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Author: Subject: Nitrate salt sources
katyushaslab
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[*] posted on 19-1-2021 at 07:28


If you are in mainland Europe, I suggest looking up the "E number" for KNO3, and simply buying it as a food additive. A Polish company by the name "Browin" sells it by the 100g pouch, amongst others. Prices vary a bit.
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Fyndium
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[*] posted on 19-1-2021 at 13:04


Thanks, I can get otc KNO3 for 10€/kg from garden fertilizer by recrystallization.

The purpose of turning AN to KNO3 is more of procedural question.
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katyushaslab
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[*] posted on 19-1-2021 at 16:54


Ah, so I can maybe help with that: you can do the double displacement with KCl and NH4NO3 to yield KNO3 and NH4Cl. That's how I used to do it, before AN became hard to get after being replaced in cold packs by urea. I can try look for some old notes.

Now for cleaning the KNO3, a recryst would do the trick, but one avenue I never explored (that seems interesting) would be to sublime the NH4Cl off. It sublimes around 330*C, and KNO3 doesn't decompose below 500*C.

Unfortunately in my country nitrates as fertiliser is almost impossible without owning a farm, due to laws on explosive precursors we passed in the 1970's which banned a few things.
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Fyndium
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[*] posted on 21-1-2021 at 05:03


It would likely require huge amounts of energy to sublime it off, and also NH4Cl does not have sublimation but decomposition temperature, upon which NH3 and HCl evaporate, condensing upon cooling. These could interact with KNO3 at some level, and also, any remaining compound form NH4NO3 will cause issues upon heating. I wouldn't carry out a reaction by thermal decomposition that has AN as an input reagent, unless I could make sure it won't cause issues.

I've always considered these raw materials as bulk, which are usually in multi kg scale, so anything that works on test tube or mini scale is not so scalable at these more special methods. Purifying otc fertilizers for useful reagents tends to require plastic buckets as reactor size.
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Fyndium
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[*] posted on 19-3-2021 at 08:12


I finally had some time to test my long-standing solution of fertilizer extract liquid.

When CaCl2 was added, a significant amount of precipitate fell out. It appears that it contains soluble sulfates and phosphates, whatsoever.

My plan herefore would be to crash out all sulfates and phosphates with CaCl2, filter, and then concentrate the solution, until ammonium chloride starts to precipitate. The solution would be likely so concentrated on nitrates that it will freeze in the filter, so it is likely it has to be hot filtered. The calcium and ammonium nitrates will remain liquid for very long, as they form a solution of 4-10kg/L of water at 100C, and it should be possible to crash basically all ammonium chloride out while keeping the solution liquid at 100C. So the final extract should be mostly composed of ammonium and calcium nitrates. It would be possible to further reduce the ACl amount by dissolving it in ethanol, as ammonium chloride has 0.6% solubility, and ammonium nitrate has 3.6% solubility. If all calcium would be crashed out, ammonium sulfate would do the job, or if water soluble nitrate is needed, sodium carbonate will also do. The calcium sulfate or carbonare sludge is not impossible to filter, with suction it's slow, but filtering a few liters can be carried out in a couple of hours with passive vacuum.

Hence it would be viable to extract both useful quality ammonium chloride and a nitrate feed source for producing nitric acid. Calcium nitrate can be well mixed with any water soluble nitrate in quite high ratios and still be extractable from a reactor after the distillation, as NurdRage proved.

Any flaws? Any improvements?
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yobbo II
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[*] posted on 19-3-2021 at 10:36




The problem with the 'crashing out' is that most of these compounds do not 'crash out' as they are fairly soluble. Calcium Sulphate will 'crash out' as it is 'insoluble.

A patent that goes into detail on making KNO3 and Amm. Chloride is US 3,595,609
(attached). It gives a Janecke diagram of the reciprocal salt pair(s).
KNO3 and Amm. Nitrate form a solid solution so a recrystallization will always be necessary (imo).
We need a Janecke diagram expert dude on the board!

Yob

Attachment: US3595609_KNO3_FROM_AN.pdf (749kB)
This file has been downloaded 61 times

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Fyndium
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[*] posted on 19-3-2021 at 19:20


Thanks for the link, although the file doesn't work.

https://patents.google.com/patent/US3595609A/en

It's a basis for test. My liquor has something that instantly crashes out with added calcium chloride, and it's sulfate and phosphate salts are known low sol compounds. Adding KCl will also precipitate instantly something, possibly potassium sulfate.
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yobbo II
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[*] posted on 23-3-2021 at 15:52



Strange as it works for me ok.

Yob
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Fyndium
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[*] posted on 24-3-2021 at 02:12


Now it works. Strange as it is. :D
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