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Old 05-21-2010, 01:01 PM
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Default Phosphoryl chloride...

Or Phosphorus oxychloride, POCl3 whatever you want to call it. it is accually quite easy to make at home with materials you can get down the street at the pool store. glassware most of us have if you are indepth with the feild of organic synthesis, or you can get it cheap on ebay... so here it goes:

There are 2 choices for your chlorine production, one is wet and the other is so wet it can hurt your yeild if not dried well. (2ft section of PVC filled with anhydrous MgSO4 works good). The first which is prefrable uses Trichloroisocyanuric acid (TCCA) tablets (or powder) which you can find at a pool store, it is used as a chlorinating agent. The other uses household bleach (remember its only 5% the other 95% is water). Both use HCl to strip the chlorine gas off the other moleclues. I prefer the TCCA as it generates much more chlorine than the bleach/HCl method and it is much dryer. The next draw back is that you will not be using the chlorine as it is generated, it must be premade and stored so your Cl2 generation vessle must be able to withstand at least 3-5 bar (40-70 psi) and safley store it for some time. A heavy walled 1000ml round bottom flask (with threaded necks) will hold that pressure easely the trick is getting the HCl into the flask either through a septum under one of the caps or squirting it in there and closing it quickly. My setup uses the said round bottom flask with three threaded necks one has the septum under a cap with a small hole drilled in it, the central neck has a pressure guage connected to it through a gland cap and tha last neck has a peice of tubing (also through a gland cap) leading to the PVC drying tube equiped with a valve at the other end. therefore when i introduce the HCL the pressure builds in the flask and the drying tube so the Cl2 gas is instantly at my disposal when i need it with out having to bleed the lines. The next step is to charge your rxn flask with dry RP powder, it can be safley baked at 200*F in your oven for a few minutes to dry it out. Use any ammount you can scrounge up as it goes a long way to have more than you expect to need (yields most often are not 100%). Just dump it in your three neck rxn flask dosent have to be a huge 5000ml or more but at least 500ml. after the rp is in the flask lead the Cl2/helium line through one stopper (use cork POCl3 attacks rubber stoppers) the center one is equiped with a glass stir bar that reaches the bottom with atleast 5cm to spare, the end in the flask has had a short section of glass rod melted to it crossways. The last neck has a hose leading out a window or to a hood if you have one. The flask is now charged with helium, not helium for baloons, that stuff is only about 35% helium and the rest air. get a small cilinder from a welding store, nitrogen will work in a pinch but you want a light gas. If you were to use argon it would blanket the RP and prevent the Cl2 from getting to it. Now that your flask in inerted slowly (REALY SLOWWWW...) turn on the supply of Cl2. The trick here is to let the chlorine 'trickle' in in small ammounts (PPH ammounts). If you put too much in the RXN goes exothermic and will produce flame, possably an explosion if you have a large enough ammount of RP or melt through your flask creating a dangerous chemical fire. If you do it right you can feel the flask by the RP and it will be warm possably hot but not flaming. Gradualy the RP will start to look 'wet' as the phosphorus trichloride starts to form you may have to break up and stir the RP from time to time to get it all to react. Eventially you will have a puddle of PCl3 with some RP that did not react. Now you can turn up the chlorine a little bit and start stiring to react the rest. Once the liquid is as clear as it is gonna get flush the flask with helium again and insert a section of glass tube into the liquid. You now have to pass pure O2 through it for several hours 2 is enough with a heavy stream but it can get real hot. a small stream of bubbles in a heavely stirred mixture (toss your magnetic stir bar in now if you have one) over night will be perfect. Next in a dry room (turn on the dehumidifyer the night before) extract your POCl3 and transfer it to a smaller distillation flask. This will be a somewhat high temp fractional distillation so use a air condencer before your allihn or graham condencer or it could crack. The first fraction that should come over will start around 70*C (158*F) this is the unreacted PCl3 once that stops (probally around 85*C (185*F) continue with heating untill the next fraction comes over around 100*C an stops when the distillation flask is dry. Congratulations you just mad some very pure (in the area of 98%) phosphoryl chloride!!! Use it wisely, it will fume in moist air and react violently with water forming phosphoric and hydrochloric acid throwing it everywhere. You dont want to get it on you either as you are mostly water it can act as a superacid and eat through your skin like a batch of conc. boiling sulfuric acid...


POCl3 boiling point 105.8*C 222.4*F

PCl3 boiling point 76.1*C 168.8*F
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  #2  
Old 05-21-2010, 08:13 PM
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Default Re: Phosphoryl chloride...

Quote:
Originally Posted by director of sound View Post
Or Phosphorus oxychloride, POCl3 whatever you want to call it. it is accually quite easy to make at home with materials you can get down the street at the pool store. glassware most of us have if you are indepth with the feild of organic synthesis, or you can get it cheap on ebay... so here it goes:

There are 2 choices for your chlorine production, one is wet and the other is so wet it can hurt your yeild if not dried well. (2ft section of PVC filled with anhydrous MgSO4 works good). The first which is prefrable uses Trichloroisocyanuric acid (TCCA) tablets (or powder) which you can find at a pool store, it is used as a chlorinating agent. The other uses household bleach (remember its only 5% the other 95% is water). Both use HCl to strip the chlorine gas off the other moleclues. I prefer the TCCA as it generates much more chlorine than the bleach/HCl method and it is much dryer. The next draw back is that you will not be using the chlorine as it is generated, it must be premade and stored so your Cl2 generation vessle must be able to withstand at least 3-5 bar (40-70 psi) and safley store it for some time. A heavy walled 1000ml round bottom flask (with threaded necks) will hold that pressure easely the trick is getting the HCl into the flask either through a septum under one of the caps or squirting it in there and closing it quickly. My setup uses the said round bottom flask with three threaded necks one has the septum under a cap with a small hole drilled in it, the central neck has a pressure guage connected to it through a gland cap and tha last neck has a peice of tubing (also through a gland cap) leading to the PVC drying tube equiped with a valve at the other end. therefore when i introduce the HCL the pressure builds in the flask and the drying tube so the Cl2 gas is instantly at my disposal when i need it with out having to bleed the lines. The next step is to charge your rxn flask with dry RP powder, it can be safley baked at 200*F in your oven for a few minutes to dry it out. Use any ammount you can scrounge up as it goes a long way to have more than you expect to need (yields most often are not 100%). Just dump it in your three neck rxn flask dosent have to be a huge 5000ml or more but at least 500ml. after the rp is in the flask lead the Cl2/helium line through one stopper (use cork POCl3 attacks rubber stoppers) the center one is equiped with a glass stir bar that reaches the bottom with atleast 5cm to spare, the end in the flask has had a short section of glass rod melted to it crossways. The last neck has a hose leading out a window or to a hood if you have one. The flask is now charged with helium, not helium for baloons, that stuff is only about 35% helium and the rest air. get a small cilinder from a welding store, nitrogen will work in a pinch but you want a light gas. If you were to use argon it would blanket the RP and prevent the Cl2 from getting to it. Now that your flask in inerted slowly (REALY SLOWWWW...) turn on the supply of Cl2. The trick here is to let the chlorine 'trickle' in in small ammounts (PPH ammounts). If you put too much in the RXN goes exothermic and will produce flame, possably an explosion if you have a large enough ammount of RP or melt through your flask creating a dangerous chemical fire. If you do it right you can feel the flask by the RP and it will be warm possably hot but not flaming. Gradualy the RP will start to look 'wet' as the phosphorus trichloride starts to form you may have to break up and stir the RP from time to time to get it all to react. Eventially you will have a puddle of PCl3 with some RP that did not react. Now you can turn up the chlorine a little bit and start stiring to react the rest. Once the liquid is as clear as it is gonna get flush the flask with helium again and insert a section of glass tube into the liquid. You now have to pass pure O2 through it for several hours 2 is enough with a heavy stream but it can get real hot. a small stream of bubbles in a heavely stirred mixture (toss your magnetic stir bar in now if you have one) over night will be perfect. Next in a dry room (turn on the dehumidifyer the night before) extract your POCl3 and transfer it to a smaller distillation flask. This will be a somewhat high temp fractional distillation so use a air condencer before your allihn or graham condencer or it could crack. The first fraction that should come over will start around 70*C (158*F) this is the unreacted PCl3 once that stops (probally around 85*C (185*F) continue with heating untill the next fraction comes over around 100*C an stops when the distillation flask is dry. Congratulations you just mad some very pure (in the area of 98%) phosphoryl chloride!!! Use it wisely, it will fume in moist air and react violently with water forming phosphoric and hydrochloric acid throwing it everywhere. You dont want to get it on you either as you are mostly water it can act as a superacid and eat through your skin like a batch of conc. boiling sulfuric acid...


POCl3 boiling point 105.8*C 222.4*F

PCl3 boiling point 76.1*C 168.8*F
Well, on the one hand, yes, the equipment and reagents can be put together quite easily, but on the other, I can see multiple life threatening possibilities. So be careful. But you seem to understand the risks, and I wont question your skills, so good luck.

PS: I like how you came out of nowhere, and started posting interesting stuff immediately.
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Last edited by BungHole; 05-21-2010 at 08:48 PM.
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Old 05-22-2010, 07:04 AM
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Default Re: Phosphoryl chloride...

Well, shit... my unnatural terror that high-pressure prolonged chlorine reflux would be involved just went way down...

Sounds easy. Deadly, but easy.
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Old 05-30-2010, 09:26 PM
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Default Re: Phosphoryl chloride...

This may come of use to anyone looking to store pressurized chlorine gas, it's from the Cole-Parmer chemical compatibility database:

Code:
Material                      Compatibility
304 stainless steel           A-Excellent
316 stainless steel           B-Good
ABS plastic                   N/A
Acetal (Delrinr)              D-Severe Effect
Aluminum                      C-Fair
Brass                         D-Severe Effect
Bronze                        B-Good
Buna N (Nitrile)              B-Good
Carbon graphite               A-Excellent
Carbon Steel                  B-Good
Carpenter 20                  A-Excellent
Cast iron                     D-Severe Effect
Ceramic Al203                 N/A
Ceramic magnet                N/A
ChemRaz (FFKM)                B-Good
Copper                        A-Excellent
CPVC                          D-Severe Effect
EPDM                          A-Excellent
Epoxy                         D-Severe Effect
Fluorocarbon (FKM)            A-Excellent
Hastelloy-Cr                  A-Excellent
Hypalonr                      D-Severe Effect
Hytrelr                       D-Severe Effect
Kalrez                        A-Excellent
Kel-Fr                        D-Severe Effect
LDPE                          D-Severe Effect
Natural rubber                D-Severe Effect
Neoprene                      C-Fair
NORYLr                        B-Good
Nylon                         D-Severe Effect
Polycarbonate                 N/A
Polyetherether Ketone (PEEK)  A-Excellent
Polypropylene                 D-Severe Effect
Polyurethane                  D-Severe Effect
PPS (RytonŽ)                  D-Severe Effect
PTFE                          A-Excellent
PVC                           D-Severe Effect
PVDF (KynarŽ)                 A-Excellent
Silicone                      D-Severe Effect
Titanium                      D-Severe Effect
Tygonr                        A-Excellent
Vitonr                        A-Excellent

Explanation of Footnotes
1. Satisfactory to 72°F (22° C)
2. Satisfactory to 120°F (48° C)

Ratings -- Chemical Effect
A   = Excellent.
B   = Good -- Minor Effect, slight corrosion
      or discoloration.
C   = Fair -- Moderate Effect, not recommended
      for continuous use. Softening, loss of strength,
      swelling may occur.
D   = Severe Effect, not recommended for ANY use.
N/A = Information Not Available.
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Old 05-30-2010, 09:33 PM
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Default Re: Phosphoryl chloride...

lol OP I dunno where you came from but it is sooo good to hear it.
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Old 05-31-2010, 12:27 AM
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Default Re: Phosphoryl chloride...

i notice that list does not say anything about boro glass, i think that list is intended for long term storage under high pressure or even liquid chlorine storage. for all intensive purposes the chlorine for this experiment would only be stored for around 24hr at a pressure less than 100psi (far less as 25psi in a 1000ml flask is enough for 10g of phosphorus) even then if needed more HCL and TCCA solution could be injected through the septum. good info though, that is also why natural cork or PTFE stoppers are a must. the chlorine and the phosphoryl chloride will attack natural rubber and dissolve a stopper in a matter of hours. PTFE is practically uneffected and natural cork, mostly lignand and fibers will just bleach on the side exposed to the Cl2 gas, if it is wet there is a chance it could shrink and loose seal as the PCl3 and POCl3 are highly hygroscopic and will pull the moisture right out of the cork.
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Old 06-06-2010, 01:59 AM
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Lightbulb Re: Phosphoryl chloride...

i was looking at some other info and it looks like i may have found another easier and safer method. it is only in theory for now until i get the sodium metaphosphate ( sodium hexymetaphosphate (NaPO3)6 ) in. but it appears that one might be able to accomplish this maby as a reflux reduction in a high boiling non polar. all anhydrous of course. we all know chlorine gas is highly electrophilic and will tear apart most compounds. the chlorine is more electronegative than the -phosphate ion and will strip that off and bond with the sodium forming salt. then there is the free PO3 in solution that will insitu form PO5 and bond with the free Cl2 in the solution forming POCL3 and O2. it may have to be heated to a high temp and distill off the POCl3 as it forms or it will occur at room temp. i wont know untill i try it.


(NaPO3)6 + 12Cl2 >>> 6NaCl + 6POCl3 + 6O2




looks possible if everything is anhydrous. CL2 generated from HCL+ trichlorocyanuric acid dried with calcium chloride. the (NaPO3)6 baked before hand to dry it out a bit. as for a solvent anhydrous benzene seems like it would work if one is needed, the POCl3 is soluable in it and has a higher boiling point than benzene so the benzene can be distilled out, the metaphosphate and salt will percip out of the benzene and can be filtered to remove it. an alternative would be using xylene and distilling the phosphoryl chloride out of the xylene.

Last edited by director of sound; 06-06-2010 at 02:02 AM.
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Old 06-06-2010, 02:02 AM
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Old 06-13-2010, 10:12 AM
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Default Re: Phosphoryl chloride...

While the Cole-Parmer database says dry chlorine should never be used with brass, another source says it's fine as long as the chlorine gas is absolutely dry. Just make sure if you use any brass valves that the seal inside is PTFE or another chlorine safe polymer.

http://www.hghouston.com/coppers/brass73.htm
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Old 06-24-2010, 01:08 PM
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Default Re: Phosphoryl chloride...

WTF ?? this metod is better then my
3PCl3 + KClO3 ------> 3POCl3 + 3KCl

Just makes PCl3 from white phosphorus and chlorine (no pressure or other shit) and carefully added in small portions KClO3 to PCl3 be carefull reactin is violent then destill from oil bath and that's it ....
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Old 06-25-2010, 06:15 AM
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Default Re: Phosphoryl chloride...

On sciencemadness in the thread elemental phosphorus you have production white from red ... just heat a lot and condensate the vapour and put "destillate" in baker with water ... or you can simple buy it ... sometimes that's easiest way and cheaper , I know anything can be done but what about cost? that's important to ... to buy it's cheap
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Old 06-25-2010, 06:22 AM
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Default Re: Phosphoryl chloride...

And I am mud farmer ? what about making EASY PCl5 from RED phosphorus and chlorine in chloroform as solvent etc. and then dry it and react with P2O5 to make ONLY POCl3 .... even wikipiedia helps here: 6 PCl5 + P4O10 → 10 POCl3 , the chemist is interesing ONLY the EASIES WAY to get a chemical .... HARD is not for me , HARD id for very expensive and well paid chemistry business
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