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Topic: Pd(C) disposal  (Read 10091 times)

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Offline Honclbrif

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Pd(C) disposal
« on: March 23, 2012, 05:33:29 PM »
Hey Guys,

I've been trying to reduce a nitro group. SnCl2 and Fe have only provided sadly low yields so I'm considering hydrogenation with Pd(C) and H2. The conditions are pretty simple, I'm not worried about them (MeOH, 50°, H2 balloon). However, no one in my lab has used this reagent before, so my question is: how do I dispose of the spent catalyst without burning down the lab? I'll be using small quantities, only about 100 mg.

Thanks
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Offline discodermolide

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Re: Pd(C) disposal
« Reply #1 on: March 23, 2012, 08:06:08 PM »
Hey Guys,

I've been trying to reduce a nitro group. SnCl2 and Fe have only provided sadly low yields so I'm considering hydrogenation with Pd(C) and H2. The conditions are pretty simple, I'm not worried about them (MeOH, 50°, H2 balloon). However, no one in my lab has used this reagent before, so my question is: how do I dispose of the spent catalyst without burning down the lab? I'll be using small quantities, only about 100 mg.

Thanks

Put the catalyst residue  plus filter, filter aid in a properly labelled bottle and cover the solids with water. When it is full you can return it to the manufacturer for re-cycling.
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Offline asa029

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Re: Pd(C) disposal
« Reply #2 on: March 24, 2012, 05:04:54 AM »
I just filter it off and place both the filter paper and the spent catalyst in an empty container. I've never filled it with water, but maybe that would be safer:D

Offline discodermolide

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Re: Pd(C) disposal
« Reply #3 on: March 24, 2012, 06:12:03 AM »
I just filter it off and place both the filter paper and the spent catalyst in an empty container. I've never filled it with water, but maybe that would be safer:D

Water stops it from drying out and catching fire!
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Offline Dan

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Re: Pd(C) disposal
« Reply #4 on: March 24, 2012, 07:50:16 AM »
Make sure you degas the mixture before exposing it to air. Evacuate and charge with nitrogen or argon at least 3 times before you take the lid off. If there is still hydrogen on the Pd, it can catch fire during filtration. This is why I normally like to do these reaction in water and not a flammable solvent if possible.

Several years ago I set my glove on fire working with Pd black and not degassing properly. Luckily no injuries. 10% Pd/C is not as feisty, but don't take risks with it, I certainly do not any more.

If you degas properly, the Pd/C residues should be harmless - but always store them wet, as discodermolide has detailed already.
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Offline Honclbrif

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Re: Pd(C) disposal
« Reply #5 on: March 24, 2012, 10:35:24 AM »
Thoroughly degas and never allow the material to dry out. I shall do these things.

Thanks Guys
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