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ManyInterests
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[*] posted on 26-11-2021 at 14:16


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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[*] posted on 27-11-2021 at 05:01


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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[*] posted on 27-11-2021 at 19:38


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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[*] posted on 29-11-2021 at 05:34


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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[*] posted on 29-11-2021 at 06:06


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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[*] posted on 17-4-2022 at 14:16


I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?
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[*] posted on 17-4-2022 at 14:46


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.


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




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[*] posted on 17-4-2022 at 17:57


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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[*] posted on 17-4-2022 at 20:41


Quote: Originally posted by MineMan  
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?

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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[*] posted on 18-4-2022 at 06:05


Quote: Originally posted by Lomax  
Quote: Originally posted by MineMan  
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?

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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[*] posted on 18-4-2022 at 06:19


Quote: Originally posted by MineMan  
Quote: Originally posted by Lomax  
Quote: Originally posted by MineMan  
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?

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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[*] posted on 20-6-2022 at 12:51


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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