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ManyInterests
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That sounds good. It will need maybe some experimentation for it to work. But I got other question related to NHN synthesis.
For the hydrazine, when making it using the Hoffman degradation of urea (how I made hydrazine sulfate) would the hydrazine that is made before the
addition of sulfuric acid and cooling to extract the hydrazine sulfate be adequate to make nickel hydrazine nitrate? As in just adding the nickel
nitrate solution to the hydrazine at 65 C be enough? That seems much easier than making the sulfate then freebasing it again. I can make the hydrazine
and use it on the spot instead of storing it for later.
Also about the nickel nitrate hexahydrate. I saw people make it with nickel metal, nitric acid, and hydrogen peroxide as a catalyst. Do we need to dry
it or boil it down to extract the hexahydrate, or would simply refluxing the three reagents for a few hours be enough? And the resulting solution
added to the hydrazine as prepared above?
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katyushaslab
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No, the hydrazine in solution with unreacted urea, unreacted NaOCl, and all the side products is not going to be clean enough to work with.
You need to extract it as hydrazine sulfate, then freebase. This step will ensure that you have a clean enough starting material, no weird fucking
side reactions, etc.
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ManyInterests
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OK that makes sense.
So I think this will likely be my final question for a good while... when making the nickel nitrate. I've seen everyone react nickel metal (I have
99.6% pure nickel metal. It's very shiny and extremely clean) that's been cut to tiny pieces. The process I've seen is to add around 30% hydrogen
peroxide to it as a catalyst and 68% nitric acid in a flask and then to reflux it gently for several hours. (I plan on using a hot water bath for this
and never let the water reach a rolling boil around 90C or so should be sufficient).
After refluxing for hours, can this mixture be added directly to the hydrazine or would it need to be filtered? If the hexahydrate needs to be vacuum
filtered, what is the optimal way of cleaning the buchner funnel? Just distilled/tap water or any other solvent is necessary? I heard that that Nickel
Nitrate hexahydrate is hard to filter as it is a very fine particulate. Would it go through several layers of coffee filters?
Just getting info for the NHN synthesis. The HDN/RDX/Keto-RDX seems simple as all I need for that is fuming nitric acid at this point.
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katyushaslab
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I can't really answer to the "making nickel nitrate" question authoritatively, given I just buy my nickel nitrate.
I would, however, strongly advise filtering the nickel nitrate solution, boiling it down, and maybe recrystallizing from distilled water - just to
remove any unreacted nickel, etc. If I recall correctly, nickel might be one of those metals that can cause hydrazine to decompose.
More steps cleaning up your reactants will result in a safer, more reliable product. Taking shortcuts is inadvisable (though sometimes oh so
tempting).
As for the HDN/RDX: a good efficiency tip is to use any weak nitric (say, created from traps while distilling - see the NurdRage videos) to make the
HDN. As for the RDX part - you want white fuming nitric instead of red fuming nitric, bubbling dry air through RFNA will clear it up. Some people add
a small amount of urea to clear their nitric, but I've had mixed results with that, dry air bubbling has been more reliable.
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ManyInterests
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I have a small palm-sized 12v air pump (works for blowing and vacuum) and some clear PVC tubing. I did heard that vinyl plastic doesn't get destroyed
easily by highly concentrated nitric acid, so I will cut a short length to bubble out the NO2 when I make some more nitric acid. I know that the
specific gravity of the acid must be 1.49 or 1.50 at room temperature it for it to be WFNA and work for RDX or Keto-RDX. I think I might try doing
keto-RDX as it seems more powerful and still retains the stability of RDX. Also it would require a nitrating mixture of H2SO4 that will let me use up
my remaining H2SO4 and stretch my WFNA supply.
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Lomax
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I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?
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Rainwater
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Quote: Originally posted by ManyInterests  | | I have a small palm-sized 12v air pump (works for blowing and vacuum) and some clear PVC tubing. I did heard that vinyl plastic doesn't get destroyed
easily by highly concentrated nitric acid, so I will cut a short length to bubble out the NO2 when I make some more nitric acid.
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I have noticed considerable vacuum formation inside of a sealed apparatus connected to a bubblier, resulting in water sucking back into my collection
flask. The best method I have discovered is by using a cold trap with dry ice to solidify the gas. After the no2 generating reaction is complete, I
add an equal volume of ice to the cold trap and allow the apparatus to slowly warm up. The reaction produces a consentrated nitric acid
"You can't do that" - challenge accepted
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MineMan
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| Quote: Originally posted by Lomax | | I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine? |
Instead of sulfuric acid?
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Lomax
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Yes sience sulfuric acid can be replaced with sodium bisulfate for a number of reactions (Nitric Acid) for example. I thought it can be used as a
dehydration agent for Nitrourea or Nitroguanidine sience Conc. Sulfuric Acid is very regulated in my country.
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MineMan
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| Quote: Originally posted by Lomax |
Yes sience sulfuric acid can be replaced with sodium bisulfate for a number of reactions (Nitric Acid) for example. I thought it can be used as a
dehydration agent for Nitrourea or Nitroguanidine sience Conc. Sulfuric Acid is very regulated in my country. |
Someone on here will know. It may be better to post in general chemistry. Can you try it yourself as well… everyone would be very interested in this
answer
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Lomax
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| Quote: Originally posted by MineMan | | Quote: Originally posted by Lomax |
Yes sience sulfuric acid can be replaced with sodium bisulfate for a number of reactions (Nitric Acid) for example. I thought it can be used as a
dehydration agent for Nitrourea or Nitroguanidine sience Conc. Sulfuric Acid is very regulated in my country. |
Someone on here will know. It may be better to post in general chemistry. Can you try it yourself as well… everyone would be very interested in this
answer |
Ok
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Morgan
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I have a cylinder-shaped pencil holder like thing consisting of a tower of spaced aluminum rings and at the base a disc of clear glass bonded to the
bottom aluminum ring. It looks like a clear glue of some sort so I tried heating it as much as I dared to break the bond and also acetone for the heck
of it. Maybe it's an epoxy glue but what typically is used to glue glass and is there something that might break the bond? Maybe it's silicone.
[Edited on 20-6-2022 by Morgan]
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specialactivitieSK
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What exactly is LD-70 carrier? Thx.
https://youtu.be/h_zQUrvP_LE
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jerry0nim0
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I've found something like this:
"[...] LD-70, a plastigel binder containing polyacrylate and dinitrodiethyleneglycol (70 %), dinitrotriethyleneglycol (30 %) monopropellants"
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underground
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What is going to yield when diaminourea/diaminoguanidine dinitrate reacting with 98% H2SO4 at low temp ? (similar to guanidine nitrate forming
nitroguanidine)
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otonel
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What is the best method to make picric acid from tetryl (2,4,6-Trinitrophenylmethylnitramine)?
[Edited on 27-11-2022 by otonel]
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dettoo456
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@underground It may likely form the Aminonitroguanidine (ANQ) or Dinitroguanidine (DNQ) but the classical synth of DNQ iirc involves direct
nitration of NQ with Oleum and WFNA. Either way, the DNQ and Dinitrourea (DNU) are both known as extremely unstable to STP conditions and will
hydrolzye before they’re ever useful. ANQ is stable though but the normal synth to that involves amination of NQ - see DBXLabs’ prep for deets.
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Hey Buddy
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Nitrosoguanidine sensitivity?
I know nitrosoguanidine is referenced as a demonstration novelty, but it is reported to act as a primary explosive, sensitive to match head heat. Has
anyone tried to dope other explosives with nitrosoguanidine? to use the nitroso as a catalytic sensitizer to then initiate reaction in another
borderline secondary like ETN/PETN?
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dettoo456
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It might be useful on its own but nitrosoguanidine is notoriously carcinogenic. AFAIK the cyclic nitroso analogues are much less toxic than even their
nitro counterparts but aliphatic (especially guanidine) nitroso compounds are to be handled extremely carefully (assuming you want kids in the
future). Polynitroimidazoles, formed via the decomp and oxidative nitrosation of nucleotide bases (Adenosine & xanthines) or through condensation
of guanidines and dialdehydes or guanidines and glycine, could prove useful for boosters - at least that’s what I’m trying to look into.
Otherwise, I’d just stick with the classic trains like NiAQ-ClO4 or LS/Ba(ClO3)2 -> pressed PETN or CHP -> bulk EM. Sensitizing ETN and/or
PETN beyond their normal decomp temperatures sounds like it could be sketchy but if you think it could be useful... there’s no harm in testing
(small scale ofc).
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Hey Buddy
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Nitroguanidine reduction
I screwed up an electrolytic nitroguanidine reduction by using a copper anode. This creates a red colored substance from the nitroguanidine at cathode
on lead, with a clay pot diaphragm separation. I have actually done this before mistakenly a few years ago, so it felt really stupid to see again, but
I forgot. I also forgot what this material is. I dont want to throw it out. It's red and smells of ammonia and is in the cathode compartment. I think
Thiel writes about it but I cant find it. If anyone remembers what this substance is please share. Thank you. I think maybe it's a strange
tetrazine...cant remember
[Edited on 14-12-2022 by Hey Buddy]
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Hey Buddy
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Guanidine reaction with hydrazine?
Does anyone know what the product of hydrazinolysis of simple guanidine is? I would assume aminoguanidine, analogous to NQ hydrazinolysis giving ANQ.
--Cant find examples of this reaction anywhere.
In searching I found a NASA technical report: Aminoguanidine Nitrate can be made from NQ + N2H4 +NH4NO3 or NQ + N2H4*HNO3 in ammonia solution. Still
not sure what comes of Guanidine.
[Edited on 28-12-2022 by Hey Buddy]
[Edited on 28-12-2022 by Hey Buddy]
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Mr.Fluorine
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I've been trying to figure out what the reason is for PETN being so much more insensitive than other alkyl nitrate esters. Nitroglycerin or ETN are
considered much more sensitive, why is this? Is it due to steric strain or maybe primary nitrate esters are just much less sensitive?
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BerthelotOnCrack
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In the wiki, the proposed nitrocellulose synthesis uses only 2.5 grams of cellulose for 0.25 moles of nitrated salt and 50mL sulfuric, but according
to wikipedia a mole of nitrocellulose is 3 moles of nitrogen, so with 0.25 moles of nitrogen in the salt, say KNO3 here, you could make 0.083 moles of
nitrocellulose aka... 13.4 grams of ideally trinitrated nitro. Is there a specific reason to waste so much nitrates here ? Or was it just for safety
concerns
Edit: Also has anyone tried mashing paper to get the cellulose ? It would be more convenient than buying 20 bags of 10g of cellulose and I think they
use pure wood pulp in industrial bullet propellant production, which is exactly that
[Edited on 3-1-2023 by BerthelotOnCrack]
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Rainwater
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NOx is a side product removing nitrate from the reaction.
"You can't do that" - challenge accepted
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BerthelotOnCrack
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Given I have done only a couple nitrations yet, I'm not saying you are wrong but if 81% of the nitrates formed NO2 I would be dead or something, I
recently made ~50 grams of nitro at once and there was *zero* orange fumes, It would have been apocalyptic
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