
(Norwegian)
Ammonium nitrat fåes kjøpt i sports butikker som isposer for ca. 16 kr. Det er veldig enkelt og lage natrium nitrat av ammonium nitrat. Det gjøres
slik :
NaOH + NH4NO3 -> NaNO3 + NH4OH
Bland et mol natrium hydroksyd med et mol ammonium nitrat i vann. Dette bør gjøres på et godt ventilert sted siden det frigjøres mye ammonium
hydroksyd gass. Nå gjenstår det bare å koke løsningen for å få fordampet vekk ammonium hudroksydet og vannet. Krysstaller kommer til syne etter
vært.
Natrium nitrat har de samme egenskapen som kalium nitrat men virker mer oksyderende. (har ikke mye å si)
Jeg tar gjerne imot mer informasjon om heksametylentetramin tablettene dine.(ice8@sol.no)
Vet du for man kan få tak i salpetersyre ?
Jeg bor i en liten bygd i vest-telemark.
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reoder felgen
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Thanks plasma.
dette er også slik jeg får tak i NaNO3 og NH4NO3, men glemte å ta det med når jeg lagde listen. er du sikker på at gassen som dannes er NH4OH og
ikke NH3 + H2O? men det betyr forsåvidt ikke så mye. Heksametylentetramin kjøpte jeg på en liten "chemist sypply house" (kommer ikke på noe bra
norsk ord), men de leverer først og fremst til skoler o.l. tviler på at du har den samme butikken i telemark. virket som en "famile greie" altså
ikke en kjede.
salpetersyre har jeg aldri sett og tviler sterkt på at jeg noen gang kommer til å få se det. vurderer å lage det ved å blande så ren som mulig
svovelsyre med kalsiumnitrat (ikke kalium) for så å filtrere kalsiumsulfatet bort på en eller annen måte. virker bra for da trenger jeg ingen
destilering!
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plasma
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(Norwegian)
Kunne du kjøpt heksametylentetramine til meg og sendt det med postoppkrav. Jeg tror ikke jeg kommer meg til Kristiansand med det første. Hvis du
mailer meg på denne adressen ice8@sol.no kan jeg sende deg navn og adresse. Jeg er svært takknemlig hvis dette er gjennomførbart. Det hadde også
vært interresant å vite hva slags andre ting de selger i denne butikken også.
Thanks
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PHILOU Zrealone
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I'm not norvegian although, I understand German, Dutch and English quite wel, I can figure out some terms in Norvegian!
Anyway:
Urotropine/Hexamine/hexamethylenetetramine can be done quite easily from conc NH3 and conc CH2=O solutions:
Add an excess of freezing cold NH4OH solution (max is 30% NH3 per weight) to a freezing cold one of CH2=O (formol/formaldehyde solution is max 40% by
weight over it deposit a precipitate of polyformal).Mix the two in stoechiometric amounts following the formula:
6CH2=O + 4NH3 --> C6H12N4 + 6H2O
Taking care to have a slight excess of NH3 solution of 20 to 30%!
It will heat a little reason why we have cooled the solution prior to reaction-sothat reactants are not lost in gases form and inhalated by
experimentator.
Allow to stir for an hour and then warm up to 40°C and allow to evaporate as long as it needs to get cristaline/solid!Exces NH3 will take off quite
fast! Yield 100%!
PH Z
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plasma
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How can CH2=O be made ?
Thanks
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madscientist
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Here's a good opportunity for this:
I'm theorizing that CH2O could be prepared from CH2Cl2 and NaOH.
CH2Cl2 + 2NaOH --> CH2(OH)2 + 2NaCl --> CH2O + 2NaCl + H2O
I weep at the sight of flaming acetic anhydride.
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PHILOU Zrealone
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CH2=O can indeed be done by CH2Cl2 in the presence of NaOH (solid); the process require a long time if both reactants aren't brought into contact by
an amphiphil solvant...would you expect Water soluble NaOH to be soluble in unwater soluble CH2Cl2?
But once it is done, a vigorous exothermic reaction may take place and possibly generate in situ suffocating gases like Cl-CH2-OH (a very toxic and
reactive gas), CH2=O, Cl-CH2-O-CH2-OH (must also be quite unfriendly)!
If it doesn't start on its own, you would have to heat a little but (dichloromethane is quite volatile) and no big heat can be acheived unless under
pressure...what I strictly discourage you to do since the container might explode du to exothermic reaction and volatilisation of volatile liquid and
libération of gases!!!
A much wiser way to make CH2=O is by reacting CH3OH with a strong oxydiser in acidic media!
I would recomand to make a concentrated solution of KMnO4 or K2Cr2O7 in H2SO4; then to drop drop by drop methanol in it(under agitation)...then try to
keep T arround 40°C (by cooling if it goes too exothermic) or by gentle heating!
Formaldehyde will form and volatise (thanks to the fact it is a gaseous aldehyde and thanks to the 40°C); part of it will dissolve in the solution
(since it is quite avid of water) and perform a further oxydation into formic acid and carbonic acid!
The use of a cold trap with stirred water in it will allow you to catch most of its gaseous evolution!
Water boild at 100°C
Methanol at 65°C
Formic acid at 101°C
Carbonic acid at ambiant pressure (CO2 + H2O)
So it is very important to keep the reactor at 40°C to avoid boiling the methanol!
CH3-OH + -Oxydiser/H(+)-> CH2=O + H2O
CH2=O + -O-> HCO2H -O-> H2CO3 --> CO2 + H2O
CH2=O + H2O --> CH2(OH)2 (hydrate of methanal)
You could also use a clod trap with NH4OH sothat the CH2=O will be catched immediately as CH2=NH that will condensate into hexamine!
CH2=O + H2NH --> CH2=NH + H2O
6CH2=NH --> C6H12N4 + 2NH3(g)
Enjoy!
BTW, Madscientist and others, I have replied to many treads in all chapters of this NG!
PH Z
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