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Author: Subject: Preparation of elemental phosphorus
Duff
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[*] posted on 1-7-2020 at 09:50


Great news! A 2019 paper (attached) published in the International Journal of Materials and Metallurgical Engineering describes the process of producing phosphorus from the carbothermic reduction of phosphoric acid. This is strong evidence that the method I am trying can work.

Rather than heating the acid gradually in the tube as the Japanese researchers did, I am planning to pump the acid in with a peristaltic pump once the carbon is already hot. The procedure will be as follows:

1) Placing both ends of the peristaltic pump's tube into a beaker of phosphoric acid, purge the peristaltic line of all air by pumping the acid in a loop out and back into the beaker
2) Flush system (furnace, phosphorus collection flask, schlenk line, ...) with argon
3) While keeping peristaltic line and furnace connection tubing submerged in the acid, use tubing joiner to connect peristaltic line to furnace connection tubing (the tubing can be lifted out of the acid once the tubes are joined and a seal is made)

See the attached picture for a visual.

Attachment: Carbothermic-Reduction-of-Phosphoric-Acid-Extracted-from-Dephosphorization-Slags-to-Produce-Yellow-Phosphorus-.pdf (431kB)
This file has been downloaded 64 times peristaltic.jpg - 286kB

[Edited on 1-7-2020 by Duff]
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Cou
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[*] posted on 3-7-2020 at 10:53


I cant find any iron retorts online x( gonna have to learn metalworking at the makerspace, or buy a custom part.

Does anyone know where to buy a metal retort, or how I can make one from stuff you can get at home depot? Cant use glass for this.

[Edited on 7-4-2020 by Cou]




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metalresearcher
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[*] posted on 15-7-2020 at 11:30


I succeeded.

I heated 7g (NaPO3)6 + 3g Al + 2g silica sand in a steel tube retort with a copper tube leading into a jar with water. I heated it to 700 C, after 15 minutes I did not see anything, I removed the retort, the bum of the retort was 900 C (measured with my infrared pyrometer). Then I saw 'water' dripping from the retort tube, but it catched fire with a small bright yellow flame smoking with dense P2O5 smoke. So it were drops of liquid P4 which spilled. Fortunately the amounts were less than a gram and my fumehood is completely fire resistant and I was aware of the dangers of P4, but a WARNING applies !

When you distill P4, be prepared that P4 might spill and keep bare hands, clothes or anything AWAY and use leather gloves and a face shield and perform outdoors or in a well ventilated fire resistant fumehood !
My experiment went well, but when it goes wrong it goes BADLY wrong !
P4 on your skin results in nasty and painful burns !



[Edited on 2020-7-15 by metalresearcher]

P4-20200715.gif - 3.7MB
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garphield
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[*] posted on 2-8-2020 at 20:06


Not sure if this would work, and due to using metal phosphides it would be pretty dangerous even if it did, but would it be possible to reduce a phosphate salt with aluminium in a thermite-style reaction, then oxidize the aluminium phosphide in the slag to AlCl3 and PCl3/PCl5 via putting the ground-up slag in an inert solvent and bubbling chlorine gas through? If you need elemental phosphorus you could probably use zinc powder or something to reduce the phosphorus chlorides to zinc chloride + phosphorus. No idea if this would work tho.
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clearly_not_atara
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[*] posted on 2-8-2020 at 20:26


Quote: Originally posted by metalresearcher  
I succeeded.

I heated 7g (NaPO3)6 + 3g Al + 2g silica sand in a steel tube retort with a copper tube leading into a jar with water. I heated it to 700 C, after 15 minutes I did not see anything, I removed the retort, the bum of the retort was 900 C (measured with my infrared pyrometer). Then I saw 'water' dripping from the retort tube, but it catched fire with a small bright yellow flame smoking with dense P2O5 smoke. So it were drops of liquid P4 which spilled. Fortunately the amounts were less than a gram and my fumehood is completely fire resistant and I was aware of the dangers of P4, but a WARNING applies !

Very nice!

The success with silica makes me wonder if other acidic oxides might liberate P2O5 from NaPO3. V2O5 is the most acidic solid oxide I can think of that will withstand the high temps.




[Edited on 04-20-1969 by clearly_not_atara]
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