Sciencemadness Discussion Board - methyl nitrate

methyl nitrate

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Ral123 - 27-9-2012 at 09:11

I just found my old 2.5cc model aircraft engine. First I discovered that it can run with methanol and car oil

Then of course I nitrated some methanol... That thing greatly increased power, above like 30% there are spectacular deflagrations in the engine with flames from both the intake and the exhaust when I apply current to the hot wire(platinum coated of some kind). It also tends to not need current at all. I'll see what happens with more if I gather courage. Damn I can sell it like super powerful diesel engine

I never thought one day I'd wish my rdx and tetryl were also liquid

killswitch - 12-10-2012 at 11:35

Quote: Originally posted by Ral123

I just found my old 2.5cc model aircraft engine. First I discovered that it can run with methanol and car oil

I never thought one day I'd wish my rdx and tetryl were also liquid

You're gonna get someone killed. Irrespective of its energetic properties, MeNO₃ vapor is an incredibly potent vasodilator. Its volatility is so great that it could easily reach levels that knock someone out. Use a heavier ester and wear gloves, long pants, close-toed shoes, a jacket, and eye protection at all times.

In addition, MeNO₃ is the only nitric ester in the polyol series (EGDN, NG, ETN, XPN, MHN) with a negative oxygen balance. It's only marginally better than nitromethane as a fuel additive.

It would probably be safer to use nitroglycerin as an additive than methyl nitrate. EGDN is preferable, however.

franklyn - 16-10-2012 at 23:45

@ AJKOER

What a farrago of misconceived notions.

Boiling KNO3 in HCl will not displace HNO3 , so why should you suppose
that the covalently bound Cl of CH3Cl will.
The only scheme of this type that works is with , N I T R I T E since it
forms a weaker acid than Chlorine and so can be displaced.
http://www.sciencemadness.org/talk/viewthread.php?tid=3901&a...

U P D A T E
As always exceptions exist as shown here below _

Substitution of a Halogen by -NO3.gif - 10kB

I still remain skeptical that the proposed synthesis of CH3ONO2
in this manner is realistic. By your own reference in this other post
http://www.sciencemadness.org/talk/viewthread.php?tid=21529#...
at the bottom of the indicated page 279
http://books.google.com/books?id=aBAFAAAAQAAJ&pg=279

" It's alchoholic solution precipitates Silver Nitrate rapidly. "
In other words the reaction is reversable , and that's with
Iodine , it is also shown above for a secondary alcohol
with Bromine. Chlorine is dubious.

__________________________________________

With regard to this cited reference
http://www.docstoc.com/docs/68188299/CHAPTER13
for this _
CH3Cl + NH3 --> CH3NH2.HCl --> CH3NH2.HCl + NH3 --> CH3NH2 + NH4Cl
the first part is correct , . . . . . . . . . . . . . . . . .this next part is very wrong

Ammonia is a weaker base than Methylamine so it cannot displace it to
form NH4Cl with HCl. See _
http://www.chemguide.co.uk/basicorg/acidbase/bases.html
Comparing the strengths of weak bases

From above here _
http://www.sciencemadness.org/talk/viewthread.php?tid=744&am...
Methyl nitrate is prepared by distilling 50 grams of NaNO3 with 50 grams of
Methyl alcohol and 100 grams of sulfuric acid, in a retort without external
heating. It is a colorless liquid density 1.182 at 20 ºC (68 ºF); boils at 60 ºC
(140 ºF); has a faint ethereal oder. It's vapor detonates when heated to
150 ºC (302 ºF).
Heated with alcoholic ammonia , it yields methylamine nitrate , CH3NH2 • HNO3

It follows that CH3Cl heated with ammonia will result in CH3NH2 • HCl

bio2 posted this
http://www.sciencemadness.org/talk/viewthread.php?tid=3901&a...

Other ways to get there
http://en.wikipedia.org/wiki/Methylamine
http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0347
http://www.erowid.org/archive/rhodium/clandestine/methylamin...

Methylamine threads
http://www.sciencemadness.org/talk/viewthread.php?tid=1261
http://www.sciencemadness.org/talk/viewthread.php?tid=7410

[Edited on 18-10-2012 by franklyn]

hissingnoise - 17-10-2012 at 03:04

Quote:

Methyl nitrate is prepared by distilling 50 grams of NaNO3 with 50 grams of Methyl alcohol and 100 grams of sulfuric acid, in a retort without external heating.

<i>"Without external heating"?</i> WTF!

The distillation is extremely sensitive ─ a couple of degrees above the ~66°C B.P. will produce a spectacular runaway (great eruption of NO₂ vapour) as I found, distilling methyl nitrate from a mixture of the alcohol and concentrated (~68%) HNO₃!
Also, small quantities only to ensure a runaway doesn't progress to deflagration ─ or worse . . .

hissingnoise - 17-10-2012 at 03:31

Quote:

"Without external heating"

Is an exotherm produced on mixing the reactants, perhaps?

Kalium - 17-10-2012 at 19:09

Quote: Originally posted by killswitch

In addition, MeNO₃ is the only nitric ester in the polyol series (EGDN, NG, ETN, XPN, MHN) with a negative oxygen balance.

Perhaps with the exception of PETN.

PHILOU Zrealone - 19-10-2012 at 07:59

Quote: Originally posted by Kalium

Quote: Originally posted by killswitch

In addition, MeNO₃ is the only nitric ester in the polyol series (EGDN, NG, ETN, XPN, MHN) with a negative oxygen balance.

Perhaps with the exception of PETN.

Fist CH3-ONO2 is derived from a mono-alcohol and can't be member of the polyol family.

Secondly propandiol, butandiol dinitrate and many other polyols polynitrate esters also display negative OB.

[Edited on 19-10-2012 by PHILOU Zrealone]

AJKOER - 24-10-2012 at 14:27

Quote: Originally posted by franklyn

.......
With regard to this cited reference
http://www.docstoc.com/docs/68188299/CHAPTER13
for this _
CH3Cl + NH3 --> CH3NH2.HCl --> CH3NH2.HCl + NH3 --> CH3NH2 + NH4Cl
the first part is correct , . . . . . . . . . . . . . . . . .this next part is very wrong

Ammonia is a weaker base than Methylamine so it cannot displace it to
form NH4Cl with HCl. See _
http://www.chemguide.co.uk/basicorg/acidbase/bases.html
Comparing the strengths of weak bases
......

Franklyn, per one of your supplied references, in particular [5] cited below (http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0347 ):

"3. Discussion
Methylamine can be prepared by the action of ammonia on methyl iodide [4], methyl chloride [5], dimethyl sulfate [6], methyl p-toluenesulfonate [7] and methyl alcohol with a catalyst and at elevated temperatures [8] by the action of bromine and alkali [9] and of bleaching powder [10] on acetamide; by the action of sodamide on methyl iodide [11] by the reduction of chloropicrin [12], hydrocyanic or ferrocyanic acid [13], hexamethylenetetramine [14], nitromethane [15], methyl nitrite [16], or formaldoxime [17] from acetyl chloride and sodium azide [18] and by the action of formaldehyde on ammonium chloride [19].

References and Notes

1. Sharp and Solomon, J. Chem. Soc. 1477 (1931).
2. Werner, J. Chem. Soc. 111, 850 (1917).
3. Sommelet, Compt. rend. 178, 217 (1924).
4. Hofmann, Ann. 79, 16 (1851).
5. Vincent and Chappuis, Bull. soc. chim. 45, 499 (1886).
6. Ephrian and Gurewitsch, Ber. 43, 139 (1910); Denham and Knapp, J. Chem. Soc. 117, 236 (1920).
7. Rodionov, Bull. soc. chim. (4) 45, 109 (1929).
8. Davis and Elderfield, J. Am. Chem. Soc. 50, 1786 (1928); E. I. du Pont de Nemours and Co., U. S. pat. 2,017,051 [C. A. 29, 8001 (1935)].
9. Hofmann, Ber. 15, 765 (1882); François, Compt. rend. 147, 430, 680, 983 (1908).
10. Bader and Nightingale, U. S. pat. 1,489,380 [C. A. 18, 1836 (1924)].
11. Chablay, Compt. rend. 156, 328 (1913).
12. Geisse, Ann. 109, 282 (1859); Wallach and Boehringer, Ann. 184, 51 (1877); Frankland, Challenger, and Nicholls, J. Chem. Soc. 115, 159 (1919).
13. Mendius, Ann. 121, 139 (1862); Debus, Ann. 128, 201 (1863); Denham, Z. physik. Chem. 72, 674 (1910); Riedel, Ger. pat. 264,528 [Frdl. 11, 110 (1912–14)]; Dreyfus, U. S. pat. 2,072,247 [C. A. 31, 2619 (1937)].
14. Meister, Lucius, and Brüning, Ger. pat. 73,812 [Frdl. 3, 15 (1890–4)]; Trillat and Fayollat, Bull. soc. chim. (3) 11, 23 (1894); Kundsen, Ger. pat. 143,197 [Frdl. 7, 24 (1902–4)]; Meister, Lucius, and Brüning, Ger. pat. 148,054 [Frdl. 7, 26 (1902–4)]; Isono, J. Pharm. Soc. Japan No. 397, 209 (1915) [C. A. 9, 2232 (1915)].
15. Pierron, Bull. soc. chim. (3) 21, 783 (1899); Mailhe and Murat, ibid. (4) 7, 954 (1910); Zerewitinov and Ostromisslensky, Ber. 44, 2403 (1911).
16. Gaudion, Bull. soc. chim. (4) 7, 824 (1910); Ann. chim. phys. (8) 25, 136 (1912).
17. Takaki and Ueda, J. Pharm. Soc. Japan 58, 276 (1938) [C. A. 32, 5376 (1938)].
18. Naegeli, Grüntuch and Lendorff, Helv. Chim. Acta 12, 227 (1929).
19. Brochet and Cambier, Bull. soc. chim. (3) 13, 534 (1895); François, Compt. rend. 147, 429 (1908); Werner, J. Chem. Soc. 111, 848 (1917); Jones and Wheatley, J. Am. Chem. Soc. 40, 1411 (1918); Wietzel and Köhler, Ger. pat. 468,895 [C. A. 23, 846 (1929)]. "

However, in defense of your opinion, I suspect an important detail (like a strong base acting as a catalyst,..) is missing from the discussion, but perhaps mentioned in the cited reference [5].

[Edited on 24-10-2012 by AJKOER]

franklyn - 24-10-2012 at 15:37

@ AJKOER

My initial warning is based on elementary first principles.
Now I'm not so sure , in fact I've solicited a review.

http://www.sciencemadness.org/talk/viewthread.php?tid=18006#...

.

PHILOU Zrealone - 25-10-2012 at 02:13

Quote: Originally posted by franklyn

@ AJKOER

My initial warning is based on elementary first principles.
Now I'm not so sure , in fact I've solicited a review.

http://www.sciencemadness.org/talk/viewthread.php?tid=18006#...

.

Reply posted in the tread:

Le Chatelier's rule/principle for reactions in equilibrium...
A reaction system in equilibrium placed in a closed reactor with stable parameters (P,V,T) tends to a stable proportion of reactants (concentration)... A static equilibrium.

But if the system is open... V tends to be infinite and if a compound is volatile (gaseous) the reaction /equilibrium will be shifted to that side of the reaction and go to near completeness. The same kind of theory applies to precipitation reaction where the precipitate goes to a concentration of "zero" and is considered as dropped out of the system.

Here N2H4 is much less volatile than NH3...
So in an open system despite NH3 is more basic...N2H4 will remain because NH3 will escape faster and continuously from the reactor.
In a closed reactor:
N2H4(l) + NH4Cl(s) <==--> N2H5Cl(s) + NH3(g)
In an open reactor:
N2H4(l) + NH4Cl(s) <--====> N2H5Cl(s) + NH3(g)

In the case of NH3 and CH3-NH2... CH3-NH2 is more basic than NH3 but both are very volatile... so the question is more delicate.
In a closed reactor:
NH3(g) + CH3-NH3Cl(s) <==--> NH4Cl(s) + CH3-NH2(g)
In an open reactor:
NH3(g) + CH3-NH3Cl(s) <==?==> NH4Cl(s) + CH3-NH2(g)

AJKOER - 25-10-2012 at 16:36

Per this questionable source (http://www.hoboes.com/pub/Prohibition/Drug%20Information/Mis... ), "Methyl Chloride + Ammonia in an ether solution (CH3NH2 + NH4Cl)"

However, the use of a different medium was, in fact, suggested by the review thread as a plausible explanation ( http://www.sciencemadness.org/talk/viewthread.php?tid=744&am... ). Extract:

Quote: Originally posted by Nicodem

Quote: Originally posted by franklyn

My query relates to another post in which I assert that Ammonia is a weaker
base than Methylamine so it cannot displace it to form NH4Cl with HCl.
According to this _

CH3NH2 •HCl + NH3 => CH3NH2 + NH4Cl

Which appears analogous to the displacement of the weaker base Hydrazine
N2H4 •HCl + NH3 => N2H4 + NH4Cl

Those are just equations which essentially just define the reactants and the products, but say nothing about the synthesis. Several times I already tried to explain that bare chemical equations like those do not describe the chemical system. The problem is that it is the whole system (solvent, temperature, reagent ratios, rate and order of addition, catalyst, stirring...) that defines the reaction results. For example, if you add methylamine hydrochloride to aqueous ammonia, no product will form. But if you add methylamine hydrochloride to ethanolic ammonia, I believe it is quite likely that you will obtain a precipitate of NH4Cl. All the parameters are the same, only the solvent changes and the change can be as dramatic as that.

Also, you say ammonia is a weaker base than methylamine. That is true for aqueous solutions where ammonia is about 10-times weaker base, but this is not necessarily true for other solvents. Compare the pKa values of NH₄⁺ and RNH₃⁺ ions in DMSO and you will see how things can change. Besides the proton transfer reactions are just one of the many possible driving forces for a product to form - they are not necessarily the determinative force.

Now, I would humbly add to Nicodem's comment "The problem is that it is the whole system (solvent, temperature, reagent ratios, rate and order of addition, catalyst, stirring...) ", citing a recent example involving the decomposition of Chloric acid. Frequently unreactive chloride ions are present in commercial chlorine products (for example, Chlorine Bleach, active ingredient NaOCl, also contains NaCl) and, in the case of the discussion of HClO3, its decomposition proceeds differently in the presence of chloride ions. In effect, the once spectator chloride ions are promoted to a full reactant. Also, a previously inert energy source (for example, light) may initiate a reaction. The unexpected reaction is probably a significant factor for many garage chemists starting with impure ingredients, and I would add it to Nicodem's list. More damaging result occurs for those experimenting with energetic materials which, at times, can be made unexpectedly more hypersensitive in the presence of certain metallic impurities. On a larger scale, I have (in a prior thread) noted an event involving the loss of an entire cargo vessel. The suspected cause relates to a Mg impurity in a Calcium ore, which could have added a touch of Magnesium hypochlorite (perhaps chlorate also), to a shipment of Ca(ClO)2 made from that ore.

I would also give an illustration of how the reactant ratios can change the reaction products. In the case of the action of Oxalic acid on say NaClO3, for example, initially the H2C2O4 liberates HClO3 from the chlorate salt, but in excess, the Oxalic acid decomposes the newly formed HClO3 into ClO2.

[Edited on 26-10-2012 by AJKOER]

killswitch - 27-10-2012 at 15:56

Quote: Originally posted by PHILOU Zrealone

Quote: Originally posted by Kalium

Quote: Originally posted by killswitch

In addition, MeNO₃ is the only nitric ester in the polyol series (EGDN, NG, ETN, XPN, MHN) with a negative oxygen balance.

Perhaps with the exception of PETN.

I was talking about alcohols with a number of hydroxyl groups equal to the number of carbon atoms. Technically, yes, those are polyols, but hardly anyone uses their nitrates as energetic materials. And yes, methanol is not a polyol, just as 1 is not a prime number.

PHILOU Zrealone - 28-10-2012 at 03:50

Quote: Originally posted by killswitch

Quote: Originally posted by PHILOU Zrealone

Quote: Originally posted by Kalium

Quote: Originally posted by killswitch

In addition, MeNO₃ is the only nitric ester in the polyol series (EGDN, NG, ETN, XPN, MHN) with a negative oxygen balance.

Perhaps with the exception of PETN.

I know Killswitch

the familly H-(CHONO2)n-H (with n from 1 to infinite).
From my study of famillies of HE and explosives substances, I can tell that negative OB is not a real problem to get very usefull explosives.
PETN or polyvinyl nitrate are good examples.

Dr.Q - 24-11-2012 at 13:08

i tried to make Metyl nitrate with 10 ml %50 HNO3 and 10ml %99 H2SO4 solution.
After mixing the acids i cooled down it in a ice bath than ad slowly drops of CH3OH. After a few mins a thin layer is showed up just as i waited. I collect it and test it
I burned it with a lighter. there was a white-gray colored flame but it was not fast . It burned slowly . That means ıt is not pure.
I tried different way like changing the amount of acids but result was same.
What is the problem in my way ?!

Farnsworth - 29-11-2012 at 20:52

Question for the familiar:

Has there ever been an application of methyl nitrate dynamite? When I think "volatile liquid explosive" the next thought that always comes to mind is keiselguhr. Or perhaps something like starch / guar gum?

Just seems this stuff could be a fun toy if you could deal with it in a less sensitive, nonliquid state.

methylator - 10-12-2012 at 05:13

Hello all. I have been trying to make methyl nitrate using 40ml sulfuric acid(Rooto drain opener) 26g ammonium nitrate (instant cold packs from Rite-Aid) and 11ml methanol(Heet). I cool the acid, mix in the NH4NO3, and put it in a salt water bath. I then add the methanol drop by drop. The trouble is that when I am done, no layer forms on top. I can smell the methyl nitrate(smells really good BTW), but when I crash it into water it still doesn't separate . I am totally bumfuzzled.

methylator - 16-12-2012 at 10:53

So yesterday I decided to test the purity of my methanol. I burned about 30ml of it. After it went out there was still about 15ml of liquid left that would not burn! I checked the Heet msds but all it lists is 99% methanol and 1% "proprietary ingredient". Any idea as to what I have? I bought it at Wal- mart. Is there a possibility that it is diluted?

SherlockHolmes - 14-3-2013 at 10:24

Today I tested 100ml methyl nitrate. I did not expect that the damage would be so small. Iron on which the tested methyl nitrate was placed on the mud and buried in the ground in the explosion.

[Edited on 15-3-2013 by SherlockHolmes]

hissingnoise - 14-3-2013 at 11:04

Like the syringe detonator ─ adds a whole new dimension to the phrase "shooting-up" . . .
Which primary, BTW?

SherlockHolmes - 14-3-2013 at 11:26

Detonator is 0.20 grams of lead azide and 1.5g pyroxylin pressed into the syringe. My idiot friend accidentally deleted a video explosion. I'll do a video pictures with detailed descriptions of the test and show video.

SherlockHolmes - 14-3-2013 at 12:26

Here is the video: http://www.youtube.com/watch?v=ZT_PCuGMR68

Ral123 - 14-3-2013 at 12:27

Douh, you're still not as failo like that brisanse54 guy. You've reached the capabilities of MN. The hole, that thing dug is impressive

MN today, HN tomorrow, that target wont survive.

SherlockHolmes - 14-3-2013 at 12:54

Detonate as hard as he can. Brisantse54 failed to detonate any high explosive with high detonation velocity. With 300 grams ETN / NG only 2 mm sheet metal bent. His explosives detonates with no more than 2500 m / s Methyl nitrate density 1.15. and do much damage.

Ral123 - 14-3-2013 at 13:50

Some people should get into propellants or something

SherlockHolmes - 15-3-2013 at 02:06

A colleague pointed out to me a big mistake. Detonator has directed most of the energy away than the iron plate. You can see how the blast wave struck the ground side.

VladimirLem - 15-3-2013 at 07:46

Quote:

Quote: Originally posted by SherlockHolmes

I did not expect that the damage would be so small.

wtf?

u're getting stroppy cause the steel-target havent got more damage?

how about putting the ignitor ONTOP of the charge (like a shaped charge) to force the detonation to move towards the steelplate and not to the side of the charge?

[Edited on 15-3-2013 by VladimirLem]

SherlockHolmes - 15-3-2013 at 09:04

Exactly detonator had to do but I knew until after the test :mad:

Ral123 - 1-5-2013 at 07:06

I had s cup of water/ammonia with MN on the bottom for storage. It appears the MN dissolves in the water and evaporates from the top, even trough the layer is on the bottom. After a week there's no MN in the cup, only water. Is it possible that some other process has taken place?

WGTR - 17-4-2014 at 08:47

This looks like the generic methyl/ethyl nitrate thread, so I think this is the right place to post this.

I have an issue that might seem unusual. I'm trying to not make ethyl nitrate. I'm actually interested in making glyoxal (to synthesize ionic liquids), and am trying to avoid performing any unintentional nitrations. This is basically a sanity check of sorts, to make sure that I'm not doing something stupid. I have little experience reacting nitric acid with organics, so I'm approaching this with caution.

Debus originally made glyoxal by oxidizing ethyl alcohol slowly with nitric acid at "ordinary temperatures".

Philosophical Transactions of the Royal Society of London, Volume 148

Generally they would do this by carefully pouring the alcohol on top of the acid, so that two layers would form without mixing. The reaction would gradually occur by diffusion of the two layers.

My old friend Debus was a very smart guy, but he lived during a time when people pipetted chemicals with their mouths, and tasted unknown substances to identify them. I hope he will forgive me for not trusting his procedures 100%.

A newer patent is a bit more descriptive, but starts directly from acetaldehyde:

Attachment: US3429929.pdf (224kB)
This file has been downloaded 702 times

I intend to use the methods from the patent, but rather start from ethyl alcohol instead, to attempt performing a one-pot reaction.

Basically, the plan is to react 0.5% copper(II) oxide (catalyst) with 50% nitric acid solution. A small amount of sodium nitrite (initiates reaction) will be added to absolute alcohol, and then the nitric acid will be slowly added under stirring to the alcohol (maybe over 1-2 hours). The temperature will be maintained at 40°C with a water/ice bath. Naturally, this will have to be done on reflux to keep the acetaldehyde from escaping.

Note that I'm forming nitrous acid in situ, that there is water in the reaction (50% nitric acid), and that the acid is being added slowly to keep the temperature at 40°C.

Am I properly avoiding the conditions that would perform a nitration?

ManyInterests - 23-7-2024 at 01:43

Since I want to make some methyl nitrate to experiment with mixing it with nitrostarch to see if it does form a kind of plastic explosive with that, I just do have some questions to ask mostly about some safe storage and disposal since it could be a few weeks before I use it. Someone mentioned that putting it in a fridge or even freezer in a sealed container can be a good way of preserving it. Is this correct?

As for how I intend to make it. I will be making it in a simple nitration mixture. The proportions will be taken from the improvised munitions handbook (80ml of methanol, 145ml of 95% sulfuric acid, and 95ml of azeotropic nitric acid) and I will be washing it with a saline solution and drying with calcium chloride.

Microtek - 23-7-2024 at 08:23

I agree that well neutralized, washed and dried methyl nitrate could probably be stored for a long time in a sealed container made of a suitable material. Putting it in the freezer could also be a good idea since one of the big issues with methyl nitrate is its volatility.

ManyInterests - 23-7-2024 at 09:38

This webpage documents the cleaning process I will follow, but not the synthesis. It involves a lot of washing, which is something I am comfortable with. Especially with ice cold water since methyl nitrate is not very soluble in very cold water and it loves being cold.

For the synthesis, I will cool down the nirating mixture on its own in the freezer for at least 12 hours and I will also have a large glass bowl of ice water to float it in while I add the mixture. That way if anything seems wrong I can immediately overturn the beaker into th water and prevent an accident.

dettoo456 - 24-7-2024 at 08:09

If you’re planning to store the MeONO2 too, aside from it being in a freezer, make sure to vent it at least 1X a week and make sure to limit its exposure to UV as much as possible.

Try to invest in a full face shield (or full face respirator) and a Kevlar scarf too; glass shrapnel is no joke

ManyInterests - 24-7-2024 at 14:28

Quote: Originally posted by dettoo456

If you’re planning to store the MeONO2 too, aside from it being in a freezer, make sure to vent it at least 1X a week and make sure to limit its exposure to UV as much as possible.

Try to invest in a full face shield (or full face respirator) and a Kevlar scarf too; glass shrapnel is no joke

I have both. I have kelvar sleeves I can use to make a scarf.

I won't store it for long. Like maybe I will keep it for 10 days or so at the most. I might not put it in a glass container, but rather a plastic one I might wrap it plastic wrap.

If you look at the proportions I will be using, the end product might be over 100 grams Not sure if anything can protect me if it goes off... just how sensitive IS methyl nitrate? I saw videos where people smacked it really hard with heavy hammers (on makeshift steel anvils, too) and it did not detonate.

When I make it into a charge, I'll be using a cardboard tube with an epoxy plug on one end, I am thinking of closing the other end after I insert the detonator (a 1g melt-cast ETN charge with 0.3g of ETN:NHN mixture in a .223 Remington case... an overkill I know) This will make venting impossible, and when the epoxy hardens, it generates a lot of heat. I will be doing this the night before I go to see how much of a bang it makes.

Sir_Gawain - 24-7-2024 at 19:42

Why don't you make it into dynamite? It seems like it would be much easier and safer to handle that way. Add methyl nitrate to a mixture of ammonium nitrate and flour or fine sawdust until it is saturated, but not dripping.

ManyInterests - 24-7-2024 at 19:57

Quote: Originally posted by Sir_Gawain

Why don't you make it into dynamite? It seems like it would be much easier and safer to handle that way. Add methyl nitrate to a mixture of ammonium nitrate and flour or fine sawdust until it is saturated, but not dripping.

That is exactly what I intend to do! I mentioned before that I intend to make it into a plastic explosive by mixing it with nitrostarch. The ratio is 10:1 of methyl nitrate to nitrostarch.

Sir_Gawain - 24-7-2024 at 21:22

Quote: Originally posted by ManyInterests

That is exactly what I intend to do! I mentioned before that I intend to make it into a plastic explosive by mixing it with nitrostarch. The ratio is 10:1 of methyl nitrate to nitrostarch.

Like blasting gelatin, great! A gel or plastic is much better than liquid.

Microtek - 25-7-2024 at 09:11

We've talked about excessively cold nitrations before. A mixed acid that is too cold can lead to runaway more easily than one that is the proper temperature. I suggest you make a salt-ice bath and use that to cool the nitration mix to about 0 C, and then maintain the temp at 0-5 C by adjusting the speed of addition of the methanol. That way, the reaction has a chance to approach equilibrium before too much substrate (methanol) is in the mix.

ManyInterests - 25-7-2024 at 16:51

Quote: Originally posted by Microtek

We've talked about excessively cold nitrations before. A mixed acid that is too cold can lead to runaway more easily than one that is the proper temperature. I suggest you make a salt-ice bath and use that to cool the nitration mix to about 0 C, and then maintain the temp at 0-5 C by adjusting the speed of addition of the methanol. That way, the reaction has a chance to approach equilibrium before too much substrate (methanol) is in the mix.

Understood. I will cool the nitration mix in the fridge and not the freezer. That way it'll be closer to 0 C than -10C or so before the stuff is added. I will also add the methanol slower than what the improvised munitions handbook recommends (half teaspoon (2.5ml) per minute or so. I will add a little less than that amount every 3 or 4 minutes and monitor carefully.

I assume the same thing should be done with things like EGDN, DEGDN, and Nitroglycerine?

Quote: Originally posted by Sir_Gawain

Quote: Originally posted by ManyInterests

That is exactly what I intend to do! I mentioned before that I intend to make it into a plastic explosive by mixing it with nitrostarch. The ratio is 10:1 of methyl nitrate to nitrostarch.

Like blasting gelatin, great! A gel or plastic is much better than liquid.

Yep, I wonder why anyone thought I would be using plain methyl nitrate. I got the idea from Tim Lewis's kitchen improvised explosives. I did ask around and it seemed that the idea of nitrostarch mixing with a liquid explosive to form a putty is quite plausible, and it will be more stable than plain methyl nitrate. Albeit it must still be used ASAP.

Even the Improvised Munitions Handbook section on methyl nitrate has instructions to use it as a dynamite. They suggest using shredded cloth, paper, or sawdust as an absorbent material. I did not know that flour could work, too. I am also guessing that diatomaceous earth would work well with methyl nitrate.

ManyInterests - 28-7-2024 at 13:34

OK, so I am going to give my after synthesis report. Currently it is not 100% finished as I drying it with calcium chloride in the freezer as per the cleaning instructions. I made one mistake: I forgot to give it a 2nd salt-water wash after the sodium hydroxide deacification, I used simple ice-cold water, the water is very slightly acidic, but I am not sure if it is from the methyl nitrate... I didn't want to lose too much through washing. It is very, very slightly acidic so it probably doesn't matter. Or maybe I am wrong. I lost around 10g from the whole thing. But all in all I am quite happy with the yield. Also there is no discoloration whatsoever in my yield, which is also very pleasing to know.

The nitration itself was highly uneventful and completely boring. Neutralizing the leftover acid was SCARY, when I added simple water to it, it turned green and emitted a lot of NO2. I did not inhale any, thankfully, and neutralizing it with water and bicarbonate also had a lot of gasses come out, which I combated with my mighty spray bottle of bicarbonate solution.

The calcium chloride has thickened up quickly, I assume it has absorbed the water. I will need to treat it a 2nd time with calcium chloride according to the instructions to fully dry it. I used around 5 or 6 grams, I will use another 5 or 6 grams.

I will use my nitrostarch to make it into a plastic explosive immediately before putting it in the freezer.

[Edited on 28-7-2024 by ManyInterests]

ManyInterests - 28-7-2024 at 14:41

OK, so the guide giving the proportions of 1 gram nitrostarch to 10 grams of methyl nitrate was a lie. I needed a LOT more nitrostarch to get it to gel up, and it was not a play-dough like consistency but more like a very thick regular dough. I might have gotten a whiff of the nitrate as I was mixing since I felt mildly light headed, I did the process in the most well ventilated area in my apartment. I stopped counting how much nitrostarch I put in. but I am very glad I had enough for it. (and if I didn't, i guess regular cornstarch and flour would suffice?).

After mixing the stuff was so thick that I left the spoon in and I wrapped the tupperware in many layers of plastic film. I will keep it there until it is time to load it in its container. Then I will keep it in the freezer again until it is time to seal the other end with epoxy.

Microtek - 29-7-2024 at 08:39

When gelling a liquid nitrate ester such as methyl nitrate with nitrostarch or nitrocellulose, the colloidonization take time, especially at lower temperatures. Did you wait for it to gel before adding more? Also, what temp was this done at?

ManyInterests - 29-7-2024 at 13:02

Now I feel extremely dumb. Yes it was ice cold. I had just finished drying it with calcium chloride (I treated.it twice with the stuff) and once I was confident it was dry I started adding the nitrostarch. I hadn't done anything like this before and I wasn't sure what to expect.

It had been in the fridge and freezer while drying since the instructions were to keep it at 0C. I didn't wait too much between additions, so I must admit I added a lot...

I guess next time I should wait more. At any rate it is done and I am keeping it in the freezer until it is time to take it out for use in around 12 to 14 days.

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