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Author: Subject: Is it possible to synthesise Pd/C from home?
gorgeousgeorge
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[*] posted on 1-3-2019 at 01:08
Is it possible to synthesise Pd/C from home?


I'm aware given the right requirements anything is possible, but I'm just curious as to hot it can be done?
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[*] posted on 1-3-2019 at 01:46


Here's a very recent youtube video on preparing Pd/C. YouTube isn't always the best source of information, but it's a quick answer to the question. If you want to do it yourself, it wouldn't do any harm to read around.

https://www.youtube.com/watch?v=kspZ_w8YIR0




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Loptr
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[*] posted on 1-3-2019 at 11:00


I plan to give it a try soon, too. I plan to dissolve a palladium ingot in nitric acid, and then reduce it with a formaldehyde solution to palladium(0) in the presence of activated carbon.

You will know when it's done because the red color of palladium ion will be gone.




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zed
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[*] posted on 1-3-2019 at 15:27


Yes, you could do that.

Still, reduction via NaBH4 probably produces a more active catalyst.
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Loptr
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[*] posted on 3-3-2019 at 07:42


Quote: Originally posted by zed  
Yes, you could do that.

Still, reduction via NaBH4 probably produces a more active catalyst.


Yes, you do keep recommending using NaBH4 for catalyst preparation. I just think it's weird to use it when it's more difficult to get than formaldehyde.




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[*] posted on 3-3-2019 at 08:22


http://www.orgsyn.org/Content/pdfs/procedures/CV3P0685.pdf

Formaldehyde reduction produces a product without adsorbed hydrogen and is less likely to catch on fire. That's a substantial benefit, aside from the difficulty of procuring NaBH4.

Carbon source is also important. I'll see if I can find the paper again, but the type of carbon had a dramatic effect on catalyst activity. IIRC, coconut carbon was actually the worst. It has very fine pores and a lot of the palladium was inaccessible to substrate.
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[*] posted on 3-3-2019 at 11:13


Maybe my substrate and beshitted hands would do better with this Pd, Pt, or Rh. Maybe one already has some for other uses for BH4. One would think that amateurs not equipped with high pressure tanks and a shaking Parr need all the help they can get. One can of course have good reasons for wanting a less active catalyst, but making the catalyst only to dry and safely store it sounds strange.

It's been available online from various US sources for as long as I've been a member here. Maybe not as cheaply as we'd like, unless from China by the bucket.

Of course the support can be omitted for a less active catalyst. I'm not too worried about fires from "Powdered sodium borohydride (0.19 g, 5 mmol) is added portionwise at room temperature over a period of 5-10 minutes to a stirred suspension of 0.443 g (2.5 mmol) of powdered palladium chloride in 40 ml of absolute methanol. Stirring is continued until the evolution of hydrogen has ceased (about 20 minutes). The solvent is decanted from the black settled catalyst which is washed twice or three times with a solvent to be used in hydrogenations."

[Edited on 4-3-2019 by S.C. Wack]




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zed
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[*] posted on 3-3-2019 at 14:30


Why would I suggest catalyst preparation via Borohydride reduction, vs Formaldehyde?

Possibly because I consider it a much, much, much, better method.

And, as Dr. Wack pointed out.... Make a catalyst to dry and store? Why?

I suppose there might be reasons to do such a thing.

But, in my corner of the Universe, Pt, Pd type-catalysts, are primarily used for hydrogenations.

Make 'em fresh, on the spot, just before use. Otherwise, performance may be lacking.
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Dan Vizine
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[*] posted on 7-3-2019 at 11:43


Quote: Originally posted by Loptr  
Quote: Originally posted by zed  
Yes, you could do that.

Still, reduction via NaBH4 probably produces a more active catalyst.


Yes, you do keep recommending using NaBH4 for catalyst preparation. I just think it's weird to use it when it's more difficult to get than formaldehyde.


How is he supposed to know what you have available? It was a good suggestion.

At least he can see where you are and can make a reasonable guess at what you might be able to access.

Most users hide their whereabouts like they think it needs to be a national secret. Often, you can't even make good suggestions for finding chemicals to them because they live in Narnia or Asgard. I've used my real name and town for a long time. Pfffft. All it's brought me is business opportunities. And anyway, do you think a phony username and unknown location will stop law enforcement if they deem you interesting enough to want to find? I don't know who else people would try to conceal their identities from.

And he's right, by the way. Borohydride gives a more active catalyst.



[Edited on 3/7/2019 by Dan Vizine]





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[*] posted on 7-3-2019 at 14:11


What about ascorbate? Does that make a good catalyst?



[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 7-3-2019 at 19:50


Ascorbic Acid?

Frankly, I have no idea. If it were shown to produce a decent catalyst, I would probably prefer it over Formaldehyde.

Cheap, easy to get, safe to work with.

I've been around formaldehyde some, and I find it nasty. Though some of the nasty, was surely emanating from the corpses I was dissecting. Can't really dissect inside of a fume hood, and some of my colleagues developed lingering health problems, associated with formaldehyde exposure.
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[*] posted on 8-3-2019 at 11:48


Quote: Originally posted by Dan Vizine  
Quote: Originally posted by Loptr  
Quote: Originally posted by zed  
Yes, you could do that.

Still, reduction via NaBH4 probably produces a more active catalyst.


Yes, you do keep recommending using NaBH4 for catalyst preparation. I just think it's weird to use it when it's more difficult to get than formaldehyde.


How is he supposed to know what you have available? It was a good suggestion.

At least he can see where you are and can make a reasonable guess at what you might be able to access.

Most users hide their whereabouts like they think it needs to be a national secret. Often, you can't even make good suggestions for finding chemicals to them because they live in Narnia or Asgard. I've used my real name and town for a long time. Pfffft. All it's brought me is business opportunities. And anyway, do you think a phony username and unknown location will stop law enforcement if they deem you interesting enough to want to find? I don't know who else people would try to conceal their identities from.

And he's right, by the way. Borohydride gives a more active catalyst.



[Edited on 3/7/2019 by Dan Vizine]


Not sure why you chose to jump on what I said (and the off topic detour into using your real name is just strange), but even if access to NaBH4 was easier, and more commonly available, formaldehyde would still be cheaper, but then again it really depends on your intended use. No silver bullets, one size fits all problems.

Now, with all that said, the cost of NaBH4 might not even be an issue due to the amount of Pd you would have on hand. I think if you have NaBH4, then use it. Fine by me, either way. If were were talking about large amounts of Pd, then you likely arent an amateur, and these constraints no longer apply.

I like the idea of a more active catalyst. Experimentation will determine if its effective for your substrate




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[*] posted on 9-3-2019 at 12:43


Update: the palladium is on its way!

:D




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[*] posted on 14-3-2019 at 17:35


I've made Pd/C, Pt/C, Ra-Ni and Nickel boride catalysts several times on my own.
And to answer your question - yes, it's possible and not even that hard. Actually it's easier than making good Ra-Ni from Ni/Al alloy. The most important key ingredient imho is to use BEST active charcoal for Pd/C.
But if it's possible I would prefer nickel boride over all others, as it's much less pyrophoric than Pd/C, Pt/C and Ra-Ni but yields for most reactions are almost the same.
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