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Author: Subject: NHN synthesis not working
wessonsmith
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[*] posted on 18-2-2020 at 14:27


Quote: Originally posted by Rosco Bodine  
There is no contradiction in what you have observed. The concentration of a reaction mixture and rate of addition, generally are inversely proportional and act counter to increasing crystal size while temperature increase promotes larger crystals.

Greater dilution, slower addition, longer reaction time, higher temperature, and more turbulence to keep precipitates suspended instead of forming "sand dunes" on the bottom of the reactor promotes crystal growth to larger size, and generally the reverse of those factors results in much smaller crystals.

You could try 90 C and see what results at half the concentration with half rate of addition and 4 times longer reaction time with increased turbulence if needed...to see if there is any difference. But a disadvantage is that yield can suffer when a reaction is not being optimized for yield but for a specific physical form for the product. So what is an optimal synthesis can be a tradeoff to find what is most practical.

[Edited on 2/18/2020 by Rosco Bodine]


I think 90C would be pushing the safety limit for hydrazine. Here is a study that was done on NHN. They tried both 65C and 25C and documented the results.

https://www.amazon.com/clouddrive/share/sRTDsJNM9rHNa7FPQ9gh...
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Rosco Bodine
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[*] posted on 18-2-2020 at 16:07


Temperatures well exceeding 90C won't likely be a problem for aqueous hydrazine.

It is used industrially as a boiler water oxygen scavenger, and superheated under pressure in steam plants.

Personally I would have no huge fear issue running it into a complexation reaction mixture even at 95C.


Sigma pump it into the reactor, microaddition stream through a capillary well below the surface and it will complex and be sequestered before air exposure degrades it.


[Edited on 2/19/2020 by Rosco Bodine]
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wessonsmith
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[*] posted on 18-2-2020 at 16:28


Quote: Originally posted by Rosco Bodine  
Temperatures well exceeding 90C won't likely be a problem for aqueous hydrazine.

It is used industrially as a boiler water oxygen scavenger, and superheated under pressure in steam plants.

Personally I would have no huge fear issue running it into a complexation reaction mixture even at 95C.


Sigma pump it into the reactor, microaddition stream through a capillary well below the surface and it will complex and be sequestered before air exposure degrades it.


[Edited on 2/19/2020 by Rosco Bodine]


I might experiment with a higher temp. As it stands now, the NHN I produce at the 65-70c range has excellent properties. In my detonators and as the small particle size energetic for my plastic. I can't imagine it can get any better, but perhaps.
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Rosco Bodine
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[*] posted on 18-2-2020 at 20:01


So continuing this "stream of consciousness" ....I can offer this idea ...

Tris semicarbazide manganese perchlorate is another possible compound that might be interesting. I have investigated *zero* references about this speculated material.

Maybe form a solution of calcium perchlorate by reacting Calcium Hydroxide in excess with Ammonium Perchlorate and heating to drive off byproduct Ammonia, filter to obtain solution of Calcium Perchlorate. Mix solution of Calcium Perchlorate with solution of Manganese Sulfate and filter precipitated Calcium Sulfate from solution of Manganese Perchlorate. React solution of Manganese Perchlorate with 3 equivalents of Semicarbazide to form Tris Semicarbazide Manganese Perchlorate.

That would be the perchlorate analog of the nitrate variant described in attached patent US6127564


Attachment: US6127564 Semicarbazide Manganese Complex.pdf (79kB)
This file has been downloaded 21 times



[Edited on 2/19/2020 by Rosco Bodine]
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wessonsmith
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[*] posted on 19-2-2020 at 07:29


Quote: Originally posted by Rosco Bodine  
So continuing this "stream of consciousness" ....I can offer this idea ...

Tris semicarbazide manganese perchlorate is another possible compound that might be interesting. I have investigated *zero* references about this speculated material.

Maybe form a solution of calcium perchlorate by reacting Calcium Hydroxide in excess with Ammonium Perchlorate and heating to drive off byproduct Ammonia, filter to obtain solution of Calcium Perchlorate. Mix solution of Calcium Perchlorate with solution of Manganese Sulfate and filter precipitated Calcium Sulfate from solution of Manganese Perchlorate. React solution of Manganese Perchlorate with 3 equivalents of Semicarbazide to form Tris Semicarbazide Manganese Perchlorate.

That would be the perchlorate analog of the nitrate variant described in attached patent US6127564
[Edited on 2/19/2020 by Rosco Bodine]


Interesting. Here is a link to a PDF of experiments done on various NHN analogs.
https://www.amazon.com/clouddrive/share/pI2jIvnYirlhkCnj1ioc...

[Edited on 19-2-2020 by wessonsmith]
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Rosco Bodine
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[*] posted on 19-2-2020 at 12:49


That linked paper seems familiar ....:D

http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...

Pasteurized Sunglasses.bmp - 1.6MB
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wessonsmith
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[*] posted on 19-2-2020 at 13:11


Quote: Originally posted by Rosco Bodine  
That linked paper seems familiar ....:D

http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...


Great minds think alike:)
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Rosco Bodine
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[*] posted on 19-2-2020 at 13:26


Hindsight is 20/20 and what da ya know .....
looking back it is like deja vu all over again....
and here we are in 2020 for real
Hindsight is like a time machine for sure :D

https://www.youtube.com/watch?v=Rp20xUdx62Q Out Of The Blue - APP

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Rosco Bodine
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[*] posted on 19-2-2020 at 14:44


Mixed complexes and complex double or multiple salts are likely possible in this class of compounds where it might be interesting to first form an ammonium complex in solution and then add the desired substituent complexing agent of higher molecular weight which should in part or completely displace the ammonium. Methylamine, glycine, betaine, hydrazine, semicarbazide, carbohydrazide, aminoguanidine, ethanolamine, ect, should act in this way when added alone or in combination, and interesting products should be precipitated having compositions that would depend on the ratio of substitutents added.
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[*] posted on 20-2-2020 at 11:30


Quote: Originally posted by wessonsmith  
Here is the NHN synthesis video.

https://youtu.be/rPxdDSUGxo4


Hi Wessonsmith, has this been deleted? Just tried to check it out and no luck.
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[*] posted on 20-2-2020 at 12:49


Quote: Originally posted by B(a)P  
Quote: Originally posted by wessonsmith  
Here is the NHN synthesis video.

https://youtu.be/rPxdDSUGxo4


Hi Wessonsmith, has this been deleted? Just tried to check it out and no luck.


it's back up. I take down my videos to stay under the radar. Please download anything you like.
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[*] posted on 20-2-2020 at 13:25


Quote: Originally posted by wessonsmith  
Quote: Originally posted by B(a)P  
Quote: Originally posted by wessonsmith  
Here is the NHN synthesis video.

https://youtu.be/rPxdDSUGxo4


Hi Wessonsmith, has this been deleted? Just tried to check it out and no luck.


it's back up. I take down my videos to stay under the radar. Please download anything you like.


Great thanks so much! Another excellent video.
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Rosco Bodine
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[*] posted on 21-2-2020 at 06:47


Quote: Originally posted by wessonsmith  
Quote: Originally posted by B(a)P  
Quote: Originally posted by wessonsmith  
Here is the NHN synthesis video.

https://youtu.be/rPxdDSUGxo4


Hi Wessonsmith, has this been deleted? Just tried to check it out and no luck.


it's back up. I take down my videos to stay under the radar. Please download anything you like.


You could upload the video files to the scipics directory here, if the allowable file types permit this and files aren't too huge.
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