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Thermal
2008-12-19, 20:09
All I could find was preparation of Pd negro was from Pd compounds, but this question is quite elementary so i apologize.

What is the best way to prepare a small chunks (0.5g) of Pd to serve as catalyst? grind them down?
Or does it really need to bond n unbond with another molecule ?

And while I am at it, is $38 a gram for pure Pd decent price? Or would it be better to get PdCl2 @ $21 per gram ? I know how to calculate mol. weight but I was wondering which is "better" in terms of simplicity of preparation.

Wow I feel stupid for askin this shit.

Approx. how long does it take to say, hydrogenate a gram of veg oil with 0.5g of catalyst (Pd) under certain pressure/h2 supply ? I know it is dependant on the method and apparatus efficiency but if any of you can give me an example to get an idea I woud be grateful.

I am not doing anything illegal, just studying hydrogenation reactions. FYI.

nshanin
2008-12-19, 20:30
I am not doing anything illegal

Well then forget it! :mad: You'll find no help here!

Thermal
2008-12-19, 20:40
Well then forget it! :mad: You'll find no help here!

:(

I will not be doing anything illegal, but my friend Drown might and I will be sure to have Drown take pics to post them here. Actually Drown asked me to find that out about Pd in exchange for synth pics so lets help Drown, he is a cool guy and he will send me pics along with info on yield n such so it can be posted here :) Thanks

nshanin
2008-12-19, 20:54
http://www3.interscience.wiley.com/journal/109076042/abstract?CRETRY=1&SRETRY=0

http://aiche.confex.com/aiche/2008/techprogram/P122801.HTM

http://www.springerlink.com/content/g0074110h2j05584/

Those are what I saw on the first 2 pages in google with "Pd hydrogenation vegetable oil". Maybe google scholar? :confused:

Thermal
2008-12-19, 22:32
http://www3.interscience.wiley.com/journal/109076042/abstract?CRETRY=1&SRETRY=0

http://aiche.confex.com/aiche/2008/techprogram/P122801.HTM

http://www.springerlink.com/content/g0074110h2j05584/

Those are what I saw on the first 2 pages in google with "Pd hydrogenation vegetable oil". Maybe google scholar? :confused:

Man did you even read my post? These links are unrelated to my questions, and I know how to use google. And i already did a basic research on these keywords.So not to be a dick, because I appreciate your effort, but if you dont know the answer already, giving me google search results for few keywords and links to unrelated articles will not make you look smarter, but will make me look dumb and lazy :) Please dont make me look like a lazy dumbass :(

And forget the veg oils for a second, because my question didn't ask for that, just for an example of how much time to give for a process with given amount of specific catalyst under certain pressure etc.

so let me rephrase:
- What is best way to make pure Pd into Pd black? or do I just need to grind it to powder?
- For the prices i stated above, which is cheaper/easier to utilize Pd or Pd black
- How to figure out how much time is needed to fully reduce a substance given specific quantity of catalyst, h2 pressure, temp., etc.

nshanin
2008-12-19, 23:39
Oh. :o Well then I have no idea. I would look for specific reactions in the literature and play around with values near that (if you have the capacity/resources). Hydrogenation time/pressure/temp varies by compound so you will always get a varaible answer.

TheWhiteMan000
2008-12-20, 04:22
pd itself is not a catylist, you need to make a mixture of pd and tin then dissolve the tin with a strong acid, not really something you can do your self

for most substances the temp will increase 1C for every IV level gained, you need to heat to about 330 f or 140 C then, if you're completely hydrogenating the easiest way to go is just keep the hydrogen on till the temp stops rising. you should only break the pressure with nitrogen under vaccume, (heat+hydrogen+o2=bad) plus o2 and heat will degrade the color of your product(if it is an oil)

TheWhiteMan000
2008-12-20, 04:28
ps the average catylist needed is .2% and use nickle, easier, cheaper, and easier to come by

Thermal
2008-12-20, 09:22
pd itself is not a catylist, you need to make a mixture of pd and tin
how would you go about mixing a chunk of pd with tin? melting them together?

then dissolve the tin with a strong acid, not really something you can do your self
are you kiddin me? is dissolving tin with a strong acid so much beyond synthesis of numerous nitrate esters, nitroaromatic or nitramine compounds? Do I REALLY need my dad's supervision?

My bad, i couldnt help it :)


for most substances the temp will increase 1C for every IV level gained, you need to heat to about 330 f or 140 C then, if you're completely hydrogenating the easiest way to go is just keep the hydrogen on till the temp stops rising. you should only break the pressure with nitrogen under vaccume, (heat+hydrogen+o2=bad) plus o2 and heat will degrade the color of your product(if it is an oil)

Thank you, this actually helps.

Von Bass
2008-12-20, 10:57
- What is best way to make pure Pd into Pd black? or do I just need to grind it to powder?
- For the prices i stated above, which is cheaper/easier to utilize Pd or Pd black

In general, I believe it is easier to go to Pd Black from PdCl rather than straight Pd. Don't quote me on that one, I've never tried it, but did some research into it a while ago, found a few peoples experiences, I think on the arcHive. There's also a member here who might well be doing this, but I'll leave that up to him/her/it if he/she/it wants to spill the proverbial beans.

For the prices, generally Pd black has more uses, can be used more easily and is in a ready-to-use format. It is though apparently pyrophoric, so inert atmospheres are your friend.

Thermal
2008-12-22, 19:31
In general, I believe it is easier to go to Pd Black from PdCl rather than straight Pd. Don't quote me on that one, I've never tried it, but did some research into it a while ago, found a few peoples experiences, I think on the arcHive. There's also a member here who might well be doing this, but I'll leave that up to him/her/it if he/she/it wants to spill the proverbial beans.


I came to the same conclusion when only ingo I found for making Pd black required PdCl. But OTOH maybe it is because turning Pd into Pd black is so elementary that there is no info on that ?


For the prices, generally Pd black has more uses,
I am not sure what you mean, I can not buy straight Pd black, only PdCl or pure Pd...