zzz said:Recovery the nitrate salt for make distillation: obviusly the nitric used to make aqua regia is irrecoverable...
goldenchild said:zzz said:Recovery the nitrate salt for make distillation: obviusly the nitric used to make aqua regia is irrecoverable...
Could you not recover nitric if a reaction is performed in a distillation setup? This process seems a bit involved. Would you ever consider making a video?
goldenchild,goldenchild said:I was actually thinking of fractional distillation with the feed stock placed into the reaction vessel to react. No bubbling.
zzz said:goldenchild,goldenchild said:I was actually thinking of fractional distillation with the feed stock placed into the reaction vessel to react. No bubbling.
there are not distillation of nitric from aqua regia because with heat you will form nitrosyl chloride (and not nitric) that decompose in NO2 and Cl.
goldenchild said:zzz said:goldenchild,goldenchild said:I was actually thinking of fractional distillation with the feed stock placed into the reaction vessel to react. No bubbling.
there are not distillation of nitric from aqua regia because with heat you will form nitrosyl chloride (and not nitric) that decompose in NO2 and Cl.
So the red fumes coming off a reaction are not nitric and can't be condensed? I'm talking about dissolving metals with both AR or just nitric.
"I tried also to add directly sulfuric acid into reaction vessel of gold pins with nitric to restore nitric strengt, it work, but is a little wasteful and you need to work with an excess of water because sulfate salt created can crystallize, or can form foam, and could give you a lot of trouble (like metastannic)."
butcher said:"I tried also to add directly sulfuric acid into reaction vessel of gold pins with nitric to restore nitric strengt, it work, but is a little wasteful and you need to work with an excess of water because sulfate salt created can crystallize, or can form foam, and could give you a lot of trouble (like metastannic)."
zzz,
Did you read how I do the reaction in to kill two birds with one stone?
The pins need to be clean of tin and solder for best results, also cutting the pins help to get all of the copper to react easier.
I have no foaming other than when concentrated HNO3 in solution azeotropes, this reaction of vigorous bubbling that I am talking about at the point of azeotrope of the acid would happen even if the only thing I had in the reaction vessel was NaNO3 and sulfuric acid, I am not sure if the reaction I have is the same thing as you are describing when your mentioning you noticed foam or not, but when I see the tiny bubbles of this reaction begin the heat is lowered till the reaction of vigorous bubble are slowed from HNO3 wanting to react too fast and boil out almost all at once later the heat is raised again.
A little extra water I use in the reaction is not a problem for me because I can concentrate the nitric made to 68% by evaporation, or use the more dilute nitric as is, or dilute it further if needed.
The blue copper sulfate that forms if you do not let them cool or form hard salts (keeping them hot and adding boiling water before they harden to salt, to dissolve them before they harden so your gold foils precipitates to the bottom of the dilute blue copper sulfate solution.
The brown fumes of NO2 if bubbled into water will form nitric acid, a little peroxide in solution can help and if some clear fumes of NO the H2O2 can help to make nitric out of these also, there is some lose of the gases also because the bubble are usually large and some of them will not covert the first time they go through water (not enough reaction time in the jar going through water if you were concerned with the little bit of lost gas you could rig up a series of jars to bubble the gases through.
As far as recovering nitric from aqua regia, capturing the NOx gas bubbling it into water to make nitric acid, yes some chloride gases will be carried over and as the NOx forms. Chlorides could be removed with silver nitrate, but that would take a lot of silver nitrate and you then be making silver chloride to deal with, I would not mess with that.
What I do every once in a while is use the evaporated gases from the aqua regia process bubbling it into a water diluted HCl solution with additions of 3% peroxide to make a very dilute aqua regia that can be used with the heat of evaporation on another batch, but aqua regia cannot be stored, and does not last long so this is not done if you cannot use it soon on another batch, (can also be used help clean some of the heavy sludge bubbled into in a stock pot), (this can help to tame some of those rougher fumes from around your aqua regia solution and do a little work with them).
With intuition, because large scale is ever better than small scale...butcher said:If you have not read or done a process, how would you know if it would work or not?
zzz said:Hi everyone, some weeks ago i wrote a post where i said that i'm able to make 5 liters of high concentrated nitric acid with 2 $ of spending.
Well the yield is better because you will only need the first spending for sulfuric and nitric salt than you can recovery all you have used.
We need to have an initial point where to make our first nitric acid distillation. I personally prefer potassium nitrate and sulfuric used for clean.
Making the right proportion for distillation: 2 KNO3 + H2SO4 > 2 HNO3 + K2SO4
Recovery the nitrate salt for make distillation: obviusly the nitric used to make aqua regia is irrecoverable, but if you used that for dissolve silver for inquartation (silver will passivate in the chloride solution) or for dissolve copper in gold pin, you can reuse copper nitrate as salt to make distillation, forming useful CuSO4 as product, (if this came from aqua regia distillation You would still have chlorides involved) and now everybody know that with electrolisys you can recovery the sulfuric acid (and also pure copper) from this, but above all, this allows you to skip the next step that consists in recovering sulfuric acid from everyother sulfiric salt different from CuSO4.
Recovery sulfuric acid procedure from everyother sulfuric salt different from copper sulfate (what everyone wants to know): in this distillation example we have as product K2SO4.
Take it and make a satured solution in water (is a little bit difficult to dissolve once is cristallized, use hot boiling water to do that)...
now all you can do is to add Copper Chloride (in satured solution or in powder as you prefer -> so keep copper chloride) and you will have a white precipitation of Potassium Chloride (CuCl2 + K2SO4 --> NO Reaction you just have a solution of potassium, chlorides,sulfates and copper ions floating around in solution nothing here is insoluble so there is no reaction) (very useful and expensive chemical product) and a satured solution of Copper Sulfate, that brings you to the end of point 1. You will have a precipitation of Potassium Chloride because his solubility is very very lower than Copper Sulfate, so Copper Sulfate will take the place in solution. .(see above no precipitant)(i've never tried point 2 with calcium sulfate so i don't know if it will work with it, but it should)
Putting togheter point 1 and point 2, now you know why I said that.
Now you have also a trick to use well copper chloride and how to recover copper from it.
I hope i was helpuf to everybody.
butcher said:I do have good luck when I make nitric acid, I make it with many different methods and different strengths, I also like use my byproducts in several reaction's or other processes.
If I am just making nitric acid, one of the things I like using my sulfate salts for is a batch of pretty green crystals of ferrous sulfate, (this works best when using bisulfate salts from when you make the stronger nitric) , I use the ferrous sulfate (copperas) crystals to test for gold in solution or to precipitate gold from solution.
ZZZ, I like how you are also working (and thinking) to use your byproducts when you work, that is a good idea, and a smart thing to do. I noted some things below from what I understood in your the post above, that I believe would not work well, if I am understanding what you were saying in that post.
zzz said:Recovery the nitrate salt for make distillation: obviusly the nitric used to make aqua regia is irrecoverable, but if you used that for dissolve silver for inquartation (silver will passivate in the chloride solution)
Recovery sulfuric acid procedure from everyother sulfuric salt different from copper sulfate (what everyone wants to know): in this distillation example we have as product K2SO4.
Take it and make a satured solution in water (is a little bit difficult to dissolve once is cristallized, use hot boiling water to do that)...
now all you can do is to add Copper Chloride (in satured solution or in powder as you prefer -> so keep copper chloride) and you will have a white precipitation of Potassium Chloride (CuCl2 + K2SO4 --> NO Reaction you just have a solution of potassium, chlorides,sulfates and copper ions floating around in solution nothing here is insoluble so there is no reaction)
zzz said:butcher said:I do have good luck when I make nitric acid, I make it with many different methods and different strengths, I also like use my byproducts in several reaction's or other processes.
If I am just making nitric acid, one of the things I like using my sulfate salts for is a batch of pretty green crystals of ferrous sulfate, (this works best when using bisulfate salts from when you make the stronger nitric) , I use the ferrous sulfate (copperas) crystals to test for gold in solution or to precipitate gold from solution.
ZZZ, I like how you are also working (and thinking) to use your byproducts when you work, that is a good idea, and a smart thing to do. I noted some things below from what I understood in your the post above, that I believe would not work well, if I am understanding what you were saying in that post.
zzz said:Recovery the nitrate salt for make distillation: obviusly the nitric used to make aqua regia is irrecoverable, but if you used that for dissolve silver for inquartation (silver will passivate in the chloride solution)
Recovery sulfuric acid procedure from everyother sulfuric salt different from copper sulfate (what everyone wants to know): in this distillation example we have as product K2SO4.
Take it and make a satured solution in water (is a little bit difficult to dissolve once is cristallized, use hot boiling water to do that)...
now all you can do is to add Copper Chloride (in satured solution or in powder as you prefer -> so keep copper chloride) and you will have a white precipitation of Potassium Chloride (CuCl2 + K2SO4 --> NO Reaction you just have a solution of potassium, chlorides,sulfates and copper ions floating around in solution nothing here is insoluble so there is no reaction)
In the first example the subject was nitric acid.
In the second = maybe it will form also a little bit of uranium in addition to what you said.
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