AlteredMatter Posted April 24, 2016 Posted April 24, 2016 Mumbles is right about the vacuum distillation of nitric acid. Although the nitric acid is perfectly usable even though it will be slightly yellow due to Nitrogen dioxide contamination, if you want clear nitric acid you must employ a vacuum. The higher temperature causes the nitric acid to decompose slightly with a cloud of nitrogen oxide gas. Vacuum distillation is no problem to me, but the amateur must educate himself on vacuum distillation first before even attempting such a complex method as opposed to distilling it at atmospheric pressure. You would have to use a cold trap, so the nitrogen dioxide does not get into your vacuum pump - most likely destroying it or heavily contaminating the oil. It would be quite an expensive mistake. So to make a long story short, atmospheric pressure distillation of nitric acid is the most economically feasible way to do it - of course in a well ventilated area.
blitzfike Posted June 13, 2016 Posted June 13, 2016 (edited) My local walmart has the liquid fire for $9.95, the search shows only 5 bottles in stock at this time. I much prefer to dissolve the smokeless powder in acetone for making the NC paint. I have done both the single base powders and the double base, but the DB stuff wasn't used in anything but as a coating. I use h2so4 in metal prep for some of the plating processes I do. None of it is nearly that strength for my purposes. I also use HCl with MnO2 and H3PO4 as part of another coating process for steel. All this supports the necessity for adequate ventilation and in an area where nothing is going to be destroyed by reacting with the fumes. Edited June 13, 2016 by blitzfike
pyrojig Posted June 15, 2016 Posted June 15, 2016 WTF ......How does this even remotely contribute to the Nitric acid thread??????????????????????????????????????????????
WSM Posted June 15, 2016 Posted June 15, 2016 WTF ......How does this even remotely contribute to the Nitric acid thread?????????????????????????????????????????????? It looks like the discussion of making nitrates drifted. A legitimate way to make nitrates is to neutralize nitric acid with the base of the metal nitrate you want, potassium carbonate, bicarbonate or hydroxide in the case of trying to make potassium nitrate. If you don't have nitric acid, but do have the laboratory equipment to properly make it, you then need sulfuric acid (the Queen of industrial acids) plus a nitrate salt to make nitric acid (to make whichever nitrate you need). I see why the discussion turned to sulfuric acid, but lets steer it back to making nitrates, which is the point of the discussion, after all. WSM
CrossOut Posted June 20, 2016 Posted June 20, 2016 (edited) To increase your yield, be sure to keep the reaction under 83c and cover your apparatus with aluminum foil to keep light out. I would also recommend pumping ice water through your condenser. But I'm usually to lazy for that step. A dark glass bottle should be used for your nitric acid as light will make it decompose. Alternatively you can just cover your bottle something to make it dark... Honestly, i use aluminum foil just try not to spill.. Glass stopper is required for this and I don't recommend keeping an air tight seal as pressure will build up. Just curious, Has anyone tried creating nitro cellulose by nitrating cellulose dissolved in a cellulose solvent? Edited June 20, 2016 by CrossOut
Arthur Posted June 20, 2016 Posted June 20, 2016 Rather than storing acid, if you have the facility to make it then make it when you need it, then use it all.
pyrojig Posted June 27, 2016 Posted June 27, 2016 Just curious, Has anyone tried creating nitro cellulose by nitrating cellulose dissolved in a cellulose solvent? I think it may pose problems with a nitration of said solvent, interfering with the NC nitration., I would follow text book nitration techniques from Patr and Copae and urbanski . I like my fingers .
Differential Posted June 28, 2016 Posted June 28, 2016 (edited) I don't think it's been mentioned yet, but the reason that 95-98% sulfuric offers such a big advantage over 60% sulfuric is that pure nitric acid has a much lower boiling point than the azeotrope. Pure nitric boils at 83C, and the 70% azeotrope boils at 121C. Nitric acid decomposes into water, oxygen, and NO2 the more you heat it. The ratio that works best for me is 1 part 95% H2SO4 (Rooto) and 1 part KNO3, by weight (H2SO4 in about 100% excess). If you add the KNO3 SLOWLY, and both chemicals are ice cold, you will get some nitric oxide but no NO2. Your boiling flask should be in an ice bath during the addition. The reaction fumes most when most of the nitric acid has been distilled, and I start heating more to get the last bit of it. I haven't tried vacuum distillation or bubbling dry air through the finished product, but I have high hopes for it! Edited June 28, 2016 by Differential
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