| Pages:
1
2
3 |
AH-Poster
Harmless
Posts: 9
Registered: 16-10-2010
Member Is Offline
Mood: No Mood
|
|
1-Amino,2-Nitro Ethane
Quote: Originally posted by Rosco Bodine  |
NH4ClO4 + HCHO ---> CH2=NH(HClO4) + H2O
CH3NO2 + CH2=NH(HClO4) ----> CH2NO2CH2NH2(HClO4)
[Edited on 18-10-2010 by Rosco Bodine] |
This is potentially a good idea!
It should be noted that aldehydes actually disproportionate upon reaction with salts of ammonia. Also note that NH4ClO4 is one of the least soluble
ammonia salts.
To perform the reaction, formaldehyde could be slowly added over the period of 1h, in several small additions, to a 60% alcohol solution of ammonium
perchlorate and nitromethane.
There should be doubts about whether this could work, however. CH2O reacts with ammonia salts, the reaction can be written as:
(2)CH2O + NH4ClO4 ==> CH3NH2*HClO4 + HCO2H
Also note that methylene imine quickly loses ammonia and condenses into hexamine. Whether a solution of hexamine and ammonia could be used in an
addtion reaction with nitromethane is not known.
Whether CH3NO2 could react with the intermediate imine (not shown) before it gets reduced is doubtful. It is, however, more likely that such an
addition reaction could take place under alkaline conditions.
Nitromethane only reacts to form addition compounds through its "aci-form", and this tautomer only dominates under alkaline conditions. Formaldehyde
actually disproportionates into methyl formate ester under very strongly alkaline conditions (sodium methoxide). Michael reactions, of the type
between CH2O and CH3NO2, usually require a strong base to catalyze them.
Ammonium "nitromethanate" could possibly exist under normal pressure. Cold anhydrous NH3 would be bubbled into liquid nitromethane cooled to (minus)
-25degC.
The salt of hydrazine and nitromethane, which is a liquid mixture, is mentioned on wikipedia: "With nitromethane, hydrazine forms an explosive
salt..." The explanation is ellaborated upon in another forum: "nitromethane proton is "acidic" enough to be removed by a relatively weak base such as
hydrazine (indeed forming a salt) and thus can act as an acid." http://webcache.googleusercontent.com/search?q=cache:20uotFw...
The formation of the salt of ammonia and nitromethane will probably raise the boiling point of the ammonia, in the same way that NH3 can be handled as
a liquid in the form of concentrated NH4OH. This "salt"/ liquid mixture, may react with formaldehyde in a Michael reaction to form the desired
product, NH2CH2CH2NO2. The formaldehyde, in this case, should be solid trioxane dissolved in an excess of pure alcohol, and the resulting solution
very slowly added to the NH3-CH3NO2 mixture.
However, nitromethane is known to react with formalin (CH2O) under alkaline conditions to form Tris(hydroxymethyl)nitromethane (not sure if this
reaction requires heat). To summarize, CH2O and CH3NO2 may react to form an undesirable byproduct under basic conditions, while
CH2O and ammonia condense together into hexamine, or under acidic conditions, will form undesirable byproducts . It is unknown what product(s) would
form if CH2O was added to a mixture of ammonia and nitromethane. Not having any formalin, this reaction cannot be investigated by me.
If too much CH2O present, it likely will react with the imine before the imine has a chance to react with CH3NO2.
NH4+ and CH2O ==> CH2=NH2+
CH2=NO2- and CH2=NH2+ ==> O2NCH2CH2NH2
[Edited on 19-10-2010 by AH-Poster]
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Actually I have my own strong skepticism that it would work, however it does seem plausible so it continues to be intriguing. Yes nitromethane is
reactive towards formaldehyde ....however the formaldehyde is reactive also towards the ammonium and it would seem more favorably so in acidic medium.
So I thought
the formation of the methyleneimine might be preferential ...and that then the
nitromethane would couple directly with it. It was my thinking that solubility might drive this route for a reaction in aqueous methanol
particularly if the desired product had low solubility as its perchlorate salt....the product desired may simply drop out of solution as fast as it
was formed. Of course there are a whole lot of "ifs" there .....but sometimes such things do occur.
I was hoping that Nicodem may propose an alternative route as he mentioned using the Michael reaction. Paraformaldehyde is what I have on hand and
will doubtlessly convert some of it to methylamine perchlorate as I have no doubt that simpler well known reaction will work. I was simply intrigued
by the considered and described possibility that the same unsaturated methyleneimine intermediate in that known reaction might combine directly with
nitromethane leading to a possibly even more energetic derivative.
That last reaction equation which you show is not balanced.
For that last reaction you mean 3 CH2O rather than 2 CH2O
and the balanced reaction would actually be
3 CH2O + 2 NH4ClO4 ----> CH3NH2*HClO4 + H2O + HCO2H + CH2=NH*HClO4
If that does happen, then a methylamine perchlorate mixed product or double salt is possible if the methyleneimine does indeed conjugate with the
CH3NO2.
[Edited on 19-10-2010 by Rosco Bodine]
|
|
|
Nicodem
Super Moderator
Posts: 4230
Registered: 28-12-2004
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by Rosco Bodine |
You just lost me there ...where is the final CH3 coming from ?
As for the other .... ( amending the bond symbol for methyleneimime ) |
Never mind that. With all those methyls and methylenes I mistakenly believed you are presenting a new reaction using methylamine.
| Quote: | | Possibly the shorter chain would not cyclize and the reaction would proceed if the formaldehyde was added gradually or there was simultaneous addition
so formaldehyde was not present in excess ? |
No, the disubstitution Mannich reaction on nitromethane is the consequence of the inherent property of nitroalkanes which tautomerize more easily when
they are RCH2CH2NO2 or R2CHNO2 compared to nitromethane (for example, compare the pKa of nitromethane and nitroethane to see the difference). So, once
the monosubstituted Mannich product forms, it will be a much better substrate for another Mannich reaction compared to nitromethane itself. The
initial product of monusubstitution is an amine and can efficiently participate as bifunctional substrate for the Mannich, thus leading toward
cyclization or oligomerization. Essentially, you can forget about forming 2-nitroethylamine this way. If you check the references above, you can see
that enough effort was already put into this and it does not work. The only route that actually worked was alkylating ammonia with nitroethene via
Michael reaction.
| Quote: Originally posted by AH-Poster | To perform the reaction, formaldehyde could be slowly added over the period of 1h, in several small additions, to a 60% alcohol solution of ammonium
perchlorate and nitromethane.
There should be doubts about whether this could work, however. CH2O reacts with ammonia salts, the reaction can be written as:
(2)CH2O + NH4ClO4 ==> CH3NH2*HClO4 + HCO2H
... ... |
Instead of diving in idle speculation and off road wilderness, why don't you put some effort and actually read the preceding posts and the references
provided? You were already explicitly told to change your ways several times. Don't you think it is about time you change? Why do you insist in
ignoring theory and literature? Such attitude can cost a chemist his life and this forum does not promote carelessness or ignorance.
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Thanks Nicodem,
Yeah, if the reaction continues for the ( first ) Mannich base, as is likely, rather than it dropping out of solution as a salt ....then the hoped
reaction fails and a more complex product results. Oh well, it wasn't a totally dumb idea and it was fun while it lasted 
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
aminoacetonitrile perchlorate ....exist?
Further contemplation has been done about a possible similar compound which may have potential usefulness as an energetic perchorate, and with regards
to this hypothetical
compound, I also welcome any thoughts from you all.
The organic perchlorate being contemplated is "glycine nitrile" perchlorate, or aminoacetonitrile perchlorate
NH2CH2CN-HClO4
proposed synthetic route
NH2CH2CN-HCl + NaClO4 ----> NaCl + NH2CH2CN-HClO4
Perhaps for the hydrochloride precursor is possible to use a method using TCCA and glycine, reacted in aqueous medium for a half hour at 5C and basic
conditions as per description on page 3 of attached paper, reaction following the example
details on page 5 as for the conversion of phenylalanine to phenylacetonitrile: The synthesis could be simplified as there would be no need for
isolation of the aminoacetonitrile hydrochloride.
General One-Pot Procedure for the Preparation of
Nitriles from a-Aminoacids. The reported procedure is
representative: L-Phenylalanine (1.20 g, 7.6 mmol) was
dissolved in an aq solution of 2 N NaOH (3.8 mL) and
treated with TCCA (1.17 g, 5.1 mmol) at 25 °C. After 10
min, when TLC analysis showed the complete absence of the
L-phenylalanine, the reaction mixture was treated with HCl
(15 mL), followed by an aq solution of 3 N HCl (2.5 mL).
After 10 min the mixture was extracted twice with Et2O (15
mL). The organic layers were washed with H2O (10 mL),
dried on Na2SO4, filtered and concentrated in vacuo to yield
2-phenylacetonitrile (20, 0.87 g, 98%). 1H NMR: d = 7.38
(m, 5 H), 3.75 (s, 2 H). 13C NMR: d = 142.1, 129.1, 127.9,
127.8, 117.8, 23.5.
A bit of scientific trivia perhaps is that aminoacetonitrile is a material detected in the far reaches of interstellar space ...... (see link)
........
http://medgadget.com/archives/2008/04/scientists_spot_amino_...
http://www.youtube.com/watch?v=3hEfcawx6Fc&feature=relat...
http://www.youtube.com/watch?v=DNjzzDNIJWw&fmt=18
Attachment: An Insight of the Reactions of Amines with Trichloroisocyanuric Acid.pdf (160kB)
This file has been downloaded 1428 times
[Edited on 26-11-2010 by Rosco Bodine]
|
|
|
nitro-genes
International Hazard
Posts: 1048
Registered: 5-4-2005
Member Is Offline
|
|
Sort of OT:
What would happen if NH3 was used under the same conditions? Presumably it would form nitrogen nitrille. (a fancy word for nitrogen gas) I was
wondering what makes the formation of Cl-NH2 more favorable in the the hydrazine synthesis, while Cl2-NH (Cl3-N?) is apparently the result of the
direct reaction of TCCA.
[Edited on 26-11-2010 by nitro-genes]
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Ummm ....
I think for a nitrile there must be a C having a triple bond to N as a CN .....
nitrile being synonymous with cyanide .....right ?
therefore, your nitrogen nitrile would be NCN ??
( because if it was CNN .... then it would be a TV station )
And yes I am a blonde  , or I used to be long ago before I became a silver
Ummm....anyway there is a unusual amount of energy contained (and releasable) from a CN group ....so it seemed like as a fuel component of an
energetic organic perchlorate that it may provide excellent performance.
[Edited on 26-11-2010 by Rosco Bodine]
|
|
|
nitro-genes
International Hazard
Posts: 1048
Registered: 5-4-2005
Member Is Offline
|
|
( because if it was CNN .... then it would be a TV station )
Haha, you may have lost your blonde manes, but clearly not your humor!
It's been a while since I've done anything even remotely chemistry related. I increasingly tend to write brain-fart-inspired posts and then think
about it later, srry about that...
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
No problem, I have my moments too when things get kind of foggy. I drink way too much coffee just to try to keep from sleeping excessively....I'm
like an old lion who wakes up when hungry, eats too much and then goes back to sleep till hungry again.
http://www.youtube.com/watch?v=THWgH85TyJQ Bungle In The Jungle
Anyway .....
what about the speculative and hypothetical cyanoglycine perchlorate ?
Seems worth an experiment and simple enough. It would be great if it is stable and non-hygroscopic.
The stuff could even be a primary and the energy potential there is probably somewhere around that of tetryl or better.
[Edited on 26-11-2010 by Rosco Bodine]
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
It looks like the actual precursor required for oxidation to aminoacetonitrile would be aminoglycine since the amino is the source of nitrogen for the
formation of the nitrile. Glycine would be oxidized to acetonitrile. I have been looking at this for a few days and that is my conclusion.
Aminoglycine is mentioned as a component of hair treatments.
It may be interesting also to see what would be the oxidation product of hydantoic acid (ureidoacetic acid) NH2CONHCH2COOH .
[Edited on 2-12-2010 by Rosco Bodine]
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Diammonium Hydrazinium Tetraperchlorate
Diammonium Hydrazinium Tetraperchlorate US4053566
This is interesting because of the numerous possible different synthetic routes and the likelihood it is energetic,
along with an absence of literature references to the material. It suggests that other complex double salt perchlorates involving substituted
ammonias and/or substituted hydrazines are also possible. For example perhaps a methylamine perchlorate with semicarbazide perchlorate would form an
analogous double salt.
Good luck trying to find any further information. It appears this may be obscure or in the realm of purely experimental.
According to a Dow Chemical research report this is not an actual compound, but is a physical mixture which has been misidentified.
http://oai.dtic.mil/oai/oai?verb=getRecord&metadataPrefi...
An additional patent US3743701 (attached) subsequent to the Dow Chemical report evidently disputes the Dow finding.
Attachment: US4053566 Diammonium Hydrazinium (tetra)Perchlorate.pdf (151kB)
This file has been downloaded 968 times
Attachment: US3743701_DIAMMONIUM_HYDRAZINIUM_TETRAPERC.pdf (378kB)
This file has been downloaded 1114 times
Thiokol is the patent holder for what indeed does appear to be an actual compound.
[Edited on 9-2-2011 by Rosco Bodine]
|
|
|
DougTheMapper
Hazard to Others
Posts: 145
Registered: 20-7-2008
Location: Michigan, USA
Member Is Offline
Mood: Energetic
|
|
This is some really neat stuff. The diammonium hydrazinium tetraperchlorate isn't all that far out of reach for those with perchlorate salts, esp.
pertaining to the first patent.
If the compound is able to sustain detonation it might find use when plasticized since the relatively large amount of binder needed for plasticization
could bring the overly-positive oxygen balance into check. Of course, this would then serve to reduce sensitivity (which is probably pretty low anyway
since the patent talks about using it as a propellant) as well as increase power but probably reduce brisance.
Decomp seems to be (NH4)2(N2H6)(ClO4)4 --> 2N2 + 6H2O + 2HCl + 5O2 with a whopping oxygen balance of +40.3 wt%!
For that matter, this compound could probably be used to make oxygen candles once the HCl has been scrubbed.
Victor Grignard is a methylated spirit.
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
DAHTP could be useful as an energetic oxidizing perchlorate explosive component, especially if compatable with another energetic oxygen deficient
perchlorate based explosive fuel in a mixture achieving oxygen balance. It would be a bonus if such a mixture was a nonhygroscopic eutectic....such a
composition could be very stable, and dense and powerful. It is good to have valid alternative compositions to the more usual nitration products used
as energetic materials.
Of course DAHTP could be an interesting component also with the usual fuels
which might be used with other energetic oxidizers, fuels like nitronaphthalene, dinitrotoluene, ect. It would be my expectation that such mixtures
would be
cap sensitive and would be brisant and powerful, although more expensive than more usual nitrate oxidizer based analogues.
|
|
|
DougTheMapper
Hazard to Others
Posts: 145
Registered: 20-7-2008
Location: Michigan, USA
Member Is Offline
Mood: Energetic
|
|
If the perchlorate double salt forms in perchloric acid, why not the picrate salt in picric acid? Instead of ammonium perchlorate and perchloric acid,
ammonium picrate in picric acid with a halide hydrazine salt. Or is picric too weak of an acid? I don't know much about this sort of chemistry but the
TNP anions might be too bulky to "stick." Starting with chlorides might be a bad idea since the reaction might favor chloropicrin... bromopicrin
wouldn't be unnecessarily hazardous though.
Diammonium hydrazinium tetrapicrate? That would be quite a compound.
(NH3)2(N2H6)(C6H3N3O7)4 --> 8N2 + 10CO2 + 24CO2 + H2O + 11H2
And with a terrible lack of oxidants, possibly the answer to what to mix with the DAHTP. I wonder if there's a reliable way to estimate the density of
such a compound?
By the way, do you think this would favor the water and tend to produce more elemental C to keep the oxygen deficit? Like TNT, I think because of the
similar structure and already existent C=C bonds. Hm.
Possibly impossible to manufacture but maybe split it 50/50 and do Diammonium hydrazinium dipicrate diperchlorate... what a mess. Heck, mixing
perchloric acid with picric acid sounds like a positively terrible idea.
Theoretically:
(NH3)2(N2H6)(C6H3N3O7)2(ClO4)2 --> 5N2 + 8H2O + 7CO2 + 5C + 2HCl
Or diammonium hydrazinium picrate triperchlorate. I guess anything could exist on paper.
I think the general theme here is that much like a mixture of explosive compounds is usually better than a mix of an explosive and a fuel (NC gelled
NG vs. ANFO for instance), molecules made of two explosive ions are usually better than an explosive ion with a metal or something. (Like pentazenium
azide vs. NaN3) The main problem is finding the salts which are stable enough to exist for any useful length of time.
[Edited on 10-2-2011 by DougTheMapper]
Victor Grignard is a methylated spirit.
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
The OB mixture of DAHTP with Triaminoguandine Perchlorate would be something that comes to mind as a possible candidate mixture. Betaine Perchlorate,
Choline Perchlorate, Trimethylamine Perchlorate, and Tetramethylammonium Perchlorate
in OB mix with DAHTP or some complex mixture in specific proportions of these compounds could result in one or more eutectics having desirable
properties.
In my last post above immediately before the subject of DAHTP, there is my speculation concerning a nitrile derivative gotten by oxidation of
hydantoic acid, also having a perchlorate of potential interest. In an earlier thread regarding glycine nitrate,
http://www.sciencemadness.org/talk/viewthread.php?tid=2642&a...
hydantoic acid was mentioned by Axt in a related interest as an intermediate. And a simple synthesis of the hydantoic acid was described, taken from
GB991644. See example 1 of the patent attached. It is also possible that hydantoic acid itself may form an energetic perchlorate, properties also
unknown.
Attachment: GB991644 Hydantoic Acid and derivatives.pdf (146kB)
This file has been downloaded 1489 times
[Edited on 10-2-2011 by Rosco Bodine]
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Here's an interesting find and perhaps a useful method for simultaneously getting the water out and putting the fuel into molecular explosive
compositions where otherwise a hydrated oxidizing salt could be problematic. Basically it appears that the water of crystallization can be azeotroped
from DMSO solution of the hydrated oxidizer salt and then DMSO of crystallization substitutes for the previous water of crystallization, this
substitution resulting in an energetic material instead of what was before a benign hydrated oxidizer salt.
US3463684 DMSO substituted Hydrate Oxidizer Salt Molecular Explosives
Attachment: US3463684_Explosive DMSO substituted Hydrates of Perchlorates and Nitrates.pdf (156kB)
This file has been downloaded 1261 times
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
That may not be necessary. Organic amine perchlorates tend not to be hygroscopic, and indeed they have much lower solubilities than the corresponding
nitrates.
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
I was thinking more in terms of producing an energetic fuel component for another possible chemically compatible candidate mixture with DAHTP, which
could achieve OB for the mixture. Such a DMSO adduct could also possibly be used with other oxidizers in mixture to achieve OB.
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Ethylenediamine Perchlorate Picrate
Here's something interesting I found. US2406573 describes that a complex salt can be formed by half neutralization of ethylenediamine to form the
monoperchlorate can be followed by another half neutralization with picric acid
resulting in a perchlorate-picrate ethylenediamine salt which has explosive properties. Other similar combination salts may also be possible.
Attachment: US2406573 Ethylenediamine Perchlorate Picrate.pdf (123kB)
This file has been downloaded 1019 times
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Among the similar possible combination salts which might be worth investigation
is a possible Ethylenediamine Hydrazine Tetraperchlorate similar to the DAHTP described in the other patents posted earlier. Ethylenediamine and
hydrazine both should displace ammonia from ammonium perchlorate, the ammonia being volatile. Therefore it might be possible to form the speculated
Ethylenediamine Hydrazine Tetraperchlorate easily if indeed it does exist as speculated. It would seem possible the result could also be a
triperchlorate or other multiple salt as opposed to a tetraperchlorate.
[Edited on 15-2-2012 by Rosco Bodine]
|
|
|
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
Posts: 1986
Registered: 2-3-2011
Member Is Offline
Mood: No Mood
|
|
Both hydrazinium di-nitrate and di-perchlorate hydrolyse in water. So it would not be possible to obtain the di-perchlorate by reacting hydrazinium
perchlorate with an aqueous solution of perchloric acid.
More information about hydrazinium di-perchlorate:
| Quote: |
Not only is the monoperchlorate much less energetic as an oxidizer than the hydrazinium diperchlorate, but it is much more sensitive to detonation by
shock than the diperchlorate.
Preparation of hydrazinium diperchlorate using sodium perchlorate and hydrazinium dichloride In a reaction vessel equipped with stirring means, a
cooling device and inlets for supplying nitrogen and liquid hydrogen fluoride, the following reactants are added; a pulverized and intimately admixed
mixture of 2.45 parts by weight of anhydrous sodium perchlorate and 1.05 parts by weight of hydrazinium. dichloride. The mixture is chilled to -80'
C., purged with a nitrogen atmosphere, evacuated and 9.88 parts by weight of anhydrous liquid hydrogen fluoride is added to the reaction mixture. The
system is brought back to atmospheric pressure by reintroducing nitrogen to the system and the reaction is initiated by allowing the reaction mixture
to warm to room temperature. The solvolysis of the hydrazinium dichloride to the fluoride salt is evidenced by the evolution of bubbles of hydrogen
chloride gas. The hydrogen fluoride suspension is stirred vigorously for 5 hours and allowed to settle. The insoluble fraction is hydrazinium.
diperchlorate and the soluble fraction is principally sodium fluoride, which has a solubility in hydrogen fluoride.
Preparation of hydrazinium diperchlorate using potassium perchlorate and hydrazinium dibromide as reactants. In this example the same
equipment and procedure is followed as described in before, except that 2.77 parts by weight of anhydrous potassium perchlorate, 1.94 parts by weight
of hydrazinium dibromide and 10.65 parts by weight of anhydrous liquid hydrogen fluoride are used as reactants.
US 317459210 (1973)
|
|
|
|
Rosco Bodine
Banned
Posts: 6370
Registered: 29-9-2004
Member Is Offline
Mood: analytical
|
|
Agreed, from an aqueous system and ammonia displacement reaction from ammonium perchlorate, a triperchlorate product consisting of Ethylenediamine
Diperchorate + Hydrazine Monoperchlorate is about all that would be likely.
And it is unknown if such a triple perchlorate exists or what would be its properties......other than it would likely be highly energetic.
|
|
|
woelen
Super Administrator
Posts: 8012
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
| Quote: Originally posted by mnick12 | | [...]woelen, interesting expiriments! Have you tried methylamine perchlorate? I was going to attempt this once I get some more conc HCl to make
perchloric acid, but money is kinda tight right now. I have a feeling methylamine perchlorate would be pretty soluable, but also could be a good
energetic oxidizer when mixed with other fuels. |
I just received my order of methylamine (40% in water) and I
remembered this thread, so I looked it up again. I have done the experiment with methylamine. Making methylammonium perchlorate is remarkably easy.
I took 2 ml of 40% methylamine in water and added appr. 3 ml of water. The resulting liquid is around 15% of methylamine and has a fairly strong
smell, but it is not pungent anymore at this lower concentration. I took appr. 2.5 ml of 50% perchloric acid and added 3 ml water to this to make it
more dilute.
Using these amounts, the methylamine is in excess amount. I slowly mixed the liquids (some heat is produced, but not as much as I expected). After
mixing, a clear and colorless liquid is obtained. No crystals are formed.
I poured the liquid in a petri dish and put this aside in a dry warm place without dust (40 C or so). The next day, I had a nice amount of crystalline
mass, which I scraped off the glass and crushed somewhat. Then I put the petri dish on the same place for another day. After that I had a perfectly
dry snow-white solid.
I assured in this experiment that I had excess methylamine. On drying, the methylamine evaporates, together with the water, and simply disappears.
This allows me to prepare a nice dry solid. If there is some excess HClO4, then you will get an ugly sticky and humid mess, which never gets dry.
HClO4 does not evaporate (like H2SO4) and is very hygroscopic. You can easily check whether you have excess methylamine. If the liquid has a "yummy"
smell, then there is free methylamine
The white salt is totally odourless.
Next, I tried ignition of this compound. It is comparable with the ethylene diamine complex, described at the start of this thread. The color of
combustion, however is a beautiful blue.
I also tried a small amount of this material in a test tube (only 10 mg or so, DO NOT SCALE UP!). Put it in a test tube, and then heat the test tube
in the flame of a bunsen burner. The material starts to fizzle a little, and then suddenly it decomposes with a blue flame and a kind of whistling
noise. After cooling down of the test tube, I added some water. On addition of the water, very dense fumes are formed in the test tube (I think due to
formation of HCl).
I have a camera which can make high speed movies at 1000 frames per second. I'll try to make a movie with this camera of the decomposition reaction.
Lighting is a difficult thing, however, with such high frame rates, the base/background lighting must be such that you get a meaningful image at at
most 1/1250 seconds expposure time.
|
|
|
fusso
International Hazard
Posts: 1922
Registered: 23-6-2017
Location: 4 ∥ universes ahead of you
Member Is Offline
|
|
Wont the excess MeNH2 absorb CO2 from air and form some methylamine bicarbonate?
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1386
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
@ woelen
All about perchlorates + some fuel (or anything) in interesting. Because here can be something for replace classic primary substances. But I am
afraid, that methylamine (commerce solution 40%) can be difficult available. Also HCLO4 is not some easily available. OIf course, that both compound
is possible prepare. Any way, very easy reaction and clear result. I think, that testing on Anvil is necessary for basic properties....  ...LL
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
| Pages:
1
2
3 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
