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Author: Subject: Preparation of elemental phosphorus
WGTR
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[*] posted on 21-3-2017 at 08:37


Can't access the references page of this book, but here's some info for you. You'll likely have to use an excess of carbon, with carbon monoxide as a product instead of carbon dioxide.

Also, in coal or charcoal there's going to be some hydrogen in there, which likely means phosphine production.

P_1.jpg - 50kB
P_2.jpg - 38kB P_3.jpg - 33kB




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clearly_not_atara
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[*] posted on 22-3-2017 at 13:13


A eutectic of tin and zinc phosphates forms a glass with softening temperature approximately 440 C. These are much cheaper than barium or silver as was discussed before. However there is still the unfortunate possibility that the melt will react with Pyrex :p

http://repository.kulib.kyoto-u.ac.jp/dspace/bitstream/2433/...

As WGTR notes, you want to use plenty of carbon. CO is the waste product.

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BluePlanet1
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[*] posted on 23-3-2017 at 20:18


Thanks everyone for the responses. I doubled the weight of carbon but still got a few small issues to figure out.

Like packing the reagant into the retort. I have to "drop pack" it in, then turn it sideways and it still spills out too close to the neck.
Although I could just use less powder I'm trying to pack it as much as possible. So there's less air in the retort and also to test
how easy it is to clean out large loads.

What I'm doing is lightly plugging the retort with tissue before screwing the distiller on.

My hope is that the heat will burn out the tissue to flakes BEFORE CO gas starts spewing out.

Otherwise if pressure builds up too quick it could be dangerous.

So right now I need to run a few dry fires just to time how lightly I need to pack the tissue so the seal breaks before the reaction begins.

It's a small detail but I need to get this right so hopefully by the weekend I"ll be ready. :-)

[Edited on 24-3-2017 by BluePlanet1]
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[*] posted on 26-3-2017 at 23:37


Interesting. I hope your phosphorus synthesis works out.

This may sound like a bit of an odd request, but if you happen to have some tin and iodine handy, I'm deadly curious to see what would happen if the phosphorus stream were condensed in the presence of SnI2. It might have to be done under anhydrous condition or in a hot solvent to prevent disproportionation (SnI2 >> Sn + SnI4), but under the right conditions, condensing phosphorus vapor in the presence of SnI2 produces black phosphorus -- and it would be nothing short of incredible if this could be done with a freshly synthesized stream of phosphorus. If you do produce black phosphorus, it would be worth tens of dollars per gram, AFAIK.

A bit of a crazy idea -- no need to try it, right? :p
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