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Author: Subject: DIAMINOURONIUM (DI)NITRATE
twelti
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[*] posted on 14-6-2019 at 11:30


Quote: Originally posted by underground  
The dinitrate does not worth cause it forms a mono-hydrate. I have seen some other compounds with the same properties from NileRed. When a solution is super saturated sometimes it does not crystallize out. Scratching the container by pressing the crystals it will crystallize out. Also by dropping a single crystal it will crystallize out too. I don't think so we will have any issues. Also he used vacuum to drive off the water. I guess he did not dry the compound completely with vacuum cause he was afraid for decomposition. As long as i do not have any vacuum distillation set up, i will just use some cacl into a desiccator bad to drive all the water off. It may take a while but i believe it will remove all the water completely to dryness.

Any idea on whether a cheap vacuum pump (not rated for corrosive chemicals) would be ok to use for that?
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Yamato71
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[*] posted on 15-6-2019 at 23:21


If this product feels more comfortable existing as an oil after nitration, who are we to insist that it conform to a rigid crystalline structure? If I've learned one thing about EM's, it's that trying to make them do anything they don't want to do is not the path to true enlightenment. I know what you're thinking. "But we like our product to be nice and solid and dense and not runny and stuff".

So do I.

Say hallo to my leedle frenn. Fumed silica. This stuff is about the best thing to come along since perforated toilet paper. In the 1860's Alfred Nobel discovered that nitroglycerine would adsorb onto diatomaceous earth, simultaneously turning it into a pasty mass that could be extruded into paper cartridges and lowering its sensitivity. In 2017, Yamato71 discovered that adsorbing nitroglycerine onto fumed silica, another form of silica with a ridiculously high surface area to weight ratio, converts it into a non Newtonian fluid with some amazing properties. Only 5-7% by weight fumed silica added to NG converted it to a free standing gel that would not weep or puddle, even at elevated temperature. This form is easily dispensed from a syringe into places where liquid NG would leak out. !0% SiO2 stiffens it into a fair approximation of a translucent plastique. You might try that with your oily nitrate. I suspect that it will eventually crystallize in a fumed silica matrix anyway, but maybe not. In the meantime you will be able to tailor the final compound to any viscosity you desire.

Y71
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[*] posted on 16-6-2019 at 02:56


Quote: Originally posted by twelti  

Any idea on whether a cheap vacuum pump (not rated for corrosive chemicals) would be ok to use for that?


Get something like this, literally translated it would translate to "water jet pump", they are cheap (10 dollar-ish) and go down to the vapour pressure of the water being used.
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[*] posted on 16-6-2019 at 04:32


Quote: Originally posted by Yamato71  
If this product feels more comfortable existing as an oil after nitration, who are we to insist that it conform to a rigid crystalline structure? If I've learned one thing about EM's, it's that trying to make them do anything they don't want to do is not the path to true enlightenment. I know what you're thinking. "But we like our product to be nice and solid and dense and not runny and stuff".

So do I.

Say hallo to my leedle frenn. Fumed silica. This stuff is about the best thing to come along since perforated toilet paper. In the 1860's Alfred Nobel discovered that nitroglycerine would adsorb onto diatomaceous earth, simultaneously turning it into a pasty mass that could be extruded into paper cartridges and lowering its sensitivity. In 2017, Yamato71 discovered that adsorbing nitroglycerine onto fumed silica, another form of silica with a ridiculously high surface area to weight ratio, converts it into a non Newtonian fluid with some amazing properties. Only 5-7% by weight fumed silica added to NG converted it to a free standing gel that would not weep or puddle, even at elevated temperature. This form is easily dispensed from a syringe into places where liquid NG would leak out. !0% SiO2 stiffens it into a fair approximation of a translucent plastique. You might try that with your oily nitrate. I suspect that it will eventually crystallize in a fumed silica matrix anyway, but maybe not. In the meantime you will be able to tailor the final compound to any viscosity you desire.

Y71


Glad to hear you again. Keep the good work and ideas.
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twelti
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[*] posted on 16-6-2019 at 09:31


Quote: Originally posted by Tsjerk  
Quote: Originally posted by twelti  

Any idea on whether a cheap vacuum pump (not rated for corrosive chemicals) would be ok to use for that?


Get something like this, literally translated it would translate to "water jet pump", they are cheap (10 dollar-ish) and go down to the vapour pressure of the water being used.

Yes, an aspirator. Unfortunately for me, I don't have running water closeby. I should probably put in a sink?
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[*] posted on 16-6-2019 at 09:56


You can use a water pump and a with a big bucket where you collect the water to reuse.
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twelti
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[*] posted on 16-6-2019 at 15:56


Quote: Originally posted by Tsjerk  
You can use a water pump and a with a big bucket where you collect the water to reuse.

True, but I think you need a a strong water pump.
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[*] posted on 16-6-2019 at 17:39


Quote: Originally posted by Yamato71  
If this product feels more comfortable existing as an oil after nitration, who are we to insist that it conform to a rigid crystalline structure? If I've learned one thing about EM's, it's that trying to make them do anything they don't want to do is not the path to true enlightenment. I know what you're thinking. "But we like our product to be nice and solid and dense and not runny and stuff".

So do I.

Say hallo to my leedle frenn. Fumed silica. This stuff is about the best thing to come along since perforated toilet paper. In the 1860's Alfred Nobel discovered that nitroglycerine would adsorb onto diatomaceous earth, simultaneously turning it into a pasty mass that could be extruded into paper cartridges and lowering its sensitivity. In 2017, Yamato71 discovered that adsorbing nitroglycerine onto fumed silica, another form of silica with a ridiculously high surface area to weight ratio, converts it into a non Newtonian fluid with some amazing properties. Only 5-7% by weight fumed silica added to NG converted it to a free standing gel that would not weep or puddle, even at elevated temperature. This form is easily dispensed from a syringe into places where liquid NG would leak out. !0% SiO2 stiffens it into a fair approximation of a translucent plastique. You might try that with your oily nitrate. I suspect that it will eventually crystallize in a fumed silica matrix anyway, but maybe not. In the meantime you will be able to tailor the final compound to any viscosity you desire.

Y71


Very interesting ideas! If you want I can send you some diaminourea?
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[*] posted on 17-6-2019 at 07:42


What exactly is the liquid component left after the dinitrate is crystalized out? Would it be an inert if left in and absorbed like Yamato suggests? Also, won't it be even less sensitive? If it is already less sensitive that RDX, maybe hard to detonate?
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[*] posted on 17-6-2019 at 08:08


I wouldn't call RDX insensitive, any blasting cap can set it off.
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[*] posted on 17-6-2019 at 14:32


Quote: Originally posted by Tsjerk  
I wouldn't call RDX insensitive, any blasting cap can set it off.

Yes, it as all relative i suppose. Still, you are including an inert if you don't crystalize the dinitrate out and just absorb it all into the fumed silica.
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[*] posted on 17-6-2019 at 15:04


I think the point made by Yamato71 is that you don't need to crystallize it. And does it really matter if you add 10% of something inert? It got Nobel rich enough to have the most prestigious price named after him by paying for them.
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[*] posted on 17-6-2019 at 18:26


Quote: Originally posted by Tsjerk  
I think the point made by Yamato71 is that you don't need to crystallize it. And does it really matter if you add 10% of something inert? It got Nobel rich enough to have the most prestigious price named after him by paying for them.


True. But dynamite was the first truly usable high powered EM...

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[*] posted on 18-6-2019 at 02:32


By having 10% inerts it will drop the performance for sure. I can not see any reason why not to crystallize it and keep it as a liquid.
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[*] posted on 20-6-2019 at 16:33


I've described my experience with fumed silica in another thread since it doesn't relate directly to the subject of this thread. Having said this, I'll drop one more little nugget about fumed silica. When mixed with a stoichemetric amount of 325 mesh magnesium powder it makes an interesting flash powder. For one thing, it only flashes. Igniting a pile of it on a plate will result in a very intense flash of white light... and not much else. There will be a puff of white smoke, but almost no report. It can be packed into clear plastic tubing and will act as a fast fuse without rupturing the tubing. Have fun coming up with novel uses for this.
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[*] posted on 30-6-2019 at 14:33


All,

I am confused. If 65 percent nitric acid is used will the dinitrate form? Is 30 percent needed for the mononitrate??

Both sources from Klaptoke seem a little contradictory. Must I dilute the 65 percent nitric to ensure the dinitrate does not form? How do I choose one over the other?

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[*] posted on 30-6-2019 at 15:26


All. The carbohydrazide has an ammonia like odor that is very strong when the bag is opened. Is this a hydrazine odor or ammonia? Any safety precautions like a mask, or is this not necessary, this is new territory for me?
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[*] posted on 30-6-2019 at 18:25


It is quite normal to smell like ammonia since it is made out of hydrazine. Try not to smell it and use protective equipment. The concentration of nitric acid is not important as long as you use 1:1 molar ratio of NA and DU.
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[*] posted on 30-6-2019 at 22:41


But if I don’t add it all at once the concentration changes. But the tempture won’t allow adding all at once. So. I don’t understand...

Because with the first gram addition the concentration is 10M to 1M
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[*] posted on 30-6-2019 at 23:32


The formation of the mono and the di-nitrate are equilibrium reactions, so if you add the carbohydrazide to the nitric acid you will form the di-nitrate first. But when more carbohydrazide is added the not nitrated molecules will pick up the second nitrate from the di-nitrated molecules which will make you end up with a batch of mono-nitrated carbohydrazide.
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[*] posted on 4-7-2019 at 12:27


Quote: Originally posted by underground  
By having 10% inerts it will drop the performance for sure. I can not see any reason why not to crystallize it and keep it as a liquid.

Just wondering what those "inerts" are? I am not a chemist, but in looking at the equation, DAU just picks up an H and a nitrate group from the HNO3. I'm guessing the water takes part in the equilibrium process, but at the end there should just be DAU mononitrate and water. SO, can higher strength NA be used so there is less water at the end? Also, if we tried yamato's fumed silica idea, would the water just evaporate anyway? I would think it would evaporate rather quickly, due to the large surface area. Then no inerts. Maybe density would then be low though...?
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[*] posted on 4-7-2019 at 12:29


Read that PDF out and all your questions will be answered.

http://www.sciencemadness.org/talk/files.php?pid=614532&...
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[*] posted on 4-7-2019 at 12:57


Quote: Originally posted by underground  
Read that PDF out and all your questions will be answered.

http://www.sciencemadness.org/talk/files.php?pid=614532&...

I have read it. I may not understand all of it, not being a chemist. I don't see the answers to my questions there. For example it says that the DAU is a strong base, so only weak NA is needed. It doesn't say you can't use stronger NA (less water to get rid of at the end). I'm also wondering if the solution could be heated to drive off water, since it does not decompose until 240 degrees. If I understand correctly.
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[*] posted on 4-7-2019 at 13:12


The mononitrate and dinitrate can be made by adjusting the nitric acid molar ratio. 1:1 molar ratio of DAU and NA will produce the mononitrate, while 1:2 molar ratio will produce the dinitrate. We may have to dilute the NA a bit too and keep it cool. From PDF, they used 2M NA witch actually contains 22.2 mmol per 11.1 mL. It may dry out by heating once the mononitrate decomposes at 242 C. Also a desiccator bag may drive off all the water too. We have to both them out.

To give you an idea, distilled water was added to 97gr of 65% NA (1MOL) until 500ml reached. Then 90,09g of DU (1MOL) was added to that solution.

Now i am not sure if the NA have to be diluted that much, another person with some better knowledge in chemistry is welcome to answer.

[Edited on 4-7-2019 by underground]
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[*] posted on 4-7-2019 at 16:13


Quote: Originally posted by underground  
The dinitrate does not worth cause it forms a mono-hydrate. I have seen some other compounds with the same properties from NileRed. When a solution is super saturated sometimes it does not crystallize out. Scratching the container by pressing the crystals it will crystallize out. Also by dropping a single crystal it will crystallize out too. I don't think so we will have any issues. Also he used vacuum to drive off the water. I guess he did not dry the compound completely with vacuum cause he was afraid for decomposition. As long as i do not have any vacuum distillation set up, i will just use some cacl into a desiccator bad to drive all the water off. It may take a while but i believe it will remove all the water completely to dryness.

I thought we were after the mono nitrate. That is 5 ml 10 mmole 2M NA.
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