arrowsmith (Stranger)
08-17-00 05:03
No 41796
      O2 wacker, my version  Bookmark   

I made an oxygen generator out of PVC pipe, complete with pressure gauge. Then I charged it with hydrogen peroxide. My reaction vessel was a filter flask, wrapped up in 9 layers of duct tape. I connected it to the O2 generator with braided 1/4" hose.

I got the O2 by adding a pinch of cobalt hydroxide. Went like a mo-fo. I had the thing rigged up with a stopcock/syringe subassembly so's I could inject more H2O2 as needed.

I used magnetic stirring - this was a very small scale dream. I turned it up so that the stirbar kept the stuff splashing all over the inside of the flask. This contraption withstood 3 atm!

I got about a 60% yield.

Not claiming a technical breakthrough here, but someone might find this variation useful.

"On that Tower of Babel they knew what they were after."
(Hive Bee)
08-17-00 15:00
No 41944
      Re: O2 wacker, my version  Bookmark   

Way to go arrow arrowsmith!

Few questions: How long did the rxn go for? What was the average pressure. Did it run at 3atm throughout? What was involved in regulating the pressure? What size filter flask was used?

Jimi loves ya!
08-17-00 15:40
No 41955
      Re: O2 wacker, my version  Bookmark   

Amazing!  No Palladium!    I think you've invented a whole new branch of Chemistry!    Catalytic Oxidation without the catalyst!    Call JACS!


Aminate and see if the product is active.
09-12-00 23:43
No 51464
      Re: O2 wacker, my version  Bookmark   

It was a 500 ml filter flask. The average pressure? Geez, you got me there. I fed the O2 in through the sidearm, and vented it periodically through a stopcock I had stuck in a one hole stopper in the mouth of the flask.

My inspiration was Spiceboy's KRV that he made out of a soda bottle. I figured I could do with a lot less pressure(and shaking!), since I was using pure O2 instead of air.

Sorry it took so long for me to get back to you. Happy dreams, buddy.

"On that Tower of Babel they knew what they were after."
09-12-00 23:54
No 51471
      Re: O2 wacker, my version  Bookmark   

Yeah, smart fella; I waved the amulet of the Grand Bazoo over the flask, it cost a lot less than palladium.

Of course I used Pd; in fact, I closely followed the Spiceboy KRV procedure on Rhodium's page as far as reactant proportions. I vacuum distilled the product and got a light yellow liquid with greenish highlights, that had the cardamon odor described in various posts.

Amination was done according to *your* procedure - except I used thick Al sheet, not foil. It always worked fine with the unsubstituted compound. But with this rxn it was a mistake. I got a fizzle yield (about 15%) of a very light pink finely crystalline solid. Active? Well, never having done this stuff before, I ate 120 mg and sat down to watch a B movie...about 90 minutes later my cerebrum was undergoing total meltdown.

BTW, not sure I like this stuff. I've done lots of acid in the past. I no longer enjoy that either. I think I've had enough mind "expanders" - now what I need are mind "fabric softeners".

In any case, thanks for your well written procedure. It helped me.

"On that Tower of Babel they knew what they were after."
(Hive Addict)
12-18-00 18:49
No 76319
      Re: O2 wacker, my version  Bookmark   

What about using cobalt salts as the oxidation catalyst.  Page 191 of "Liquid-Phase Oxidation of Hydrocarbons" by Emanuel, Denisov, and Maizus begins chapter 6 - Catalysis with Salts of Metals of Variable Valence.

They talk about using organic salts of cobalt, manganese, iron, copper, chromium, lead, and nickel to oxidize various hydrocarbons.  The oxidation of aldehydes to ketones with cobalt acetate looked interesting, but most of the text was so far over my head I have paper cuts on my scalp!

Perhaps someone who actually knows something could check it out.

(Hive Bee)
12-19-00 02:14
No 76412
      Re: O2 wacker, my version  Bookmark   

There are hundreds of oxidative catalysts available, comprised of dozens of different transition metals in various oxidative states, with various ligands, etc. However, palladium is unique because it yields specifically alpha-methyl ketones from terminal olefins, while others would result in the formation of epoxides or diols - both quite useful, but requiring an additional isomerization step to form the ketone, costing time, money, and product.

Still, its good to keep in mind. Perhaps some day palladium will become more difficult to obtain (especially with the prices going up as they are), and its smart strategy to have other options.
(irritable and cranky)
12-20-00 03:02
No 76652
      Re: O2 wacker, my version  Bookmark   

arrowsmith, (if you are still around?)
What solvent was used in the O2 wacker?

Let's fuck!
(Hive Bee)
12-16-02 21:15
No 390050
      Would sodium hydroxide work instead?  Bookmark   

Would sodium hydroxide work instead of cobalt hydroxide to force the peroxide to release the o2?

Not a chemist I just follow directions on the box mix
(Hive Bee)
12-17-02 12:28
No 390193
      Soda pop syrup tank as the ideal pressure vessel?  Bookmark   

2 pressure fittings. 1 for o2 in and 1 for a pressure gauge and pressure release.
Removable cap for putting in the glass that has the safrole you are converting.
Cheap $10 used. Probably spend way more on the gas fittings.
Reuseable indefinitely.
Drawbacks: cannot be stirred, the cap opening is not that wide. Shaker or rocker is needed. For rocking you probably need to use a tall cylinder to avoid spilling. Baby rocker?

<copied from usenet not verified information>
These 5 gallon tanks were originally used by soda
pop manufacturers to hold soda syrup (extract). 
They made from stainless steel,  rated to 130 psi and designed for repeated use. They are 25 inches tall and about 8 inches in diameter.

Not a chemist I just follow directions on the box mix
(Hive Bee)
12-17-02 16:17
No 390234
      A question  Bookmark   

I'm just wondering about palladium chloride on metal,
any side reactions could be goign on? It's just a question, not a statement
(Hive Bee)
12-17-02 17:31
No 390252
      Yes  Bookmark   

That will not work you don't want to do a wacker oxidation in stainless steel. It won't go the palladium will coat the steel.
(Hive Bee)
12-17-02 17:41
No 390256
      Not running the reaction on bare steel  Bookmark   

from my previous post
Removable cap for putting in the glass that has the safrole you are converting.

As long as you keep the solution in a glass container inside the syrup canister how would this be a problem?  The glassware has soft airy material around it to cushion it and hold it in place yet still provide room for o2. Wish they made epoxy glass like epoxy plastic, steel and copper putty. It would be nice to be able to coat the inside of the syrup can in glass or maybe teflon. Since that is not practical though a long neck boiling or volumetric flask that can fit thru the opening would be used. A baby rocker can rock this back and forth sloshing the ingrediants. I think a boiling flask would be ideal for mixxing in o2 while rocking. The shape would work well for the fluid pouring back down during the down swing to mix the liquid. Rocking would probably take longer but with an electric baby rocker it can be rocked indefinitely. Seems better than trying to shake a pop bottle that can explode.

I think these are an ideal pressure vessel and also great for reactions that can be done in stainless for bees who cannot get glass.

If anyone has a baby rocker can they try rocking a small boiling flask that has some water in it to see how well it sloshes without spilling out? Wrap it in a towel and stick it in a big pot to simulate the syrup can.

I think glass pipe wrap would be an ideal inert non flamable cushioning to secure the flask in the syrup can. No need to repeat the Apollo 1 fire.

Not a chemist I just follow directions on the box mix
(Hive Bee)
12-17-02 20:11
No 390277
      I like your idea  Bookmark   

The idea of placing a glass container in a stainless steel container isnt bad.
But I'm wondering at what pressure you want to put a small boiling flask. I dont think these are made to withstand 40 PSI.

But what about a flask of some sort with a small opening, placed in a sealed stainless steel container. Placed to rock in such a way that even opened, it cant leak(say for example you plug your opening with a tube, and then secure that tube in place, the opening always facing up).
If you leave the an opening, pressure should be equal on both sides of the glass, with no chanvce of breaking it right? Of course the whole systme wouyld be closed. That way the pressure would be taken by the stainless steel vessel, and the glass would be fine,
What do you think?
(Hive Bee)
12-17-02 20:23
No 390281
      The flask is open  Bookmark   

Aye the syrup can holds the pressure. You want the flask open not sealed shut. This is why a long neck flask is desired. The glass makes the mdp2p easy to remove and keeps the paladium chloride out of contact with the stainless steel. If the flask is sealed then it does not get o2. Might be able to fit in 3 or 4 glass coke bottles or an empty 40 ounce beer. The beer bottle has a volume advantage over a boiling flask that can fit in a 5 or maybe 6 inch opening. I think a stopper in the top with hdpe tubing could work to contain spills but may not be needed. I still think a long neck boiling flask may do best for mixxing due to its shape.

For the money a used syrup canister cannot be beat. What other cheap pressure vessels have 2 gas fittings, a main opening and can handle 100 psi+?

Not a chemist I just follow directions on the box mix
(Hive Bee)
12-17-02 22:04
No 390302
      There are many bees already using this keg ...  Bookmark   

There are many bees already using this keg design. But they don't want to give up there secrets on how they managed to get it glass lined (enamel, as in appliance coatings) or how they went about approaching such a coatings company on why they want such a dispensing container cut open, modified, and re-welded. I just want to know how much the SS impedes the magnetic field on these and if a HD stirrer is required instead.