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Author: Subject: Wich salt makes the most attractive nitration mix with H2SO4?
Dany
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[*] posted on 11-8-2013 at 14:22


Hello Papaya,

Aryl boronic acid can be used with alkylnitrite for aromatic nitration of electron rich substrate. Electron poor substrates need the addition of Boric acid to accomplish the nitration

see Sheme 18 of the following paper on aromatic nitration:







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Fantasma4500
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[*] posted on 28-8-2013 at 10:24


Quote: Originally posted by caterpillar  
You, boys, are wrong about Ca(NO3)2. It has its own advantages. I tried all of aforementioned salts. I used KNO3 for TNP preparation and I think that it is the best choice for this particular compound. I got a runaway reaction, when I tired to use NH4NO3 instead. It was a mild reaction, but I got a foam with red bubbles and had to stop process. Ca(NO3)2 is the best choice for NC or NG. There are some simple tricks with it. You have to delete all water from it and then smash this mass to small pieces, but not to dust. 1-3 mm in size. Then put it into H2SO4- I used 92-94 % acid. Wait for a day and night. some times you have to turn a bottle with mixture bottom up- pieces of Ca(NO3)2 must go down through acid. Then you may decant the upper layer. Yeah, you'll loose some mixed acid with CaSO4, because it forms very small crystals. But most likely it extracts some water from acid and therefore increases concentration of resulting mixed acid.


would this mean, that you would be able to make pretty well 99% HNO3 somewhat, without any CaSO4 being suspensed in the solution?? thats very interesting, i didnt consider that the H2SO4 / Ca(NO3)2 mix would create runoff when i filtered it through paper. anyhow i still stick to the idea that it will fully work if using a nice big sheet of NC for filtering it with (bought NC perhaps, or extracted from fireworks?)




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https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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caterpillar
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[*] posted on 28-8-2013 at 14:16


The upper layer was transparent, therefore there was no CaSO4, floating in. You may use glass material or asbestos for filtering after decantation of the upper layer. I do not think, that in that way one may get pure HNO3- same problem with floating CaSO4. I made usual mix- 60% H2SO4 and 40% HNO3. Therefore, initially I had large enough amount of liquid and pieces of Ca(NO3)2 was completely covered with sulfur acid. If one take smaller amount of H2SO4, wanting to get only HNO3 plus gypsum, he surely will get mess of liquid and small crystals and no upper layer to decant it. But may be even in such case liquid could be extracted, using vacuum filtering. I never tried- do it for yourself.



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