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Author: Subject: Ethylene diamine perchlorate
woelen
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[*] posted on 14-5-2019 at 00:19


MeNH2 does not form a carbonate (at least not in appreciable amounts). I once tried this by putting a little 40% methylamine in a petri dish and allowing it to evaporate. Hardly any residue is formed, the glass only is a little frosty at the place which was wet. That may also be due to impurity of the methylamine solution.

I also tried this with ethylamine (70% by weight) and with ethylene diamine. The ethylamine also does not form any residue. The ethylene diamine leaves behind quite a lot of yellowish solid. It is somewhat oxidized and it forms a carbonate.

You can see the difference already when you keep the liquid in contact with air. Methylamine and ethylamine do not give off any visible fumes, ethylene diamone gives off dense white fumes in contact with air.

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I tried the same experiment with HClO4 and methylammonium chloride (a.k.a. methylamine HCl, CH3NH2.HCl). The latter is a salt. I tried dissolving this in a small amount of water and then adding 50% HClO4 to it. I used a slight excess amount of methylamine HCl.

When this liquid is allowed to stand in a warm place, you don't get any crystals. A colorless somewhat viscous liquid is produced, which does not dry further. This liquid is strongly acidic.
I tried heating some of this liquid, trying to drive off water and HCl. To some extent this works, but I could not get a clean dry solid compound. Before making it completely dry, it decomposes violently, with a blue flame and a loud WHOOSH sound. I think that the liquid invisibly goes from the aqueous solution form to a molten form and then it decomposes.
I dared not try the boiling down of a larger volume than a few drops. I can imagine that a few ml of this liquid, suddenly starting the violent decomposition reaction may lead to an explosion, due to self-confinement. I do not want pieces of glass flying around at high speed.

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Methylamine is easy to obtain in the EU, either as its salt methylamine HCl, or as 40% solution in water. I ordered both of them, no questions asked. Use of methylamine for making crystal meth is not a problem in NL. Here we have quite some illicit drugmakers, but they make other drugs than crystal meth (eg. GHB, XTC, purified THC).

HClO4 is not that difficult to obtain as 60% solution, but it is expensive. A price of 70 euros per liter is not uncommon. For my small-scale experiments with 1 gram quantities this is not a real problem. Half a liter of acid goes a long way. Making KClO4 or NaClO4 from the acid is easy, but economically not feasible if you want quantities useful for a serious explosive device. So, there was no need to make HClO4 a forbidden chemical, it is not interesting for terrorists trying to make bombs.
The compound NH4ClO4 is available in NL as well (only the sodium and potassium salt are forbidden), and probably it also is available in the USA. It can be used to make (somewhat impure) HClO4. In order to do so, you first need to mix solid NaOH with solid NH4ClO4 in a 1 : 1 stoichiometric ratio. Dissolve the NaOH in as little as possible of water. Once you have a solution, slowly add the NH4ClO4 in small batches. In the beginning, after each addition you get a lot of NH3 gas. At the end of the reaction, you may need to heat to get all of it dissolved and to drive off all NH3. Keep on heating, until all NH3 is gone.
Next, allow to cool down. If any crystals are formed, add a tiny amount of water in order to dissolve them. Afther that, pour the solution slowly in concentrated HCl, while stirring. You get a precipitate of NaCl. Filter the solution from the NaCl. Allow to cool down to remove more NaCl.
Next, boil down until the liquid is 150 C or so and then allow to cool down again. You most likely get another small amount of solid NaCl.
The remaining liquid is fairly pure HClO4 (50% by weight or so), containing only a small amount of sodium ions and it may be colored a little, due to colored impurities of your HCl. If you use reagent grade reagents, then your HClO4 should be (nearly) colorless. This acid is perfectly suitable for experiments as described in this thread.


[Edited on 14-5-19 by woelen]




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[*] posted on 14-5-2019 at 01:59


Incredibly comprehensive and detailed answer. In particular, the preparation of HClO 4 appears to be more advantageous, cheaper when using NaOH. I tried NH4ClO4 + HNO3 + HCl method. It works. In HClO4 remains NH4ClO4 as reziduum. With your NaCl method. The second part of the reaction is almost identical, thus increase temperature to 150 ° C. In this step excess HCl is evaporated. HClO4 remains. Good method, thank you....:cool:...LL



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[*] posted on 14-5-2019 at 03:38


I know of the HNO3 method, but nitric acid is forbidden in the EU since 2016. You cannot purchase it anymore.
Hence, I worked out the method with NaOH. NaOH can be obtained in any hardware store and conc. HCl also is no problem.

In the past, before HNO3 was forbidden, I have tried the HCl/HNO3 method myself. It didn't work for me very well. I got a lot of left-over NH4ClO4, I had the impression that even after prolonged boiling not all NH4(+) ions were oxidized, while at the same time tons of Cl2 and ONCl were released. Very unpleasant! Maybe my acids were not sufficiently concentrated at that time (I used 30% HCl and 53% HNO3).



[Edited on 14-5-19 by woelen]




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[*] posted on 14-5-2019 at 08:57


Your method is clearly better. NaCl has (I estimate) smaller solubility in HClO4 than NH4ClO4. Therefore is final product purity better. A lot experimentators has problem with availability HClO4. Your method is base key for much attempts. Easy and cheap. Almost the invent.....Thanks.....:cool:...LL



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