ryan81
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POCL3-Phosphorus Oxychloride
Any custom apparatuses that one could recommend for the primary synth.
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ryan81
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Why is this chemical so hard to create, I guess any chemical which reacts with 02 is.
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careysub
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That question is discussed in this thread:
http://www.sciencemadness.org/talk/viewthread.php?tid=50249
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ryan81
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Mr. Careysub,
I am very familiar with this, but cannot picture this part, nerveless re-create it. Can you advise. ). The reaction vessel is placed in an
air oven and connected to a bend leading through a Liebig condenser to a receiver flask
immersed in cold water. The outlet from the flask is vented through a CaCl2 protection
tube with a bubbler optionally attached for observation of reaction progress.
Diagram would be much appreciated
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byko3y
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Wiki has already described all the easy routes:
PCl5 + SO2 => POCl3 + SOCl2
PCl5 + RCOOH => POCl3 + RCOCl
3 PCl5 + 2 B(OH)3 → 3 POCl3 + B2O3 + 6 HCl
3 PCl3 + KClO3 → 3 POCl3 + KCl
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softbeard
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POCl3 does not react with O2 and is not sensitive to it. POCl3 does react with H2O and is easily
hydrolyzed by water vapor in the air. The reason POCl3 is air-sensitive is moisture, not oxygen.
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chemrox
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and hydrated POCl3 is known to detonate ;^)
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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zed
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"Wiki has already described all the easy routes:
PCl5 + SO2 => POCl3 + SOCl2
PCl5 + RCOOH => POCl3 + RCOCl
3 PCl5 + 2 B(OH)3 → 3 POCl3 + B2O3 + 6 HCl
3 PCl3 + KClO3 → 3 POCl3 + KCl"
If you can acquire the above precursors, you can probably acquire POCl3 itself.
Wiki also mentions production via Phosphorus Pentoxide. Unlike the other mentioned reagents, Phosphorus Pentoxide is more or less, available. At any
rate, its distribution is probably not as restricted as that of other precursors.
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Aqua-regia
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Other ways to get the stuff:
PCl3 + Cl2 ——> PCL5
3PCL5 + P2O5 ——> 5POCl3
just mix in right molar ratio, bubble in the mix chlorine till the solution will be constant yellow and distill
Ca3(PO4)2 + 4(NH)4H2PO4 ——> 3Ca(PO3)2 +6H2O + 4NH3
Ca(PO3)2 + 2C + 4Cl2 ——> 2POCl3 + CaCl2 + 2CO2
For this methode need electric tube furnace reactio goes 650 C degrees
reference: an old patent. I already tryed, its OK.
http://worldwide.espacenet.com/publicationDetails/originalDo...
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byko3y
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There's pretty much no way to the POCl3 directly except from phosphorus halides/oxides. Well, Aqua-regia actually described the only well-known
phosgen mediated direct synthesis of POCl3, however, the actual reaction is more complex and the equiation only superficially describes the process:
Ca(PO3)2 => Ca3(PO4)2 + P2O5
P2O5 + C => P2O3 + CO
CO + Cl2 => COCl2
P2O5 + COCl2 => POCl3 + CO2
P2O3 + Cl2 => something
and so on.
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chemrox
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All glass ware must be clean and dry. The round bottom distilling flask containing 21 g of finely powdered potassium chlorate is connected with a
condenser and receiver. From the dropping funnel slowly 69 g of phosphorus trichloride are added into the flask a little at a time. After each
addition of small amount of phosphorus trichloride, reaction takes place by a gentle ebullition. If reaction is slow slight warm may be applied. When
the reaction is complete, phosphorus oxychloride is distilled. Further purification is performed by re-distillation and collecting fraction boiling at
110° C.
Laboratory methods of inorganic chemistry by H. Biltz, 77h, 1928
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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