Sciencemadness Discussion Board - Synthesis checks for HMTD

Synthesis checks for HMTD

Arcus - 26-9-2020 at 09:56

I plan on synthesising some HMTD for fun in the coming days, but I just want to check that I am doing everything as safe as possible, so I don't blow something up in my face.
I have HMTA, and I will react it with Hydrogen Peroxide under a citric acid catalyst. This will be done using an ice bath. With a rough 50% yield (what it says on the wiki page) I should get about 4g using 5.4g of the HTMA.

Are there any other 'this is vitally important' thing I need to know before cracking on with is?

ArbuzToWoda - 26-9-2020 at 09:59

Yeah - keep the reaction below 8C at ALL TIMES. Using lower concentration of peroxide is actually better. Runaway reactions happen VERY READILY with this compound and your whole shed/house/balcony will stink of piss and your nose will die of the sour, putrid feeling if you inhale any of the fumes.

Please be careful.

Arcus - 26-9-2020 at 11:53

I have 12% peroxide - is that okay? it's a garage btw

[Edited on 26-9-2020 by Arcus]

ArbuzToWoda - 26-9-2020 at 12:05

It is okay. A couple of years ago, when I attempted this preparation I found some very old thread on some HTML forum with many writeups that proved useful. Can't find it now, but you should look for it before proceeding.

aromaticfanatic - 26-9-2020 at 16:21

Quote: Originally posted by Arcus

I just want to check that I am doing everything as safe as possible, so I don't blow something up in my face.

Are there any other 'this is vitally important' thing I need to know before cracking on with is?

Just stay away from HMTD and TATP. TATP is worse but HMTD is right behind it. 4 grams is enough to really fuck yourself up with. Unless you are really experienced or already knew stuff like PPE at all times and not handling it directly, I'd say to not make it. If you already knew that I assume you knew about the other hundreds of rules to keep yourself safe.

HMTD is nothing to take lightly at all. People say it isn't too sensitive if made right but in the end it's still an organic peroxide which are notoriously known for being unpredictable. So let's say 9 people had the safer stuff but 1 had even more sensitive crap using the same synthesis, would you be fine being that 1 guy? I'd look into other primaries because HMTD is one of those that will eventually blow up since you will make a mistake at some point. The difference between those who keep fingers and those that don't is that they chose better primaries.

Of course you can ignore everything I just said and go your way but I wouldn't if I were you.

Keep temp as low as possible, use weaker acids and don't use sulfuric or HCl, use citric acid, and do not store it. In the US storing is illegal and even though HMTD doesn't sublimate into the container as fast as TATP, I believe there is still some volatility but worst of all is that it is easy to get some grains in the container opening area and twisting, pulling, and vibrations can set it all off. I don't think HMTD will detonate when under water but why take the risk? It's easy enough to make so make the exact amount you need.

Joeychemist - 26-9-2020 at 21:32

The Sciencemadness-wiki page on HMTD is too short and poorly written to be considered a serious reference for a procedural writeup that no one should use as their main source. The reference linked to at the bottom of the wiki page are all valuable sources of information though.

For example the author seriously contradicts himself by way of poor wording as the article reads;

"NEVER STORE HMTD! Try to use it as soon as possible.

A SM user has discovered that HMTD can be safely stored at -10 °C, with no signs of any decomposition, even after 15 years"

You should read all the referenced science madness threads in said HMTD wiki page before you fuck around and loose fingers... If you were ready to make organic peroxides you'd know that 12%H2O2 is fine. Though, you need to adjust your reactants stoichiometrically of course and amore dilute rxn. naturally means your catalyst (the citric OR HCl acid) will be more dilute in action and slow the rxn. Temperature also affects the time the rxn. takes to complete. I used to have to leave the flask in the fridge for a few days sometimes with more dilute H2O2.

Good luck, don't hurt anyone else...

hissingnoise - 27-9-2020 at 00:40

Quote:

The the author seriously contradicts himself by way of poor wording.

It's worth noting, too, that HMTD undergoes a slow decomposition in water.

(Why, oh why, do so many people misspell "lose"?)

B(a)P - 27-9-2020 at 01:47

Handle it like it is going to donate at any second. Any amount larger than a match head that detonates in your hand will do you damage. Any particular reason you are making HMTD?

hissingnoise - 28-9-2020 at 00:55

Quote:

Handle it like it is going to donate[sic] at any second

HMTD is relatively safe to handle and is a very effective primary ─ washed with water with a final rinse in ethanol, it is stable when stored dry at low temperature.

Ignited unconfined in small quantities, it simply deflagrates.

[Edited on 28-9-2020 by hissingnoise]

B(a)P - 28-9-2020 at 12:09

Quote: Originally posted by hissingnoise

Apologies for the typo, but I still stand by what I said.
It is quite sensitive to static discharge and is dramatically sensitised in contact with some other compounds, including many metals. A drop of concentrated sulfuric acid on 50 mg will make it detonate.
If the OP is making it for the first time I think my recommended precautions can only help.
To clarify I did not intent to indicate that it was not a usable primary.

aromaticfanatic - 4-10-2020 at 11:03

Quote: Originally posted by hissingnoise

Quote:

Handle it like it is going to donate[sic] at any second

Ignited unconfined in small quantities, it simply deflagrates.

[Edited on 28-9-2020 by hissingnoise]

I think you need to learn that organic peroxides are unpredictable as can be.

I think you also need to learn the concept of self confining.

Mix the two together and you have HMTD.... HMTD detonating in your hands.

Just leave them at bay. There's a reason they get a bad rap.

hissingnoise - 5-10-2020 at 01:00

Quote: Originally posted by aromaticfanatic

Quote: Originally posted by hissingnoise

Ignited unconfined in small quantities, it simply deflagrates.
[Edited on 28-9-2020 by hissingnoise]

I think you also need to learn the concept of self confining.

Which part of "small quantities" are you having trouble with?

aromaticfanatic - 6-10-2020 at 17:12

Quote: Originally posted by hissingnoise

Quote: Originally posted by aromaticfanatic

Quote: Originally posted by hissingnoise

Ignited unconfined in small quantities, it simply deflagrates.
[Edited on 28-9-2020 by hissingnoise]

I think you also need to learn the concept of self confining.

Which part of "small quantities" are you having trouble with?

What part of HMTD is an unpredictable and highly sensitive explosive are you have trouble with?

I can give you a few examples of how explosives don't behave like they should even in "small quantities." Put a number to that. Is 1 gram a small quantitiy? Or 10mg? I'd go with the latter. 10mg of HMTD is fine but 1 gram is reaching to the power of a #8 detonator which will cause devastating damage.

Pyro_cat - 17-4-2021 at 19:40

Quote: Originally posted by Arcus

I have 12% peroxide - is that okay? it's a garage btw

[Edited on 26-9-2020 by Arcus]

If thats the hair bleach, 40 volume, the bottle I had said contains phosphoric acid.

I did not have any problems with AP or MEKP using it but that doesn't mean its not a problem for hmdt, something I never made.

I had good results concentrating the usual 3% well past 12% for those projects.

Beaker full in the toaster oven @ 250 F door slightly propped open for steam escape, evaporate 90% theoretically your at 30% never tested it but its stronger then the 12% for sure.

Like everyone else said watch out these peroxide concoctions, that deflagration makes it seem like its somewhat benign but its not.

Messed with small amounts, probably did that friction test like 50 times messing around with the anvil with ear muffs on alternating between flame, impact and friction tests "this stuff is not so bad" then the 51st friction test much less pressure then some of the previous ones and a crystal broke and it popped.

[Edited on 18-4-2021 by Pyro_cat]

Pyro_cat - 17-4-2021 at 19:57

Quote: Originally posted by aromaticfanatic

I think you also need to learn the concept of self confining.
.

Also an amount below the threshold of self confining will still detonate if you come at it too slowly with the torch and melt the top layer making that insanely sensitive liquid that goes directly to DDT setting of the rest of it.

That little pile you expected to fireball pops DDT instead.

I learned this after the bright idea lets melt some in a spoon taped to the end of a 6 foot long stick that should have warned me that possibility after seeing how it reacts in liquid form.

caterpillar - 18-4-2021 at 03:15

Runaway is possible. The reaction goes slowly. Temp must be kept below 20 Celsius. I read that 50% H2O2 must be used, but I had 30% only. I dropped temp down again and again but after two hours I thought, that the temp won't grow up and left the room. After some time I got runaway.

XeonTheMGPony - 18-4-2021 at 05:46

If you are starting to do this now, take the advice others have given and treat this stuff like glowing toxic waste that is out to get you.

All so look up Explosionpedia He gives a reliable route, just scale it down as he made an insane amount at 1 go.
It does store well but loses power as time goes on, I had some stored over a year and noticed decrease in power so deflagulated the lot of it.

As you learn its behavior you will learn what it is like IRL depending on goals if pyrotechnics is going to be a long one invest in glass wear and get some resorcinol and make much better primaries and first strike compositions!

RustyShackleford - 18-4-2021 at 08:24

12% peroxide definitely works, but its quite low yield, but that doesnt matter so much since you shouldnt be making large amounts anyway

hissingnoise - 19-4-2021 at 06:32

Quote: Originally posted by Pyro_cat

I learned this after the bright idea lets melt some in a spoon taped to the end of a 6 foot long stick that should have warned me that possibility after seeing how it reacts in liquid form.

How verrry interesting?

The HMTD you prepared must've been quite markedly different to mine ─ what I had didn't melt under any circumstance...

The damp substance, though, fumed off in a quick decomposition when ignited.

[Edited on 19-4-2021 by hissingnoise]

Pyro_cat - 19-4-2021 at 21:28

The spoon experiment was AP: Melting point 131.5 to 133 °C (dimer) (91 °C (trimer)

Small amount that would deflagrate in the powdered form when liquified it DDT hard and puts a dimple in the spoon. Was a good thick teaspoon too not cheap junk. Not a full spoon either no way. less then 1/4.

Looking at the specs for HMTD: Melting point Decomposes at 75 °C Ignites spontaneously at 133 °C

I guess maybe that's what makes HMDT 'safer' it does not melt into a liquid that detonates in such small amounts.

My mistake, they are said to be so similar I just figured it had a melting point too.

How does Wiki spec work ? Decomposes at 75 °C Ignites spontaneously at 133 °C

How does something that's decomposed (separated into constituent parts or elements or into simpler compounds) then it ignites as the original stuff ?

I don't get it. What goes on with this stuff ?

TheMrbunGee - 20-4-2021 at 08:05

Quote: Originally posted by Pyro_cat

How does Wiki spec work ? Decomposes at 75 °C Ignites spontaneously at 133 °C

How does something that's decomposed (separated into constituent parts or elements or into simpler compounds) then it ignites as the original stuff ?

I don't get it. What goes on with this stuff ?

I guess decomposition is not instant, imagine putting some in oven @ 75° and it will break down slowly, put some in @ 100° and it will do so way faster , but @133° C + it will ignite, and there is nothing slow about that.

Bedlasky - 8-5-2021 at 01:17

I came across this video today:

https://www.youtube.com/watch?v=I_WDtw-prDw

Firstly: How can be someone so stupid to blow up 300 g of HMTD?

Secondly: I doubt that he blow up 300 g HMTD, explosion was too small for such a huge amount.

katyushaslab - 8-5-2021 at 06:58

Multi gram amounts of organic peroxides is asking for accidents, tbh. I'd advise scaling down. You don't need a particularly large amount of HMTD to explore its properties.

Bedlasky - 8-5-2021 at 11:34

I don't plan to make HMTD, I am not interested in organic peroxides. I just think that this video is fake.

hissingnoise - 9-5-2021 at 06:56

Quote: Originally posted by Bedlasky

I don't plan to make HMTD, I am not interested in organic peroxides. I just think that this video is fake.

You are probably right on both counts, but IMO, HMTD is relatively safe when pure and when stored cool and dry.

A prolonged wash with distilled water is required, of course.

As is a final rinse with 95% ethanol to speed up drying to minimise decomp. due to hydrolysis...

[Edited on 9-5-2021 by hissingnoise]

Laboratory of Liptakov - 9-5-2021 at 08:37

The center of the stump is undamaged. Plus, there's a white powder. If it was 300g HMTD, the stump would be divided into at least 4 pieces up to ground level. And there will certainly be no white spots on the stump. Description is bullshit.

hissingnoise - 10-5-2021 at 01:56

'Way too easy to accidentally add that extra zero when you're talking about a mere 30 grams...?

Pyro_cat - 9-6-2021 at 17:52

Quote: Originally posted by katyushaslab

Multi gram amounts of organic peroxides is asking for accidents, tbh. I'd advise scaling down. You don't need a particularly large amount of HMTD to explore its properties.

Its almost like the stuff was designed to cause accidents.

The way it deflagrates creates this false sense of security that nothing bad is likely to happen. IMO that is its most dangerous property.

Nothing bad happened but I made the mistake early on thinking my small amount in a small container with just a saran wrap top to was safe. That no way pressure could build.

Later experiments I learned confine that stuff at all and it doesn't deflagrate it pops.

A small sub gram pile deflagrates in the open air but just the confinement of a paper cup upside down with some sand on top changes everything.

I put the smallest amount in a pen cap when I was first exploring. I was sloppy and the residue on the outside premature ignition plastic hit me I was bleeding.

hissingnoise - 10-6-2021 at 02:16

Indeed. This is one news item I'll not forget in a hurry...

https://www.ctvnews.ca/chemistry-student-killed-by-exploding...