Chemgineer
Hazard to Others
Posts: 216
Registered: 25-5-2021
Member Is Offline
|
|
Nitric acid from calcium nitrate
I normally produce nitric acid from magnesium nitrate and sodium bisulfate dry distillation and it works great.
I have however allot of calcium nitrate I want to use but the Nurdrage procedure for the distillation of this with sodium bisulfate works great but
erodes chunks of glass from my flasks and breaks them!
Do you think I should be converting the calcium nitrate to another nitrate salt to avoid this or would a wet distillation of calcium nitrate and
sodium bisulfate be better.... with a fractional distillation of the nitric acid later?
|
|
|
Rainwater
National Hazard
Posts: 925
Registered: 22-12-2021
Member Is Offline
Mood: Loving every second
|
|
CaSO4 is a real pain in the !@@ to clean. I experienced glass etching with sodium metabisulfate and CaNO3
It was only noticeable after 3~4 runs
And again with potassium bisulfate(leftovers from making HNO3 via sulfuric acid & potassium nitrate)
I think its the little bit of water trapped in the salt that lets it eat glass if at any point a hydroxide forms.
"You can't do that" - challenge accepted
|
|
|
Chemgineer
Hazard to Others
Posts: 216
Registered: 25-5-2021
Member Is Offline
|
|
Quote: Originally posted by Rainwater  | CaSO4 is a real pain in the !@@ to clean. I experienced glass etching with sodium metabisulfate and CaNO3
It was only noticeable after 3~4 runs
And again with potassium bisulfate(leftovers from making HNO3 via sulfuric acid & potassium nitrate)
I think its the little bit of water trapped in the salt that lets it eat glass if at any point a hydroxide forms. |
Yes always 3-4 runs before it starts, making you think everything will be fine! Perhaps the first few runs allow some calcium sulfate to stick to the
glass and get a better adhesion on the later runs.
Hmm I wonder if it would help to alternate between magnesium nitrate anc calcium nitrate runs, would this help to clean the flasks?
|
|
|
Rainwater
National Hazard
Posts: 925
Registered: 22-12-2021
Member Is Offline
Mood: Loving every second
|
|
Not sure, a 20 minute boil in hot water usually breaks up and softens the larger chunks of plaster. My problem is getting the rbf absolutely clean. No
matter how many times i wash it, there is always a little caso4 still left in there. Washing with hot diluted H2SO4(~5%) does the trick.
"You can't do that" - challenge accepted
|
|
|
fx-991ex
Hazard to Self
Posts: 99
Registered: 20-5-2023
Member Is Offline
|
|
I may be wrong but i think calcium ion are known to attack glass.
|
|
|
Sir_Gawain
Hazard to Others
Posts: 437
Registered: 12-10-2022
Location: [REDACTED]
Member Is Offline
Mood: Stable
|
|
Do a double displacement with sodium carbonate.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
|
|
|
charley1957
Hazard to Others
Posts: 164
Registered: 18-2-2012
Location: Texas
Member Is Offline
Mood: Beginning to cool off
|
|
I have a container of steel BBs at the sink where i wash my glassware. Swirling/shaking them around in the flask works wonders to help break up
stuck-on stuff. Saves acid too.
You can’t claim you drank all day if you didn’t start early in the morning.
|
|
|
Rainwater
National Hazard
Posts: 925
Registered: 22-12-2021
Member Is Offline
Mood: Loving every second
|
|
Charley, you are a genuine genius. And its simple, love it
"You can't do that" - challenge accepted
|
|
|
Chemgineer
Hazard to Others
Posts: 216
Registered: 25-5-2021
Member Is Offline
|
|
Thanks, that is probably the best idea as long as calcium carbonate settles out of the solution nicely.
|
|
|
fx-991ex
Hazard to Self
Posts: 99
Registered: 20-5-2023
Member Is Offline
|
|
Yes it do and its very easy to filter too.
|
|
|
fx-991ex
Hazard to Self
Posts: 99
Registered: 20-5-2023
Member Is Offline
|
|
| Quote: Originally posted by charley1957 | | I have a container of steel BBs at the sink where i wash my glassware. Swirling/shaking them around in the flask works wonders to help break up
stuck-on stuff. Saves acid too. |
I do the same thing but i use coarse salt instead loll, i guess sand could work well too.
|
|
|
Chemgineer
Hazard to Others
Posts: 216
Registered: 25-5-2021
Member Is Offline
|
|
Does this sound reasonable volumes for double displacement of sodium nitrate from calcium nitrate using sodium carbonate?
120g Na2CO3 in 300ml water
185g Ca(NO3)2 (not anhydrous) in 100ml water
Should produce 190g of NaNO3 in 400ml of water once the calcium carbonate is filtered off.
Or should I add my 300ml solution of sodium carbonate directly to my calcium nitrate prills and heat and mix ending up with only 300ml volume with
less boiling down needed?
|
|
|
fx-991ex
Hazard to Self
Posts: 99
Registered: 20-5-2023
Member Is Offline
|
|
Make sure your Ca(NO3)2 are in fact Ca(NO3)2 and not CAN calcium amonium nitrate.
If its CAN then:
For 120g of Na2CO3 you should use 222g of CAN to get 192g of NaNO3, 103g CaCO3, 37g H2O, 10g (NH4)2CO3(will decompose upon heating to recrystallize).
If your Ca(NO3)2 is indeed pure then the ratio/weight are correct.
Just use as little water as possible.
Id avoid pouring the Na2CO3 sln into the Ca(NO3)2 prill, you may want to filter the Ca(NO3)2 sln before rxn.
|
|
|
Alkoholvergiftung
Hazard to Others
Posts: 180
Registered: 12-7-2018
Member Is Offline
|
|
The test for CAN should be easy. In Aceton 1l disolve 330g Calciumnitrate and only 1g ammoniumnitrate. Would be a seperation methode too.
[Edited on 15-6-2024 by Alkoholvergiftung]
|
|
|
Fulmen
International Hazard
Posts: 1720
Registered: 24-9-2005
Member Is Offline
Mood: Bored
|
|
The simplest test for CAN is to mix it with sodium hydroxide in solution. CAN will give off ammonia.
We're not banging rocks together here. We know how to put a man back together.
|
|
|
greenlight
National Hazard
Posts: 745
Registered: 3-11-2014
Member Is Offline
Mood: Energetic
|
|
You could also convert the calcium nitrate to potassium nitrate with potassium chloride if that's easy to find in your country. Potassium chloride
can be brought in large quantities in some places as water softener.
Then you have nitrate salt thats easier to dry and keep dry as it is not hygroscopic like sodium nitrate.
Distillation with concentrated sulfuric acid and done
Be good, otherwise be good at it
|
|
|
fx-991ex
Hazard to Self
Posts: 99
Registered: 20-5-2023
Member Is Offline
|
|
| Quote: Originally posted by greenlight | You could also convert the calcium nitrate to potassium nitrate with potassium chloride if that's easy to find in your country. Potassium chloride
can be brought in large quantities in some places as water softener.
Then you have nitrate salt thats easier to dry and keep dry as it is not hygroscopic like sodium nitrate.
Distillation with concentrated sulfuric acid and done |
It work but purity will be better with KOH, or he could just re-crystallize twice of course.
|
|
|
Chemgineer
Hazard to Others
Posts: 216
Registered: 25-5-2021
Member Is Offline
|
|
Yeh I produced some sodium nitrate as above but it's not convenient to use since it is so hygroscopic.
|
|
|
ManyInterests
National Hazard
Posts: 932
Registered: 19-5-2019
Member Is Offline
|
|
I actually do have one question about this. I have 15.5 calcium nitrate (meaning it has a small amount of ammonium nitrate in it as well) and knowing
that the calcium sulfate is a giant PAIN to get rid of, I did think about cleaning it from the potassium or sodium sulfates as well...
Since when I make nitric acid, whether I use sodium nitrate or potassium nitrate (further dried in the oven before hand in order to drive away any
water that it might have absorbed) getting rid of the sulfate cake after it cools is still an hours long process and I use a lot of sodium bicarbonate
or carbonate to get it clean and dissolved. Even though those sulfates are supposed to be water soluble they don't appear to be so, but just using a
basic solution to get them to dissolve is what is needed.
Am I doing something wrong here? Because the biggest issue I have with making nitric acid is the clean up afterward. I always wash all my gear and let
them air dry between runs, but it would be MUCH easier if I can get my flask cleaned up quicker.
The other issue is that the specific gravity of my nitric acid rarely seems to be in the WFNA ratio, but I am being told not to rely on that. So going
forward I will see if I can make PETN and RDX with the acid I make, but cleaning the flask more easily would be a great boon.
Any help?
|
|
|
Rainwater
National Hazard
Posts: 925
Registered: 22-12-2021
Member Is Offline
Mood: Loving every second
|
|
I find it much easier to perform a wet distillation and then use sulfuric acid to remove the water.
It is easy to clean so long as the byproducts are not heated until molten, and the sulfuric acid is recoverable. To the best of my knowledge, calcium
sulfate can not be easily cleaned.
If you could keep water out of the mix (baking reagents before use), you might be able to use a modified pressure cooker to make a dry distillation
appratus.
Aluminum would be a good choice.
Sodium sulfate's only really eat into aluminum in the presence of water, and nitric acid will simply passivate it.
It would be a disposable appratus but should survive many runs.
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 932
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: | | I find it much easier to perform a wet distillation and then use sulfuric acid to remove the water. |
I must agree with this. So far I have not done a redistillation, I usually distill as dry as possible and hope for the best. Sometimes I succeed, but
other times not so much. Nurdrage distills his nitric acid with 1:1 ratio of sulfuric acid, but I was told that an excess of even twice as much
sulfuric acid will be much better.
For me in order to make it worth it, I need to make several distillations of nitric acid before redistilling everything and collecting. I have a 2
liter boiling flask that I use mostly for this, and two runs will allow me to have around 450 to 500ml (if I am lucky) to redistill. Three runs would
requirement to use a 1 liter receiving flask.
The use of improvised distillation equipment is a no-go for me. I got dedicated stuff and I really don't want to waste any more money. Especially on
things like pressure cookers which can get pricey.
|
|
|
![[*]](images/xpblue/default_icon.gif){kind=icon}
