Author Topic: o2 is the shit  (Read 21524 times)

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DiethylEtherMan

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Re: Let's look at the literature
« Reply #140 on: November 04, 2000, 11:41:00 PM »
Beaker: I believe that was intended for me, and anyone else who needs to know since earlier in this post someone stated the water bath temp for the reaction was at 55-60F. I sincerley appreciate the tip. Thanx!

Where can one go to find this literature (journal references...college library?...Online?) that you posted above. Of course, I am a newbee. As we speak...after 24 or so hours of stirring at 55-60F...temp was brought up to 50-55C and PSI set at 45. Thanx again. Will post back with results.

How much dH20 is added after the HCI addition? (I saw someone mention 3/4??? 3/4 of what?)

kpjr.

To be loved is to be fortunate, but to be hated is to achieve distinction. --> Minna Antrim


If some of us were not so far behind, the rest of you would not be so far ahead!


placebo

  • Guest
Re: Let's look at the literature
« Reply #141 on: November 05, 2000, 07:33:00 AM »
Ok, here is an old thread I had saved, it is quite interesting and gives another idea of KrZ's for a pressure vessel.
*Note... This was prior to the soda keg idea!

Author Topic: Ketone for lazy people
KrZ
Member posted 01-12-99 01:32 PM
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I'll have to admit I'm pretty slak when it comes to shaking a coke bottle so recently the R&D team here has developed this vessel which has yet to be fully tested.
The stuff we used;

1 ft long 10" diam piece of PVC pipe
2 end caps for PVC pipe
2 x 1/2" male-male brass connector
Tire valve
1/2" brass screw-on endcap
PVC pipe sealer
2 nuts to attach to the male-male connectors
Gasolia Soft-Set
Thread Sealant with Teflon
Tire Pressure Gauge
Tank of Welding O2
1/2" Hi-pressure hose with screw caps (3ft or so)
Elec. tape or whatever
4l beaker, stirbar, stirplate

Take the PVC end-cap and drill 2 1/2" holes and one hole big enough for the tire valve. Put some Gasolia on the male-male connectors and screw them into the 1/2" hole. Screw the nuts onto the connectors on the inside of the PVC caps. install the tire valve and use some gasket sealer to make sure its nice and tight.
Seal the untouched PVC endcap to the pipe with the PVC compound. Place the capped pipe on the stirplate. Slide the beaker inside of the pipe (if its loose put some paper towels in there to stablize it and don't make it a tight squeeze so its hard to get out either). Place your standard list of SRV reactants in the beaker. Drop the stirbar in. Smear the Gasolia on the inside of the other PVC cap. Place the cap on the pipe and pull up and down while twisting so you ensure a good wide seal between the cap and pipe. Make a full loop with the tape around the hole pipe just do be sure (I did it twice to make an X pattern on top/bottom). Screw the hose onto the tank and brass fitting. Attach the tire pressure valve (If you've got a regulator on your O2 tank this isn't necess.). Spray the O2 into it with the other connector open, this way it pushes the atmosp. out. Cap the other male-male connector using Gasolia. Pressurize it on up to 125 psi (thats as high as I took it but who knows). Turn the stirrer on and wait 2 hours or so... You get the picture...

Anyway, the device has been constructed and pressure tested, but no runs yet. I'm assuming you would need to give it 2 hours but it could be less considering the ridiculous amount of O2 we'll be cramming in there. Its certainly alot harder to make than an SRV but once you've got it setup I think it has some minor advantages, I'll provide an update on how it goes in action as soon as I can.

...and here is how it proceeded.

KrZ
Member posted 01-14-99 11:18 AM
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I'm going to redistill to make sure;
In the beaker went;
3.5 g PdCl2, 45g CuCl, 295 g Safrole, 875 ml DMF.

Pressurized it up to 120psi, let it stir with a heavy ass vortex for about 2 hours(so hard a large portion of the bottom of the beaker was exposed and @#%$ was way up on the sides). Extraction as usual. Distilled off the DCM and everything else coming over before 142C, then came a fraction at 148C weighed it at 8.6g, and another one at 152C weighed it at 285g. First fraction was yellowish and had an odor, second fraction had no odor and was yellow-light-greenish with no smell. Remember this vacuum pump is retarded, it pulls safrole over at 127. I also tried using the silicone glass-joint stuff to make a seal and it didn't hold as well as the gasolia (I could hear it leaking). The room it was done in was about 50F.

...and then...

KrZ
Member posted 01-17-99 10:57 AM
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I went to a local welding supply place, they had regulators that went up to 100, 125, 150 and various other levels (with increasing cost the higher it was rated for) the one I got goes up to 125, as you might have guessed. It was a pain in the ass finding an adaptor to get it to connect to the 300psi presssure hose I bought, it was a 5/16" size regulator and the hose was 3/8", apparently a very uncommon combination cuz I had to go 5/16->1/2->3/8 with brass adaptors to hook it up. I'm perfectly content at 125, I didn't wash the filter cake when drying,(What filter cake????..placebo) left ml's of oil here and there in beakers, and knocked over a 250ml beaker with some oil in it, so I believe actual yields were very high. The PVC I bought only came in a 10ft piece at a time (got funny looks from the counter guy when I wanted only 1 ft) so I've got a big piece sitting in my backyard. I'm going to get an ABS pipe before I do it again as it seems Beagle was quite right (after reading up on it). Trying to think of a way to fit a big rubber o-ring around the inside of the pipe and designing some latches for quick snap-on loading ;-) I'm pretty satisfied with all yields but, I want to get something real nice and take a pic. of it and upload it for you guys to see.
Amination is currently proceding under nitrogen using 300g of MeAm in just enough MeOH to dissolve it (you need to dissolve the MeAm in methanol first and it takes an hour or so of careful checking   addn. to get it perfectly saturated, which is important!). You don't need to waste a kg!! Just wait longer, check the pH and adjust accordingly, use heavy ass stirring and you'll get the same yields!!

For removable endcap.

TheCat
Member posted 01-20-99 10:16 PM
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KrZ, one more thing. Have you had anyone more dreams at high preasure? If you have how were the yeilds?
Also I was a thinking. You want a nicer looking presure vessel? Go to the plumbing store and ask for a "clean-out" for you 10" ABS or PVC pipe. What a clean-out is is a section of pipe that looks kinda like an end-to-end pipe coupler with a big ass threaded plug in one side (if you go ask for one you will know what I'm talking about). What you would do is put the regular end cap on one end then attach the clean-out to the other end and there you have it. A preasure vessel with a screw on cap.

A good point by Semtex...
Semtex Enigma
Member posted 01-22-99 08:59 PM
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Small correction/note: The purpose of a regulator in situation which you are describing is not correct. You see when a regulator(say 125psi) is hooked up to the O2 tank, all it is doing is regulating the flow of gas through the tube from the regulator at a maximum pressure of 125psi. It does not control the pressure in the vessel, only how fast the gas enters it. To get an accurate reading of the pressure inside the pipe one would have to equip the vessel with a gauge.
I once suggested a modified version of Piglet's proposed bubbler for the wacker. You see I think that bubbling under atmospheric pressure would be uneffective, however I have reason to belive that it would indeed work under increased pressure. I will try to write up an outline for those in the position to dream of such things. If anyone is interested please let me know...

Results...
KrZ
Member posted 01-23-99 12:03 AM
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It was about 80%, theres still some more rexytal. in the IPA now so I don't know exactly yet. I just waited a little longer, was very careful dissolving my MeAm to assure saturation, and I filled it with nitrogn and capped w. a ballon each time, I also checked and adjusted the pH with a digital meter every 6h. Other than that its all been said before...
I told the guy at the welding place I would be injecting N2 into soil for an Ag. Exp. involving ag. engineering; oxygen/nitrogenation injection cost analysis for farms, etc. he believed every word, he said I'd need a tank and regulator, then he produced a brass piece with two pressure gages and another steel piece that fit into it with a big plastic knob and another gag, he said just hook the flow regulator to the tank and the pres. regulator up to it. Thats what you get for welding standard set up right? If the flow reg. was just on there I suppose all 1000osi or whatever that tank is at would come across, boooom! I've been looking at these stainless stell compressed gas tanks MSC direct has, 4.7 gallon capacity one for ex., some welding to attach a mechanical stirrer would be needed for anything bigger but I think a big stirbar and some fine tuning of the plate to get max spin would do it for this size. Could form alot of ketone that way....

Some wise words from psychokitty...
psychokitty
posted 02-22-99 08:58 AM
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As for KrZ's set-up, I have a little bit of information to offer.
I spoke recently to a machinist who know something about pressurized canisters and he told me that PVC pipe fittings are pretty resistant to corrosion and could possibly hold up to using the reactants directly in the container itself. But since one can't be sure, it probably would be best to conduct solvent tests.

The pressure and temperature ratings of PVC can be found printed on the sides of the pipe so that should make it easier to determine how much of a beating it can stand.

I also asked about the danger of explosion and he said that more than likely, there would be no danger as long as the temperature and pressure of the reaction did not exceed the limitations of the pipe's design. HOWEVER, if the pipe was dropped -- not even from very high up -- it could very likely break causing the undesired aforementioned explosion. And BTW, it doesn't matter if it is ABS or PVC or whatever as the impact from the released air alone could cause serious injury.

As for the easy access issue, the ends of the piping could be threaded, or installed with a threading adapter.

KrZ: I must admit that I am confused as to why you use so much O2 pressure when you could easily get away with less. We all know that 30 pounds is effective at transforming the alkene to the ketone in alcohol solvent in 2 hours using just regular air! So why not simply start with a little over 30 pounds and once the oxygen gets used up and the pressure goes down (to just a little under thirty pounds), simply inject more oxygen until 30 pounds is reached again?

Just a thought.
--Psychokitty

What type of plastic pipe should I get?
dpHarma
Member posted 02-22-99 08:24 PM
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the pipe of choice is HDPE high density polyethylene.
a great deal of study has gone into plastic pipes used for launching pyrotechnic aerial shells. when a shell explodes in it's launching 'mortar', the total combustible material is comsumed at once (or nearly) and the forces are confined in the tube.
PVC and ABS shatter into many small sharp fragments. HDPE tends to deform first and producess much less shrapnel.

dpHarma

Hope this helps a bit?
I like it!




Wanna do the rumpy pump?




psychokitty

  • Guest
Re: Let's look at the literature
« Reply #142 on: November 05, 2000, 07:39:00 PM »
That proceedure seems like it would work -- a proceedure, mind you, that was offered by "respectable" KrZ, BEFORE he was supplanted by the "hallucinogenious".

Sheesh!  I wish KrZ was as concerned for my well-being as I was about his way back in the good old days.  If I knew then what I know today, I would have recommended that he amp the O2 pressure up to 300 Ibs -- just to see if he was keeping on his toes.

I'm through ranting.  But I do believe I'm going on a post-deleting binge. Maybe then I'll be as respected as KrZ is around here in New Hive.

--PK

placebo

  • Guest
Re: Let's look at the literature
« Reply #143 on: November 05, 2000, 10:12:00 PM »
Cool, and whatever posts you can't delete, we will make the board crash and have those posts lost forever. Ok?

Don't worry psychopussy, we will get to the bottom of this!

We are all in this together and we have nobody else to help us, so we might as well try and get along and work this shit out! (Fuck, now I sound like a god damn hippy! Fuckin love-everything E-tards!)

If not, then I shall just get fucked now and save you the time. K?

But anyway, there is some interesting info in my post above, something different to what is mentioned in this thread anyway. I really like KrZ's idea for rxn vessel. Any further word/comment on the PVC pipe vessel, KrZ?

Found it by accident in some old hive info I had saved a long time ago.


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placebo

  • Guest
Re: Let's look at the literature
« Reply #144 on: November 05, 2000, 10:47:00 PM »
I noticed this in Frost's original post...

thank you bees that have helped swinf work the bugs out of this. f-man, semetex


WTF is up with that?
Semtex, have you attepted this rxn yet and/or helped Frost at all? (I know you have followed it a long time, as have I, but any hands-on?)
...and WTF did FMAN do for him, somebody please tell me that?

...Oh and what's with Frost saying he set O2 pressure by reg. on tank and not by pressure in vessel. ...and if he ever returned, (As if he isn't already talking shit under a new name), we could ask him if he had any idea what was the total psi drop over 10 re-pressurisations. Me thinks nowhere near enough.

Personally, as much as I would love to believe him, I think he was/is and always has been full of shit, and I will stick by that till the day I see him do anything other then set geese free.

That is not to say I don't believe others here. Lets just say it is a general dis-trust and cynicism I have had about him since he arrived. I am not the first to feel this way about him, more like the 1754th actually. (the other 542 are cops) I am also wary of all others that converse, substantiate and claim to be "mates" with him!

Now KrZ, pull your fucking dummy out and tell us everything! You know I wuv you big boy!



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zooligan

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Re: Let's look at the literature
« Reply #145 on: November 06, 2000, 06:35:00 AM »

But anyway, there is some interesting info in my post above, something different to what is mentioned in this thread anyway.



You mean the solvent??


placebo

  • Guest
Re: Let's look at the literature
« Reply #146 on: November 06, 2000, 06:47:00 AM »
O2 pressure.
Type of vessel.



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zooligan

  • Guest
Re: Let's look at the literature
« Reply #147 on: November 06, 2000, 07:35:00 AM »
Yeah, that's a lot more O2.  This thred's so long now I couldn't find it, but didn't someone mention a set up like this in which you put a glass container inside another (more durable) container and pressurize the outer container??

Solvent is different than what has been talked about so far no?  Everything up to this point has been alcohol, not DMF, right?

z

placebo

  • Guest
Re: Let's look at the literature
« Reply #148 on: November 06, 2000, 07:50:00 AM »
Yeah its a pretty old thread, methanol and IPA were later developments.
Osmium's was with denatured I think.

The vessel, yeah the concept of something like it has been discussed, I just thought the PVC pipe was a good idea that hadn't been mentioned.


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KrZ

  • Guest
Re: Let's look at the literature
« Reply #149 on: November 06, 2000, 07:56:00 AM »
It certainly holds up to the pressure well.

Precursor2112

  • Guest
Re: o2 is the shit
« Reply #150 on: November 06, 2000, 09:12:00 AM »
Son of a Bitch!

Cold Fusion comes to Roll Makin!

O2 works!!!!

The O2 WORKS

the Coke bottle works...

39ml from 75ml of safrole.


sYnThOmAtIc

  • Guest
Re: Let's look at the literature
« Reply #151 on: November 06, 2000, 09:16:00 AM »
I read an article in mother earth news not too long ago about building a vacuum/pressure vessel out of pvc seems like it would work. SWIK will go to HDS adn get stuff to build one and give results on pressure hold. But SWIK has recently bought a four quart stainless pressure canner he plans on giving a try. Fits perfectly into paint shaker :)

KrZ

  • Guest
Re: Let's look at the literature
« Reply #152 on: November 06, 2000, 09:19:00 AM »
You better coat it with glass if you hope to get it to work.

zooligan

  • Guest
Re: Let's look at the literature
« Reply #153 on: November 06, 2000, 10:45:00 AM »
What about epoxy or teflon paint?

Semtex

  • Guest
Re: Let's look at the literature
« Reply #154 on: November 06, 2000, 06:15:00 PM »
All the experience that SWIM had with this rxn happened a WHILE ago, long before our queen bee departed.  I've discussed it with frost, and perhaps some of the things I've told him helped him out somewhat...?  I don't really know, you'd have to ask him about it...


::)  ::)

placebo

  • Guest
Re: Let's look at the literature
« Reply #155 on: November 06, 2000, 10:03:00 PM »
He has gone and returned under a new name, I am sure you will pick who it is pretty easily. Gee, wonder why? Coz he's full of shit!


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KrZ

  • Guest
Re: Let's look at the literature
« Reply #156 on: November 07, 2000, 11:31:00 AM »
3.24g PdCl2
32.40g CuCl2•2H2O
324.36g Safrole
70mL H2O
500mL DMF

Placed everything except the safrole in a 4L reactor, stirred heavily exposed to atmosphere for 4 hours.  Added safrole, removed atmosphere with vacuum. Pressurized to 35 psi O2.

Pressure drop (psi)   Time after Last Drop (minutes)
15            17
15            18
15            20
15            20
15            29
15             38
~4            30

Total Reaction Time: 172 Minutes

Added 500 mL 5% HCl solution
Seperated precipitated Ketone/Aldehyde
Extracted 3x 100mL DCM
Pooled extracts
Wash 2x 300mL Saturated Sodium Bicarbonate solution
Wash 1x 400mL dH2O
Wash 1x 400mL Brine Solution
Dried Extracts with 50g Na2SO4 for 45 minutes
Filtered to Remove Na2SO4
Vacuum Distilled at ~2.0mm Hg to recover 311.22g Piperonylacetone fraction 105-114C.  Isosafrole forerun, minimal high bp/polymerzied glop after 114C.
Molar % Yield: 81%



placebo

  • Guest
Re: Let's look at the literature
« Reply #157 on: November 07, 2000, 12:42:00 PM »
Temp please?


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KrZ

  • Guest
Re: Let's look at the literature
« Reply #158 on: November 07, 2000, 12:43:00 PM »
Room temp. 65F According to the wall thermometor.

Antibody2

  • Guest
Re: Let's look at the literature
« Reply #159 on: November 07, 2000, 12:52:00 PM »
Cool. Why the switch to DMF? How big was the stirbar?
Thanx


I’m gonna die when it’s my time to die. I’m gonna live my life the way I want to!