bumblebeetuna (Stranger)
11-09-00 23:34
No 68282
      making palladium catalyst  Bookmark   

I thought I would post this so in the future other bee's do not have to go through the hell I did....

-------------------------------------------------------------------------------
                        Palladium Catalyst faq rev 0.01
                        Channelled By : Randolph Carter
-------------------------------------------------------------------------------

1-Palladium on Carbon (charcoal)(5% Pd)

Prepare a solution of 1.7 g of Palladium Chloride (1)in 1.7 ml of concentrated
hydrochloric acid and 20 ml of water by heating on a water bath for 2 hours or
until solution is complete, and add this to a solution of 30 g of sodium acetate
trihydrate in 200 ml of water contained in a 500 ml hydrogenation flask. Add 20
g of acid washed activated charcoal (2) and hydrogenate in an atmospheric
hydrogenation apparatus (fig 1 to follow if yer lucky...)until absorption
ceases. Collect the catalyst on a buchner funnel and wash it with five 100 ml
portions of water and suck dry as possible. Dry the catalyst at room temperature
over potassium hydroxide pellets or anhydrous calcium chloride in a vacuum
dessicator. powder the catalyst (approx 20 g yield...)and store in a tightly
stoppered glass bottle, under a stump, by the creek, around the bend, close to
the edge, down by the corner.

2-Palladium on Carbon (charcoal) (30% Pd)

Prepare a solution of 8.25 g of palladium chloride(1) in 5 ml of concentrated
hydrochloric acid and dilute with 50 ml distilled water. Cool the solution in an
ice-salt bath and add 50 ml of 40% formaldehyde solution and 11 g of acid washed
activated charcoal(2). Stir the mixture mechanically and add a solution of 50 g
of potassium hydroxide in 50 ml water, keeping the temperature below 5 deg c.
When the addition is complete, raise the the temperature to 60 deg c for 15
minutes. Wash the catalyst thoroughly by decantation with water as above and
finally with dilute acetic acid, collect on a buchner filter and wash with water
free from chlorine or alkali. Dry at 100 deg c and store in a desiccator or
under a stump as above...

3-Palladium Black

Dissolve 5 g palladium chloride in 30 ml concentrated hydrochloric acid and
dilute with 80 ml water; cool in an ice-salt bath and add 35 ml 40% formaldehyde
solution. add a cold solution of 35 g potassium hydroxide in 35 ml water
dropwise during 30 minutes to the vigorously stirring palladium solution. Warm
to 60 deg c for 30 minutes and the wash the palladium precipitate six times by
decantation with water Filter on a sintered crucible, wash with 1 liter water
and suck dry (approx 3.1 g yield) and transfer to a dessicator charged with
silica gel or alternately under a stump as above.....


Notes:

(1) Alternately, the equivalent (molar) quantity of palladium chloride dihydrate
    may bee used....

(2) Any of the commercial forms of activated charcoal/carbon ("Norit", "Darco",
    "Big K Brand", GNC etc...)may bee employed; the carbon should bee heated on
    a steam bath with 10% nitric acid for 2-3 hours, washed free of acid with
    water and dried at 100-110 deg c before use...

All water used must bee high grade distilled totally free of chlorine/ other
halogens and alkali.

The sodium acetate dihydrate may bee prepared from vinegar/sodium hydroxide
reaction as covered elsewhere.

The 40% formaldehyde may bee substituted by use of a 37% solution instead or
preperation of your own solution in that neighborhood from parformaldehyde
heated in water as covered elsewhere/when....

The potassium hydroxide may bee obtained thru photo or alternately "wet" NiCad
battery outlets (dream of airplane and medical equipment battery suppliers...)

-------------------------------------------------------------------------------

Adam's Catalyst

In a fume cupboard, dissolve chloroplatinic acid (H2PtCl6.6H2O, 0.10 g) in water
(ca. 0.5 ml) in a porcelain crucible (3-4 cm diameter). Add sodium nitrate (1 g)
and evaporate the mixture to dryness, over a low flame, with continuous
stirring. Turn the Bunsen burner full on and stir the contents of the crucible
vigorously until the mass has melted completely and the initial decomposition
has subsided. Keep the bottom of the crucible at a dull red heat for a further
30 min. (too strong a heat decomposes the oxide to the metal). Allow the
crucible to cool and wash the contents into a 250 ml. beaker with hot water from
a wash bottle. Filter off the brown platinum oxide with a small ('Hirsch')
funnel (Whatman paper No. 541) and wash the oxide with hot water (about 200 ml)
until the washings are free from nitrate ion. Dry the catalyst over calcium
chloride in a vacuum desiccator.

Palladium Black

Heat a mixture of palladium chloride (0.50 g) and water (100 ml) to 80deg.C and
carefully neutralise the suspension, to wide-range indicator paper, with 20%
sodium hydroxide solution (if the end point is overshot, palladium hydroxide
precipitates). Add 2.6% formic acid (2.5 ml) and, after about 2 min. make the
solution strongly alkaline with 20% sodium hydroxide solution (5 ml). Add more
of the formic acid (5 ml) and make sure that the solution is still alkaline.
Heat the mixture on a steam bath for 2 hours. Filter off the precipitate with a
small ('Hirsch') funnel (Whatman filter paper No. 541), wash it free from alkali
and dry it over calcium chloride in a vacuum desiccator.


5% Palladised Charcoal

Heat decolourising charcoal (7.5 g) on a steam bath for 2-3 hours with conc.
hydrochloric acid (5 ml) and water (150 ml). Wash the charcoal by decantation
with hot water until free of acid, filter it off, and dry it in an oven at
<100deg.C. Warm palladium chloride (0.5 g) in conc. hydrochloric acid (0.75 ml)
and water (5 ml) on the steam bath for ~ 20 min. Add the solution to AnalaR
sodium acetate (17.5 g) in water (50 ml) contained in a hydrogenation flask.
Introduce the purified charcoal (5.8 g) and hydrogenate the mixture until no
more hydrogen is absorbed (~ 2 h). The hydrogenation procedure is described
below. Collect the catalyst on a 7 cm Buchner filter (3 thicknesses of Whatman
No. 1 filter paper), wash it with water (5 x 100 ml) and drain it on the filter
with suction. Dry the catalyst over fresh silica gel in a vacuum desiccator and
store it in a tight stoppered bottle.


Lindlar's Catalyst (5% Pd on CaCO3, poisoned with Pb)

Stir calcium carbonate (precipitated, light; 1.1 g) in water (10 ml) in a flask
which is fitted with a thermometer and mounted on a magnetic stirrer/hotplate.
Whilst continuing the stirring, add palladium chloride (90 mg) to the suspension
and after 5 min., raise the temperature to 80deg.C for a further 10 min. Cool
the mixture and transfer it to a hydrogenation flask, using ~ 10 ml of water for
rinsing. Hydrogenate the mixture until hydrogen absorption (10-20 ml) is
complete (ca. 15 min); the hydrogenation procedure is described below. Collect
the reduced catalyst on a small 'Hirsch' funnel (Whatman filter paper No. 1) and
wash the catalyst with distilled water (20 ml). Add the damp catalyst to
distilled water (10 ml) in a flask on the magnetic stirrer/hotplate. Switch on
the stirrer, add a 5% (w/v) solution of AnalaR lead acetate in water (2 ml) and,
after 10 min., raise the temperature to 90deg.C for 40 min. During this time,
add distilled water, as necessary, to compensate for evaporation losses. Cool
the mixture, collect the catalyst on Whatman No. 1 paper in a small 'Hirsch'
funnel and wash the catalyst with distilled water (total, ~ 50 ml). Transfer the
catalyst to a clean, tared, specimen tube and dry the catalyst in a pistol at
40deg.C to constant weight (~ 1-3 h). Crush the dry catalyst to a powder with a
clean spatula or glass rod and stopper and label the tube (catalyst yield: 0.9-1 g).

-------------------------------------------------------------------------------

Preparation of Palladous Oxide (PdO) (Org Chem Coll Vol 2, p 566)

In a 350-cc. casserole, 2.2 g. (0.02 moles) of palladium metal is dissolved in
a small amount of aqua regia, and the solution is treated with 55 g. of sodium
nitrate and enough distilled water to make a thick paste. The substances are
thoroughly mixed and then heated gently to drive off the water. The heating is
increased until the mixture melts (about 270-280įC) and continued cautiously.
Just above the melting point the mixture must be stirred and heated carefully
as oxides of nitrogen are evolved and foaming occurs. After the evolution of
gases is nearly complete (about five minutes) the full flame of a Bunsen burner
is applied for about ten minutes. The entire time of heating should be about
onehalf hour. As the mass cools, the casserole is rotated to allow the melt to
solidify on the sides of the dish. After digestion with about 200 cc. of
distilled water until the sodium salts are completely dissolved, the dark brown
precipitate of palladous oxide is filtered and washed thoroughly with 1 per cent
sodium nitrate solution (1). The oxide must not be washed with pure water since
it shows a marked tendency to become colloidal. After drying in a vacuum desiccator
the palladous oxide weighs 2.3-2.4 g. (91-95 per cent of the theoretical amount) (2).

(1) The filtrates should be clear and colorless; if they show a yellow-orange
opalescence, some of the oxide has become colloidal. The palladium may be recovered (3)
as the oxide by evaporating the filtrates to dryness and re-fusing, or as palladium
black by rendering the filtrates slightly alkaline with sodium carbonate and heating
with formaldehyde.

(2) A small amount of palladous oxide adheres to the casserole and cannot be removed
by the ordinary means. The oxide is not dissolved readily by aqua regia but is easily
removed by boiling with 48 per cent hydrobromic acid.

(3) See J. Am. Chem. Soc. 46, 1684 (1924) and Adams, J. Am. Chem. Soc. 47, 1147 (1925).

-------------------------------------------------------------------------------
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 00:39
No 68291
      Re: making palladium catalyst  Bookmark   

Or go buy some... Which one sounds easier?


Wait a damn minute....
 
 
 
 
    serodronin
(Stranger)
11-10-00 00:44
No 68296
      Re: making palladium catalyst  Bookmark   

they should be about the same price either way, but which one do you think is watched?  you can buy PdCl2 over the counter.  I don't think you can acquire Pd/C without ordering it.
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 01:00
No 68304
      Re: making palladium catalyst  Bookmark   

To the contrary, you can buy Pd/c from any chem supplier or photoshop and palladium catalysts arenít watched.  The dea already has there hands full trying to watch Rp/I labs... They dont have the workforce to even consider worrying about home hydrogenation.
 
 
 
 
    bumblebeetuna
(Stranger)
11-10-00 01:05
No 68306
      Re: making palladium catalyst  Bookmark   

ok, what so what is pd/c used for in photography, ?
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 01:09
No 68308
      Re: making palladium catalyst  Bookmark   

To tell you the truth I dont remember what its used for in photography but I called a local photoshop to verify it was correct and they were selling it by the gram.


Wait a damn minute....
 
 
 
 
    bumblebeetuna
(Stranger)
11-10-00 01:18
No 68312
      Re: making palladium catalyst  Bookmark   

Funny thing is, earlier you told me it could only be bought at chem supplys, THAT WAS EARLIER IN THE NIGHT , .....
 
I ll be nice and post the message in its entirety

 
  Mystic
(Hive Bee)
11-09-00 23:48
         Re: Acquisition of 10g 3%Pd/C,    Reply   
 
Common sence hasnt told you already that you need to go to a fucking chem shop?  Comon!! Are you really expecting to find this shit at a grocery store or something?!  Buy it at a chem shop or make it.
--------------------------------------------------------------------------------
 Wait a damn minute....   
  

here is a post i found it in
Post 67606 (paranoidandroid: "Re: Pd vs. Pt", Chemistry Discourse)

palladium salts are often used in conjunction with platinum salts.  palladium gives the warmer tone to the mix.  A common mix for platinum photography is a 1:4, platinum to palladium mixed in a shot glass with some special developer.  Now this gets spread on a piece of blotter or whatcolor paper.  This smear is then covered with your negative and left in extreme sunlight.  a few hours later you have a black and white photograph of extreme resolution.  The bad part is your picture only comes out as big as your negative.  It is avery simple process, and no dark room is needed

after reading this post I doubt they sell pd/c at photo shops,  most likely they sell palladium salts
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 01:33
No 68315
      Re: making palladium catalyst  Bookmark   

What's your point?


Wait a damn minute....
 
 
 
 
    bumblebeetuna
(Stranger)
11-10-00 01:39
No 68317
      Re: making palladium catalyst  Bookmark   

mystic please refrain from posting here, the idea of the post is to present info to future bees, by elaborating on what I am learning, not to continue a battle with your ignorence,
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 01:41
No 68318
      Re: making palladium catalyst  Bookmark   

Your info is a hassle to newbees.  Why would you wanna make it when you can go buy it for the same price?!


Wait a damn minute....
 
 
 
 
    bumblebeetuna
(Stranger)
11-10-00 02:22
No 68337
      Re: making palladium catalyst  Bookmark   

JAIL
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 02:30
No 68339
      Re: making palladium catalyst  Bookmark   

Its not watched.  You dont fill out forms when you buy it. Where I live you dont even show id.  But most likely in other places you'll have to show id... so what, get a fake one.


Wait a damn minute....
 
 
 
 
    bumblebeetuna
(Stranger)
11-10-00 02:46
No 68352
      Re: making palladium catalyst  Bookmark   

so tell me how much does this pure pd/c cost at the photography store you get it at?
 
 
 
 
    Mystic
(Hive Bee)
11-10-00 02:57
No 68357
      Re: making palladium catalyst  Bookmark   

I dont buy it from a photoshop... I simply listed that as a place for people to get it from.  I've called to see that they actually sell it but I dont know how much they sell it for.  As for the chem shop I pay 150 for 10 grams 10% Pd/C.


Wait a damn minute....
 
 
 
 
    serodronin
(Stranger)
11-10-00 03:26
No 68369
      Re: making palladium catalyst  Bookmark   

ignore mystic.  the only knowledge he has of chemistry is what he reads while moderating this website (personally I think he's working with pigs to spread misinformation to newbees.)  they only sell palladium chloride at photo supply stores.  and most palladium catalysts ARE watched.(what the FUCK makes you think they aren't, hmmm?  they've been documented in multiple meth patents since the late 60's)  so making your own catalysts is a good idea.  If you stumble across a simple procedure for Pd/BaSO4, be sure to post it.  I'm sure a lot of people would appreciate it.
 
 
 
 
    Osmium
(Stonium's / Changer)
11-10-00 03:53
No 68375
      Re: making palladium catalyst  Bookmark   

Organic Syntheses has procedures for Pd catalysts, including Pd/C, BaSO4 and CaCO3.
 
 
 
 
    KrZ
(Hallucinogenius)
11-10-00 06:00
No 68406
      Re: making palladium catalyst  Bookmark   

Not to mention, most suppliers charge you an arm and a leg for something that the hobbyist could make for MUCH MUCH less.  Especially if you couple this with a Pd -> PdCl2 reaction from a coin.  A single $700 ingot could net you 600g of 5% Pd/C with a little effort!  It is a relatively dangerous synth though, lookout for those hydrogen flashes!
 
 
 
 
    bumblebeetuna
(Stranger)
11-10-00 06:31
No 68412
      Re: making palladium catalyst  Bookmark   

This can be done by useing bright stars method.....
-------------------------------------------------------------------------------
          Palladium(II)Chloride from palladium metal - by Bright Star
-------------------------------------------------------------------------------

Put your Pd(metal) in an alcohol solution. For 5 grams of Pd(metal) use 500mL of
Alcohol. Methanol, Ethanol, IPA ... it doesn't matter. Add about 50mL of water
per 5 grams of Pd. Now add an equimolar amount of CuCl2, Copper(II)Chloride.
Put in a stirrbar, seal the container, and set it stirring. Comeback in ~10
hours and there wil be copper particles on the bottom, and PdCl2 in solution.
Filter the copper out. Evaporate the alcohol and water off ... and voila.

Rate of reaction is affected by Pd surface area. IE If its a Pd coin, then it
might take several days, if its Pd Powder, then it will only take several hours.

The reason it works is that the crystal structures for Pd and PDCl2 are
completely different. The PdCl2 will go into solution due to solvation and
steric effects, exposing new Pd to react with the solution. Cu metal will
crystalize and fall out of solution.

It works.    But it takes like 24 hours ...
If you add a little (~5mL) of Muratic Acid, it will go faster.

Good Luck
-------------------------------------------------------------------------------
 
 
 
 
    KrZ
(Hallucinogenius)
11-10-00 06:52
No 68417
      Re: making palladium catalyst  Bookmark   

You must add HCl.  And it will take much longer than BS says using a coin, you must agitate the mix for a long period of time so that the corroded sections of the coin will fall off.  Current price of Platinum is $600, Palladium is at $800.

Average prices for Catalyst;
Pd/C 10% $350 per 100g
Pd/C 5%  $200 per 100g
Pt/C 5%  $300 per 100g (I know that sounds strange but that's the best I could find)

So you'r making;
300g 10% Pd/C At a cost of $800 as opposed to $1050
600g  5% Pd/C At a cost of $800 as opposed to $1200
600g  5% Pt/C At a cost of $600 as opposed to $1800!!

Plenty of room for error with big savings.
 
 
 
 
    C10H15N
(Stranger)
11-10-00 22:48
No 68617
      Re: making palladium catalyst  Bookmark   

in responce to

Why would you wanna make it when you can go buy it for the same price?!


 Mystic what you fail to realize is that it is important to
know different chemical synths. It may not be watched now but it might in the future,hard to tell what the pigs are looking at.And one day if its watched your gonna thank bumbelbeetuna for his advice on making Pd/C.
  I would encorige people to come up with different rxns for everthing.You never know when your gonna need it.
 Oh and BTW Thanks bublebee for your post on Pd/C im
behind you 100% on that post.
 And FUCK off mystic for your igoric ass trying make Bublebee think he/she wrote something stupid!FUCK some people just dont understand.

its only a matter of time.cool
 
 
 
 
    bumblebeetuna
(Newbee)
11-11-00 00:21
No 68642
      Re: making palladium catalyst  Bookmark   

thanks,  i have been doing alot of research on alternate methods for all kinds of precursos , i have just made an elaborate write up on making ephedrine,  with exact precudures for making 200 grams of p2p-alchol in 4 liters of water, with very easy to find otc chemicals,   but .... that is to come later,  i need to experiment a bit first... hey thanks again for your support, i m glad to see some realistic logical people...and its she
 
 
 
 
    SuNNySide
(Hive Bee)
11-12-00 16:50
No 68933
      Re: making palladium catalyst  Bookmark   

http://www.environment-agency.gov.uk/epns/pdf/ipr2_10.pdf


#1)NEVER MAKE DRUGS OR DO ANYTHING ILLEGAL
IT'S AGAINST THE LAW!!!!!!
 
 
 
 
    SuNNySide
(Hive Bee)
11-13-00 15:24
No 69099
      Re: making palladium catalyst  Bookmark   

Platinum and Palladium- If you have a new catalytic converter  that you want to get palladium out of here is how To insure high purity of the platinum and palladium, you will need to re-refine this material. Put this material in a fresh aqua regia bath. However, heat the acid to simmering. Continue heating until all the platinum metals are dissolved (that may take 1-2 hours). When completely dissolved at 1 ounce of ammonium chloride for every ounce of dissolved platinum metals. The platinum will precipitate as a red mud and palladium will be orange. If you want to leave the iridium in the platinum, then wait for it to precipitate before recovering the platinum and palladium. Iridium will precipitate as a blue-black mud after the platinum precipitates.


#1)NEVER MAKE DRUGS OR DO ANYTHING ILLEGAL
IT'S AGAINST THE LAW!!!!!!
 
 
 
 
    foxy2
(Hive Addict)
11-13-00 16:48
No 69115
      Re: making palladium catalyst  Bookmark   

Sunnyside
How would you suggest separateing the salts once you have them????
Anyone else have any ideas?
Maybee a fractional crystallization???

Foxy Is Interested
 
 
 
 
    bumblebeetuna
(Hive Bee)
11-13-00 18:58
No 69128
      Re: making palladium catalyst  Bookmark   

I seen a post about this.....but ?Ii dont remember what it was... check teh hive
 
 
 
 
    Mystic
(Hive Bee)
11-13-00 19:36
No 69139
      Re: making palladium catalyst  Bookmark   

C10H15N: good point... Now if you'd please take your boot out of my ass. tongue


Wait a damn minute....
 
 
 
 
    Ballistic
(Newbee)
11-14-00 01:55
No 69226
      Re: making palladium catalyst  Bookmark   

Could one substatute one palladium catalyst for another?
Example:Recipe calls for Palladium Black, but all I have
is 5% palladium on carbon. Is there a ratio between the
different catalyst that anyone knows of or is it calculated
by how much palladium is in each kind of catalyst?


The rain in Maine falls mainly down the drain.
 
 
 
 
    Osmium
(Stonium's / Changer)
11-14-00 02:02
No 69229
      Re: making palladium catalyst  Bookmark   

Bumblebeetuna, check a good industrial chemistry book the next time you are at the library. Kirk-Othmer for example. It contains all the information you need about separation of platinum metals
 
 
 
 
    bumblebeetuna
(Hive Bee)
11-14-00 05:58
No 69254
      Re: making palladium catalyst  Bookmark   

huh? i think foxy wants to know that... I know I have already read a post on seperating pd from pdcl3, i think it was called palladium black.....not sure tho...crazy
 
 
 
 
    SuNNySide
(Hive Bee)
11-16-00 18:37
No 69728
      Re: making palladium catalyst  Bookmark   


Sunnyside
How would you suggest separateing the salts once you have them????
Anyone else have any ideas?
Maybee a fractional crystallization???

Foxy Is Interested




precipitate with DMG (dimethylgloximene)



#1)NEVER MAKE DRUGS OR DO ANYTHING ILLEGAL
IT'S AGAINST THE LAW!!!!!!
 
 
 
 
    Chromic
(Hive Bee)
11-17-00 13:23
No 69892
      Re: making palladium catalyst  Bookmark   

Has anyone tried dissolving Pd metal in concentrated H2O2 with concentrated HCl(aq)?

Electrochemically, it would seem to work, and it would probably work quite fast, even faster than Bright Star's method:

H2O2 + 2 H+ + 2 e- -> 2 H2O (+1.776V)
Pd  -> Pd2+  + 2 e- (-0.83V)

I imagine this reaction would also work with copper metal (probably pretty fast too) and mercury metal (probably about the same speed) as well. I don't have any palladium or mercury metal lying around so I can't try this myself.

I'd still love to hear someone explain to me how Pd(s) + Cu2+ is supposed to give Pd2+. I bet oxygen is required for this reaction to work and I bet it only occurs in acidic conditions... so a stir bar in the flask with the coin would speed up the reaction immensely...
 
 
 
 
    Chromic
(Hive Bee)
11-21-00 21:44
No 70273
      Re: making palladium catalyst  Bookmark   

Yeah, copper gives a very very dark green solution in a couple hours w/45ml 3% peroxide and 15ml conc. HCl. A good source of high purity copper is copper tubing... of course, everyone has got copper salts lying around, but it might be useful for making Pd/Hg salts. I would love for someone to try it.
 
 
 
 
    Triton
(Newbee)
11-19-02 13:52
No 381309
      Anyone know if this would work with Pd?  Bookmark   

Anyone know if this would work with Pd?