making Pd/C - Palladium on carbon

[BrownRiceSyrup]

From what i gather its just find some activated fine powder carbon, heat with 10% nitric acid solution for a few hours. Rinse. Dry. Add 5 or 10% by weight palladium into a beaker, dissolve with hcl/h202. Add to beaker with activated carbon and stir for a bit to let it soak. Then add formic acid or formaldehyde to reduce/precipitate onto the support. Rinse. done. Right?

any tips? suggestions? This sound right?

how much 10% pd/c is considered 'catalytic' when adding to a reaction? im assuming since its 7x better as a catalyst than copper, adding 1/5 or 1/7 of the molar equivilant of palladium of copper chloride that is often called for in clandestine chem would be a correct amount right...?

 

[OrgUnikum]

This will produce an inferior catalyst, if the writeup calls for 3% w/w Pd loaded catalyst you will have to use one with 30% loading to stand a chance to get comparable results.

Making active noble metal catalysts oneself is possible though, but its not trivial, so ideally one would buy the catalyst from DEGUSSA for example (they are the best), if you find somebody who can actually buy from them and sells to you. Special catalysts are available there like resistant against amine poisoning for reductive aminations which can be re-used 10 to 50 times.

 

[BrownRiceSyrup]

Well, i did it anyway. Definitely pyrophoric... fuck lol.... But i suppose that doesnt really mean much... What makes professionally made catalysts better?

 

[OrgUnikum]

First of course the fact that they are professionally prepared

Being pyrophoric is a physical property and not related to certain chemical properties. Sorry.

Only palladium or platinum atoms which are at oxidation state zero are catalytically active and to get them there they must be derived from certain compounds in certain ways, if you seriously want to dabble in this: Its doable, the needed reagents are available the processes are doable, it is a catalyst though, and of course small contaminations can fuck them royally up so purity of everything used, at least absence of known catalyst poisons is essential.

Yes, yes ,yes "certain somethin..." sounds like obfusication, but I am not and will therefor post an article or two describing a correct method for high activity catalyst preparation as soon I can find it in the unsorted dump whats my personal archive.

Got one. Notes:
Starting palladium compound is tris(dibenzylideneacetone)dipalladium(0) (Pd2dba3), kindly note the (0) denoting the zero state of the metal. Sounds Unobtainium but this is actually easily prepared from freely available chemicals and a palladium salt like the acetate or chloride. Just Google the "preparation of...." and it should pop up.
High quality activated charcoal from coconuts is an excellent carrier and available at realistic costs, no need for fancy nanotubes or such.