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Topic: POCl3  (Read 7407 times)

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Offline vk1115

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POCl3
« on: May 06, 2013, 08:42:11 AM »
I am facing a lot of problems with handling of phosphorus oxychloride. Problem with it is that it hydrolyses to form HCl and phosphoric acid fumes as soon as it comes in contact with water in any form. My usage is minimal and I must find the best possible solution to eliminate or atleast minimize fumes.

Anybody have ideas on a closed system transfer of this material from a 50kg Carbouy to a 3000L mixer. It must also be weighed accurately

Input is appreciated
Thanks

Offline curiouscat

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Re: POCl3
« Reply #1 on: May 06, 2013, 08:57:31 AM »
Where's the water coming from? Is the mixer dry and inerted? Or is it atmospheric water vapor.

Ideally your system would be dry and pre-purged with dry N2.

One way of charging would be by pressurising the Carbouy with a slight positive pressure of N2 (Warning: If Carbouy can take that pressure. Test first with a non-hazardous liquid)

Another way would be to use a slight vacuum to suck it out.

Offline vk1115

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Re: POCl3
« Reply #2 on: May 06, 2013, 10:00:30 AM »
First of all thank you for the prompt reply.

My concern is atmospheric water vapor. Vacuum may not work since the fumes are extremely corrosive (acidic) in nature.

Offline curiouscat

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Re: POCl3
« Reply #3 on: May 06, 2013, 10:05:23 AM »
My concern is atmospheric water vapor. Vacuum may not work since the fumes are extremely corrosive (acidic) in nature.

I don't get the connection. You don't have to have a vacuum pump running while the operation is on. Just create a vacuum in a tank and use that to suck it into the tank. Then charge. Perhaps under positive pressure.

Offline cobrasniper555

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Re: POCl3
« Reply #4 on: May 09, 2013, 04:45:21 AM »
I am no where near qualified to speculate on this entry, but I am going to try. If there is reduced pressure (to an extent), water vapor may stay water vapor. And if the whole equipment is on the same pressure, then you could have a desiccant tank with dried NaOH (or equivalent), before the mixer. Correct? As if you're processing the gases before the actual operation?

I'm sorry, but I am just starting my college career this Fall, but I have A-L-W-A-Y-S been into chemistry and have a rather immaculate setup here at my house to be doing such experiments. And maybe that's what you need to do. An experiment. Do you have a place and the proper equipment?

-Cobra

Offline DrCMS

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Re: POCl3
« Reply #5 on: May 09, 2013, 04:54:31 AM »
Yes issolated vacuum charging with the full carbouy on scales to weigh by difference would be the way i'd do it.

Offline curiouscat

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Re: POCl3
« Reply #6 on: May 09, 2013, 08:40:31 AM »
Yes issolated vacuum charging with the full carbouy on scales to weigh by difference would be the way i'd do it.

Once your reaction is done you may want to break the vacuum using N2 instead of venting to air.

That'll preserve your dry conditions.

Offline Corribus

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Re: POCl3
« Reply #7 on: May 09, 2013, 02:16:50 PM »
I always have stored/handled this material (and its brominated cousin) strictly in a glove box; and transfered to sealed, purged glassware if necessary to bring to the bench, usually to use on a Schlenk apparatus.
What men are poets who can speak of Jupiter if he were like a man, but if he is an immense spinning sphere of methane and ammonia must be silent?  - Richard P. Feynman

Offline DrCMS

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Re: POCl3
« Reply #8 on: May 09, 2013, 05:12:13 PM »
I always have stored/handled this material (and its brominated cousin) strictly in a glove box; and transfered to sealed, purged glassware if necessary to bring to the bench, usually to use on a Schlenk apparatus.

Fair enough but how does this help the OP with their use of 50kg going into a 3000L vessel?

Offline cobrasniper555

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Re: POCl3
« Reply #9 on: May 09, 2013, 07:58:42 PM »
Yes issolated vacuum charging with the full carbouy on scales to weigh by difference would be the way i'd do it.

Once your reaction is done you may want to break the vacuum using N2 instead of venting to air.

That'll preserve your dry conditions.

I agree with the final step. A N2 gas purge maybe advised.

Offline Corribus

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Re: POCl3
« Reply #10 on: May 09, 2013, 09:19:28 PM »
Fair enough but how does this help the OP with their use of 50kg going into a 3000L vessel?
Er... a very big glove box?

I guess I should have read the opening post more carefully.   :-[
What men are poets who can speak of Jupiter if he were like a man, but if he is an immense spinning sphere of methane and ammonia must be silent?  - Richard P. Feynman

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