Sciencemadness Discussion Board

Pd/C

Vogelzang - 7-9-2009 at 06:11

These two patents give methods for producing Pd on charcoal.

US 4421676 Process for preparation of palladium on carbon catalysts used in the purification of crude terephthalic acid

US 6066589 Hydrogenation catalysts

Coconut charcoal is prefered for some reason.

I found something that says coal based C is superior to coconut charcoal at least for use in aquariums. Any thoughts about making Pd/C using aquarium or water/air activated charcoal filtering media? Googling palladium and charcoal turns up a lot of articles and books about Pd/C hydrogenation catalysts. Coconut charcoal is sold on Ebay.

Quote:

Heat-activated bituminous coal-based Black Diamond granules are specially sized and far more efficient than inferior coconut, wood or peat-based carbons. Premium Black Diamond works as much as twice as fast as the competition.


http://www.marineland.com/sites/Marineland/products/productd...

Aquarium Pharmaceuticals also sell a something they call super activated carbon which is coal based.

[Edited on 7-9-2009 by Vogelzang]

Sedit - 7-9-2009 at 09:55

Quote:
Coconut charcoal is prefered for some reason.


Coconut charcoal is known to produce some of the finest activated charcoal around with a super large surface area.

Formula409 - 7-9-2009 at 14:55

Whilst not exactly what you're looking for, these definitely could be of interest! Especially if you are trialling methods and don't want to break the bank.
http://www.erowid.org/archive/rhodium/pdf/nickel-on-charcoal...
http://www.erowid.org/archive/rhodium/pdf/nickel-on-charcoal...

Formula409.

[Edited on 7-9-2009 by Formula409]

starman - 7-9-2009 at 18:28

Vogelzang- is there information on the mesh sizes of these aquarium type products?
F409- interesting read. I particularly like the use of nitrate salts, evaporation and the older method of simply heating to drive off NOx and H2O.Probably also applicable to Pd.
Pd metal,charcol, nitric acid and a heat source.Much more home friendly than the methods I've encountered for Pd/C.

Vogelzang - 8-9-2009 at 13:22

The mesh size varies from 4-5 mesh to smaller mesh. I found an interesting article today (attached).

Attachment: RusChemRev1992-p168-174-Pd-C.pdf (816kB)
This file has been downloaded 2522 times

Fleaker - 9-9-2009 at 13:25

There are numerous ways to make an active Pd/C. PdCl2 can be dissolved in a suitable organic solvent, or even chloropalladic acid can be used. Best results with hot H2 as reductant, cooling under H2, and bottling that way.The most important consideration is the charcoal. I have found that pellotised charcoals are good substrates if one is planning to reduce a lot of material and easily separate the catalyst for reuse.

If I had the spare time I would do a prepublication on Adams' and a suite of palladium catalysts.

Klute - 9-9-2009 at 15:01

Damn! Can't wait for that! It would be a delightfull contribution! NERV told me a bit about your work with PtO2, very interesting! And all that from scrap metal if I understood correctly?

Have you tried the H2 reduction method for Pd yourself? How active was the catalyst compared to commercial material?

Can't wait to hear some more!

zed - 9-9-2009 at 20:19

Hmmmmm. Do you suppose coal based charcoal might contain sulfur compounds?

crazyboy - 9-9-2009 at 20:52

Quote: Originally posted by zed  
Hmmmmm. Do you suppose coal based charcoal might contain sulfur compounds?


What is coal based charcoal and why would it be preferable to any other charcoal?

Fleaker - 10-9-2009 at 03:11

Coal based charcoal is essentially coke.

zed - 11-9-2009 at 21:29

There are often good reasons for using reagents of a specific origin. These materials work well for the job at hand..

Similar materials of a different origin, might not perform properly.

My query regarding possible residual Sulfur compounds, in coal based charcoal, had a purpose. Some catalysts are extremely sensitive to such compounds. Your catalyst then, might be inadvertently "poisoned" by the trace elements in the coal-charcoal substrate. Thereby causing your intended reduction, to completely fail.

Such screw ups are commonplace.

watson.fawkes - 12-9-2009 at 06:16

Quote: Originally posted by zed  
My query regarding possible residual Sulfur compounds, in coal based charcoal, had a purpose.
According to a table in Coke - A Treatise on the Manufacture of Coke and Other Prepared Fuels and the Saving of By-Products (1905), residual sulfur range between 0.6 % and about 2 %, with outliers for high-sulfur coal.

Paddywhacker - 14-9-2009 at 13:44

If you just want to buy Pd/C, then you might try Artcraft. I bought some 10% Pd on C from them about a year ago for US$6 per gram.

Waffles - 18-9-2009 at 08:48

I have a bunch of excess Pd/C, Engelhard material in original container I believe, give a U2U if you're interested. I could also trade for Pd raw material if you already have some.

UnintentionalChaos - 19-9-2009 at 17:13

http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=cv3...

Have a lookee there. Pd is fairly cheap, about $10/g at spot value. One gram would be enough for 20g of 5% Pd/C after dissolving in a little aqua regia.

The coal based activated charcoals have higher surface area than the organic matter based ones, IIRC, which is a definite advantage for water purification. However, they almost surely have residual sulfur compounds in them, and platinum group metals are highly sensitive to sulfur contamination.

Vogelzang - 20-9-2009 at 11:07

I found an article about coconut charcoal.

http://www.fileden.com/files/2008/8/24/2063601/chemistry/JCE...

Picric-A - 25-10-2009 at 03:49

Hi i am looking to buy some Pd/C for a school project (rasberry ketone).
My source will be Acros but i have a few questions first. What difference does the % Pd make? I guess its just speed of hydrogenation but thats just a guess. Also when it says 10g, is that 10g of the palladium and carbon together or just 10g of Palladium metal on carbon.
thanks

gsd - 25-10-2009 at 09:50

Quote: Originally posted by Picric-A  
Also when it says 10g, is that 10g of the palladium and carbon together or just 10g of Palladium metal on carbon.
thanks


It is Pd and C together making 10 gm.

gsd

[Edited on 25-10-2009 by gsd]

Picric-A - 25-10-2009 at 10:26

awsome thanks,

Vogelzang - 25-11-2009 at 16:21

This experiment gives a method of producing a supported Pt catalyst using sodium borohydride. I can't remember what book it comes out of.

Attachment: Ch16-CatHyd.pdf (227kB)
This file has been downloaded 968 times


ANDLOS - 18-12-2009 at 11:27

I want to ask how to handle pd/c after use is there any method for reuse after first time used in reduction to use it second time,

thanks alot

entropy51 - 18-12-2009 at 11:34

One answer from Googling.

ANDLOS - 18-12-2009 at 11:40

but this answer from trade source need money I mean if there is simple procedure for recycling that I can carry out

entropy51 - 18-12-2009 at 15:31

I know, but when I worked in industry we never recycled hydrogenation catalysts. I once asked asked why not, because they were expensive. The Real Chemists who ran the labs said it wasn't worth the trouble. Others here may know better, though.

Nicodem - 19-12-2009 at 15:27

Quote: Originally posted by ANDLOS  
but this answer from trade source need money I mean if there is simple procedure for recycling that I can carry out

You might find the answer if you UTFSE. As far as I remember, this topic was already discussed and the regeneration processes for Pd-C were posted and I think it was pretty simple.

stoichiometric_steve - 20-12-2009 at 08:44

Quote: Originally posted by Nicodem  
the regeneration processes for Pd-C were posted and I think it was pretty simple.


Oh yeah, it is. Wash your used catalyst with whatever organic solvent will take off the crap that you just processed, wash with dilute NaOH, wash off the NaOH until pH=7, dry in plain air, and re-reduce it if necessary.

Vogelzang - 27-12-2009 at 18:32

Look at the patents in http://www.uspto.gov/web/patents/classification/uspc502/sche...

Vogelzang - 27-12-2009 at 18:38

http://patft.uspto.gov/netacgi/nph-Parser?Sect1=PTO2&p=1...

Vogelzang - 27-12-2009 at 18:50

http://patft.uspto.gov/netacgi/nph-Parser?Sect1=PTO2&Sec...

Vogelzang - 27-12-2009 at 19:18

http://www.google.com/patents?id=PvWfAAAAEBAJ&printsec=a...


http://v3.espacenet.com/publicationDetails/originalDocument?...

Vogelzang - 29-12-2009 at 15:40

Regeneration of Pd and other noble metal catalysts:

US 2208616 Reactivation of spent hydrogenation catalysts

US 2270874 Method of activating catalytic surfaces

US 2344208 Process for regenerating a "spent" noble metal oxide hydrogenation
catalyst

US 2664404 Regeneration of selective hydrogenation catalyst

US 2692240 Reactivation of alumina supported palladium catalysts

US 2955089 Reactivation of deactivated catalyst

US 2963444 Reactivating noble metal containing catalysts

US 3134732 Reactivation of regenerated noble metal catalysts with gaseous
halogens

US 3135699 Process for regenerating a hydrogenation catalyst

US 3214385 Reactivation of spent palladium-oncarbon hydrogenation catalyst

US 3650983 ALKALINE WASH REACTIVATION OF PALLADIUM CATALYSTS USED IN VINYL
ACETATE SYNTHESIS

US 3542863 PALLADIUM CATALYST TREATMENT WITH FORMIC ACID

US 3879311 Catalyst regeneration

US 3959382 Method for reactivating palladium catalysts

US 4092267 Process for regenerating palladium catalysts

US 4147660 Method for reactivation of platinum group metal catalyst with aqueous
alkaline and/or reducing solutions

US 4164481 Process of regenerating a noble metal catalyst used in the reduction
of organic nitro compounds

US 4190554 Method for reactivation of platinum group metal catalyst with aqueous
alkaline and/or reducing solutions

US 4260518 Process for the regeneration of metallic catalysts

US 4422954 Method to restore the metal content of a noble metal hydrogenation
catalyst

US 4717696 Regeneration of a supported palladium catalyst used in the conversion
of cyanohydrins to their aldoses

US 4891346 Redispersal of Ru, Os, Rh and Pd catalysts and processes therewith

US 4914256 Reactivation of partially deactivated catalyst employing ultrasonic
energy

US 4952543 Process for dispersing or redispersing a Group VIII noble metal
species on a porous inorganic support

US 4980324 Regeneration or activation of noble metal catalysts using
fluorohalocarbons or fluorohalohydrocarbons

US 4992614 Reactivation of partially deactivated catalyst employing ultrasonic
energy

US 4999326 Palladium catalyst reactivation

US 5068477 Process for reducing a refining catalyst and use of the catalyst in
hydrogenation

US 5573988 Catalyst regeneration process

US 6071843 Process for reactivating catalyst systems containing a platinum group
metal

US 6740615 Regeneration of used supported noble metal catalysts

US 6753285 Process for regenerating a used precious metal catalyst

US 6908873 Regeneration of spent supported metal catalysts

US 7368409 Regeneration method of heterogeneous catalysts and adsorbents

US 7622416 Hydrogenation catalyst, its preparation and use