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Ozonelabs
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Parr Shaker Hydrogenator
Hello everyone.
At Ozonelabs, having recently sourced pure, pressurised Hydrogen as well as an appropriately priced Hydrogenation catalyst we are searching for a
Shaking Parr Hydrogenator.
Should anyone happen to have one that is in full working order for sale please do personal message us!
We seem to recall having seen (perhaps by Sauron) these offered on this board in the past...
Thankyou in advance for any replies.
Ozonelabs
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chemrox
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I got the one Sauron posted about and am delighted with it. The vendor is no longer in business; a victim of the 'free market economy.' I have Pd/C
and nothing else but am going to use Rainy Ni some day (a Rainy day?) soon.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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Sauron
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Actually the vendor IS still in business, just under another name, This is the 4th name change in the decade I have been doing business with these
people. The proprietor is Larry Turner in Muskeegon, MI. Used to be Turner Technologies, then WestShore Tech, then Surplus Labs, now Waters Edge.
AFAIK same location.
As chemrox knows I had a dispute with one of their staffers, and quit doing business with them. That was shortly after chemrox bought that Parr
shaker. I goy own Parr shaker from someone else but my Parr autoclave from Larry Turner and a whole lot of other stuff.
They terminated the woman who gave me a problem. But I have not bought from them since.
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stoichiometric_steve
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i need one, too!
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chemrox
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Maybe you should give him another shot. It can take awhile to get rid of a bad apple. I had a guy hassling all my other employees (when I had an
environmental shop). Reminds me of one of the mods here. I got rid of him but it took ahwile to get wise to it all and I tried to rehabilitate him
for both our sakes. Could you offfer a little more detail on how to get hold of the guy? Is it "Waters Edge" now? The old phone # died... I learned
that.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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Sauron
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Try Waters Edge Surplus in Google.
http://watersedgesurplus.com/index.aspx
I am still on their spam list but I always delete it so I do not have the details, sorry. I no longer have warehouse and transshipping facility in USA
as my friend closed his business. So I won't be buying much in US I'm afraid, as it would have to be shipped piecemeal and that is too costly.
Anyway all my funds are going into the fume hood purchase this year.
Once I get past that, we will see.
A moment of googling got me:
CONTACT US
Waters Edge Surplus
P.O. Box 626
Grand Haven Mi 49417
Phone: 231-955-0038
sales@watersedgesurplus.com
buying@watersedgesurplus.com
http://watersedgesurplus.com/index.aspx
Another reliable lab equpment supplier is Mike Hnatow of HiTechTrader
Http://www.hitechtrader.com
However, their Parr shakers tend to be pricey. At least compared to the ones that chemrox and I have obtained in the past.
If you want a bargain, monitor labx and ebay and look for something in the $500 range.
If you need one now, look at Mike's site, they are in the $2000 and up category.
I got a bargain on mine but then changed the motor out for 220V, added a mantle, pressure bottle and some hardware, and now have maybe $3000 tied up,
the motor from Parr, a GE, was costly. If you are in USA you will not have to do this but you always have to get little bits and pieces. I have yet
to ever see one of these come with the bottle, and treyc are usually missing the shield.
The larger model is the best, but rarely turns up. What I have is limited to 500 ml with a working capacity 2/3 of that.
[Edited on 21-2-2009 by Sauron]
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Sauron
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Slightly off topic, but it's an auction for a Parr temperature controller and allegedly a 4521 reactor.
However it is obvious from the photo that the "reactor" is merely the baseplace and mantle for a 4522 2 liter reactor. No stirrer, no motor, no
autoclave, and the seller wants an opening bid of $6100! He has stuck a flask on top to try to pass this off as an ordinary mantle. But ever see an
ordinary mantle and controller priced used for $6000+?
I have dealt with this seller and less said about him the better.
While I would like to have the mantle, it is worth about 1/10th of asking price. I already have the controller.
It is always best to know more than the seller does and it is a mistake to educate him.
[Edited on 21-2-2009 by Sauron]
[Edited on 21-2-2009 by Sauron]
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stoichiometric_steve
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i can get a new 700ml one complete with stirrer heater etc. for about 3500 EUR.
| Quote: | Originally posted by Sauron
Slightly off topic, but it's an auction for a Parr temperature controller and allegedly a 4521 reactor.
However it is obvious from the photo that the "reactor" is merely the baseplace and mantle for a 4522 2 liter reactor. No stirrer, no motor, no
autoclave, and the seller wants an opening bid of $6100! He has stuck a flask on top to try to pass this off as an ordinary mantle. But ever see an
ordinary mantle and controller priced used for $6000+?
I have dealt with this seller and less said about him the better.
While I would like to have the mantle, it is worth about 1/10th of asking price. I already have the controller.
It is always best to know more than the seller does and it is a mistake to educate him.
[Edited on 21-2-2009 by Sauron]
[Edited on 21-2-2009 by Sauron] |
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Sauron
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I have a complete 1000 ml Parr 4521 and controller and paid $2000 for it.
The money is in the pressure vessel, all else is ancillary.
[Edited on 21-2-2009 by Sauron]
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stoichiometric_steve
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sell it to me, you dont use it for the right things anyways! 
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Sauron
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Well, if I ever were to sell it I will give you first shot at it. But I have plans for it.
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zed
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Ummm. There was a Parr unit at auction on e-bay a few months ago, and it was located near me. I was tempted, but I passed on it. I could have
obtained it for less than $100 U.S., but balked. I have better stuff laying around, if I ever get the notion, and to my way of thinking, the classic
"shaker" design is clunky and less than efficient.
For those of you that don't have a unit, I recently came across some simple plans for quickly assembling a usable machine at very low cost.
Hopefully, the following link will take you there.
http://springerlink.metapress.com/content/l38433856746r7u2/f...
[Edited on 28-3-2009 by zed]
[Edited on 28-3-2009 by zed]
[Edited on 28-3-2009 by zed]
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Sauron
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That document has been available on Rhodium for many years.
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zed
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Yup! It has indeed, you are correct, yet somehow I missed it on Rhodium. I accessed the document via the UC Berkeley, Chemistry Library, online.
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Sauron
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That unit is designed for 250 ml Parr bottles, which have a working capacity of max 150 ml. While scaling the design up to 500 ml is not too
difficult, I found that trying to do same for the 2.2 L Parr bottle was not practical.
Besides, you still need the hydrogen storage, gauging and delivery subsystem as it would not be prudent to connect this apparatus directly to the
regulator of a H2 tank.All in all an autoclave is better. The performance envelope of the glass shaker bottles, in terms of psig and temp, is quite
limiting.
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zed
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All true. The Pressure Reactor is far superior. And, it isn't limited to low pressure, low temperature hydrogenation. It can do almost anything, is
very durable, and used units aren't prohibitively expensive.
As I recall, it can even be used to manufacture LiAlH4. Not a commonly required reagent, but sometimes you need it and nothing else will do. What
the Parr unit can't reduce, the LiAlH4 can.
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Sauron
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Making LAH is easy if you can obtain or make LiH
With LiH and anhydrous AlCl3, LAH is easy and does not require an autoclave.
If you mean use the Parr to make the lithium hydride then you are probably right.
The downside of used SS pressure reactors is possible catalyst poisoning. If so then only fix is a new vessel, head and all wetted partts and that is
expensive.
I have a 1 liter Parr stirred reactor and its controller as well as a 3911 shaker 500 ml setup. They are both useful.
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Magpie
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Sauron says:
| Quote: |
Besides, you still need the hydrogen storage, gauging and delivery subsystem as it would not be prudent to connect this apparatus directly to the
regulator of a H2 tank.
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I'm curious as to what exactly you mean here? Do you mean that you need some type of backflow prevention like a check valve or surge vessel? Please
explain.
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chemrox
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go to the Parr web site and dl the manual. Parr 3911 medium pressure shakers have a built in tank. A H2 tank fills that through the plumbing and a
regulator. I was fortunate enough to get a controller, heating mantle and H2 regulator with mine.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
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Sauron
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Chemrox and I apparently have people at a disadvantage because we both own Parr shakers.
http://www.parrinst.com/default.cfm?Page_ID=241
To access manuals and sales literature you have to register with Parr and login.
Yes they have a built in tank 1 liter with valves and gauges in and out and the connecting hoses to go to the inlet of the pressure bottle and to the
main H2 tank.
With the outlet valbe of the secondary tank closed you charge the tank with H2 to not more than 100 psig then you close input valve. You now have a
liter of H2 @100 psi and you can calculate if that is enough for your reaction. If so you can shut the regulator on main tank and disconnect the hose
and remove tank to its normal location as a safety measure.
For details on how to conduct the reduction see Parr manuals and also Org.Syn. original writeup by Roger Adams, the prototype shaker he designed is
very little different from the commercial Parr model based on it.
If you only do smaller scale reductions you can replace the 1 L tank with a 200 ml one, limit is still 100 psig. Limit of the glass bottles is 40-60
psig depending on sisze and temperature.
Optional accessories
Heating mantle
Controller for mantle, displays output of t/c
Cooling jacket - some reductions are exothermic
Thermouple
[Edited on 30-3-2009 by Sauron]
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Magpie
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Yes, I see the equipment layout for the Parr shaker hydrogenator. But for the UC Berkeley knock-off it seems that all that would be required is a H2
cylinder and a regulator w/valve and gauges. Of course connecting tubing and a teed vent valve would also be needed, as shown in the UC Berkeley
literature.
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Sauron
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Most catalytic hydrogenations involve some risk of fire and explosion because of the pyrophoricity of the various catalysts.
Part of the acculturation of a chemistry student is to teach the proper manipulation of the catalyst.
Look at what is on or at the bench:\
A pressurized cylinder of flammable H2
Flammable solvent and substrate
Highly pyrophoric catalyst.
It always has seemed to me, in the 35-40 years since I first read Roger Adams' writeup on this apparatus in Org.Syn., that the smaller lower pressure
tank was there to allow the main H2 tank to be gotten well out of the hazard zone. A 1 L tank at <100 psi would be dramatic enough is things went
wrong. A full sized cylinder at 3000 psi would be a catastrophe.
Bypassing the subsystem is not a prudent idea.
What UC Berkeley knockoff? The stirred unit described in the paperposted by zed is from Cal State San Bernardino. Not even Northern California!
[Edited on 31-3-2009 by Sauron]
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Magpie
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Although my experience with catalytic hydrogenation is very limited I can appreciate the hazards. I was simply amazed to see some Pd/C soaked in H2
burst into flame when exposed to the atmosphere.
Yes, I had my California institutions confused. I just scrolled up to one of zed's posts. I do know where San Berdo is as I was stationed nearby
compliments of the USAF.
To address this hazard you can locate the 3000 psi H2 tank anywhere that you want, say in the next room behind a concrete block wall. It's just a
matter of running a long enough tube to reach the Parr bottle. It looks like the Parr shaker is using a PE tube; if so, that would be easy enough.
I do see that by having its own local supply tank the shaker becomes quite portable, however.
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Sauron
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Remember, for small runs, the 200 ml tank is even safer.
The shaker is larger and heavier than it looks. The motor is quite heavy and altogether it is a pain in the ass to move from one bench to another.
Even more so from one room to another. I would recommend a wheeled cart for such jobs. I would say, operate it on the cart, but IMO inside the hood is
the best place.
H2 tanks are often actually 5000 psi and special regulators are beeded if you need to deliver H2 to an autoclave (not a shaker) at 1000-1500 psi - in
comparison to the low pressure delivery to charge the smaller tanks of the shaker.
The sequence of opening and closing the regulator and valves ought to be pretty obvious. When filling the small tank you set the regulator to no more
than 100 psig and open inlet valve while outlet valve is closed. When inlet valve reads the desired pressure, never more than 100 psig, close inlet
valve and close regulator.
Prior to working with H2 you really need to test the enrire system end to end for leaks using N2 or Ar. Do not use compressed air as you will want to
purge O2.
I attach the original Adams peper from Org.Syn. which describes the complete procedure on an apparatus very akin to the Parr and from which the Parr
was developed with Adams' involvement.
[Edited on 31-3-2009 by Sauron]
Attachment: Adams.pdf (157kB)
This file has been downloaded 1160 times
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zed
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Actually, I was referring to LiAlH4 synthesis via Heat/Pressure/Li+Al+2H2+THF.
I've always thought it is wasteful to use 4 moles of LiH to produce 1 mole of LiAlH4.
But, I digress. The subject is Parr shakers. Easy to build they are.
Not my cup of tea, but I have had several friends that built their own. Not much to it really, and the finished units worked quite well.
Overall, I'd prefer to entrain my H2 by stirring. And, I saw an interesting stirrer patent yesterday. I don't know if the units are commercially
available. Heck, I don't know if they are likely to work. Have any of you seen such devices? http://patapsco.nist.gov/TS/220/sharedpatent/pdf/6585405.pdf
[Edited on 31-3-2009 by zed]
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