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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 102 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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Triflic Acid
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[*] posted on 5-11-2020 at 18:04


Just a thought, but reacting sodium hypophosphite with an oxidizer should make elemental phosphorus. Its a byproduct in electroless nickel plating: https://en.wikipedia.org/wiki/Electroless_nickel-phosphorus_...
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Bedlasky
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[*] posted on 5-11-2020 at 18:14


If you mix hypophosphite with oxidizer you get phosphite or phosphate.

Phosphorus which forms in nickel plating is in form nickel phosphorus alloy, it doesn't form as a pure element.




If you are interested in aqueous inorganic chemistry look at https://colourchem.wordpress.com/main-page/

"An old friend once told me something that gave me great comfort. Something he had read. He said that Mozart, Beethoven and Chopin never died. They simply became music." Dr. Robert Ford, Westworld
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[*] posted on 5-11-2020 at 19:09


Then dissolve away the nickel with an acid, that might work
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B(a)P
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[*] posted on 5-11-2020 at 19:34


This is an interesting concept.
Not that many will have the ability to perform electrolysis on a liquid at 850 C.....
https://pubs.acs.org/doi/pdf/10.1021/acssuschemeng.0c04796

Attachment: yang2020.pdf (3.8MB)
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[*] posted on 5-11-2020 at 19:44


I decided to just buy red phosphorus from chemcraft.su. I need it for regioselective bromination of alcohols. I don't do any illegal drugs so I'm not worried about the possibility of police coming knocking. If they search my house expecting to find empty Sudafed boxes, they're wasting their time.

My life will not be complete until I can regiospecifically brominate alcohols. Civil asset forfeiture a risk I'm willing to take.

[Edited on 11-6-2020 by Cou]




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[*] posted on 6-11-2020 at 07:37


Quote: Originally posted by Cou  
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]


I accidentally found these examples:
https://indonesian.alibaba.com/product-detail/high-recovery-...
https://indonesian.alibaba.com/product-detail/mercury-retort...

It seams that this type of retorts is used for distilling of mercury from gold amalgam (so, search "mercury retort". I don't know whether this type of retorts is suitable for producing of white phosphorus because they have a very narrow pipe.

[Edited on 6-11-2020 by teodor]

[Edited on 6-11-2020 by teodor]
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[*] posted on 11-11-2020 at 22:14


Thought I'd give an update. The amount of time I've been able to spend on chemistry has been limited over that past few months, but hopefully I can spend more time on phosphorus production in the coming months. Right now I'm thinking hard about how I can effective do "unit testing" of various parts of my setup, e.g. can the o-rings on my flange valves withstand the required pressure and temperature, can my condensers sufficiently cool the gases exiting the furnace, dealing with possible phosphine formation, etc.

Another problem I've been wrestling with is how to place the activated carbon in the furnace's quartz tube in a way that ensures any phosphorus produced will not condense before it leaves the tube. The tube is 30 cm long, but the heating zone in the furnace is 10 cm long. I may have to place the tube so that the exit flange is closer to the heating zone.

There might be an easy solution to the problem of phosphine formation. The attached document claims that
Quote:

Sodium hypochlorite in aqueous solutions reacts practically instantaneously with phosphine so that such solutions are particularly suitable for removing traces of phosphine from a gas stream

So passing the gases through a solution of sodium hypochlorite at some point might be an idea.

I want to minimize the amount of combustible or toxic gas that enters my pump, so if I can remove phosphine from the gas stream before it gets there that would be fantastic.

There are so many hypotheticals, I think at some point I just have to admit that I can't account for everything, and just go ahead and try to do it, if something doesn't work out I can try to understand why and try again. I just haven't had time to work on this for a while.

Attachment: 2494-The-Chemistry-of-Phosphine807f.pdf (857kB)
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MidLifeChemist
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[*] posted on 13-11-2020 at 09:22


Quote: Originally posted by Duff  
but hopefully I can spend more time on phosphorus production in the coming months.



Have you produced any phosphorus yet?
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