Author Topic: o2 is the shit  (Read 18788 times)

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FarQ

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Re: o2 is the shit
« Reply #20 on: October 14, 2000, 06:58:00 PM »
What is this vessel you speak of?
What is it's original purpose?
Please elaborate.

frost

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Re: o2 is the shit
« Reply #21 on: October 14, 2000, 07:17:00 PM »
it is a sprayer for chemicals it has a pump handle its black its made by hudson who made a teflon coated sprayer of this kind a year back which was pimp for o2 work also until the teflon coating wore off. its called the commando sprayer its withe the other sprayers at l***s swinf likes this one even better because of its endurall nonreactive epoxy inner liner only modifications it needs are clipping the inner tube and clamping an air hose on its outlet. it has a good enough seal to hold 80psi swim tested this for 6 hours soo far rock solid. it looks like it could bee the concorde of ghetto reactors!
when he gets through with his new high speed hotplate and robinater vaccum distilling imaginary ketone hes gonna give it a go.
btw the bottom is very flat and about 10 inches across good stir action!

chinacat

  • Guest
Re: o2 is the shit
« Reply #22 on: October 15, 2000, 11:19:00 AM »
As to the glass qstn./debate....mason jars..you can get them in many diferent sizes..they're cheap, and of course, made to withstand enormous pressures. Also come with hany-dandy metal vacume seals..somethign to think about I guess..I have always belonged to the Mason jar/snapple jar labware contingent myself,,,much easier to explain to nosy roomates..ect..
   But,,Frost..I'm intrigued, the Commando Sprayer??/.the Hell you say!...how much did it cost? Sounds very cool.

frost

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Re: o2 is the shit
« Reply #23 on: October 15, 2000, 02:42:00 PM »
28.50 + tax

scram

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Re: o2 is the shit
« Reply #24 on: October 15, 2000, 02:49:00 PM »
oK bro, I get jealous when my ideas get improved (I believe I'm the first to try to garden sprayers here). You gotta let me in on this since the garden sprayer I was using in March can not be found in my town anymore as it went to 90 psi and I'm sick of explosions with others at a mere 65psi. If you got a sprayer that is lined like you mention and the epoxy doesn't crack given the abnormally high pressures we are putting in these things then you have hit the bulls-eye with the whole problem KRZ has been talking about with using the wacker in SS (standard pump pressure is meant for ~20-40psi by the manufacturersi). This would be a revelation. You could do big ass oxidations in a 2gallon deal and with a flat bottom it could be kept to stay upright without have to use hook straps to contain it to the stir-plate. Cum-on guy, spill the beans (pun intended). If you can email me at jerryspringer@hushmail.com

scram

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Re: o2 is the shit
« Reply #25 on: October 15, 2000, 02:54:00 PM »
BTW, I have used a paint shaker and it worked very well in a 3 liter bottle. The only problem is that a paint shaker, despite weighing some 75+ lbs still tends to move around a concrete floor by itself given its jolting action. It also has to be reset every 15 minutes as this is the maximum timer limit. You can do 2 at once. It creates one hell of a soapy looking mix while in action. I broke the damn thing thoug. Fucking knob got stuck and it stayed on and the only way to turn it off was to unplug it. A real hassle and very noisy overall.

FarQ

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Re: o2 is the shit
« Reply #26 on: October 15, 2000, 03:12:00 PM »
Just bolt it to the concrete, very easy with masonry drill and a few ramset bolts. ANd its not permanent, just put in place and tighten down, remove when finished. If its not your house remove bolts as you leave. The timer should be taken out of the circuit and just controlled with a switch, also easily undertaken. But yes I imagine it would be quite loud in any normal living environment.


"ML"

scram

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Re: o2 is the shit
« Reply #27 on: October 15, 2000, 03:22:00 PM »
Excellent find frost. Will check this out. Let us know if its successful

http://www.hdhudson.com/catalog.html#Comando®


FarQ

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Re: o2 is the shit
« Reply #28 on: October 15, 2000, 03:37:00 PM »
That looks awesome, you will have to let us know how that goes, SWIM might get one sent over if they can't be found here.


"ML"

scram

  • Guest
Re: o2 is the shit
« Reply #29 on: October 15, 2000, 05:06:00 PM »
I just came back from the hardware store and took a look at this model. Frost if you look closely with a light you'll see the the epoxy coating tends to diminish just 2 inches from the top of the sprayer. It seems that additional epoxy (also avail at the same hardware store) would be needed to cover the upper inside lid area if the unit was laying on its side. Otherwise it looks good if your doing the oxidation with the unit standing upright. In fact the bottom is slightly bevelled with the apex of the bevel just reaching right at ground level. 3 boxes were opened and looked at, one of which you could see the run marks where the epoxy ran down the sides to the bottom and hardened. They had a display model that was up and when I took out the pump to that one it seemed as if it was a returned model that had be chemically abused inside. The epoxy was completely corroded off. I hope this doesn't happen for our useful purposes. If that epoxy is not strong enough there are several epoxy and "Appliance finishing" epoxies available at the same place. There must also be a way of somehow rigging a spray wand to allow the can to spray evenly inside the container without having to make it difficult. Man, let us know what that finish looks like once you wack the bitch!

frost

  • Guest
Re: o2 is the shit
« Reply #30 on: October 15, 2000, 06:34:00 PM »
frost was g'd out and had a very groovy dream, it was about this new find of his.he first clipped the tube in the pump with some angled blade steel cutters. then he clamped on a 3/4 inch welding hose. so it would work upright.then into the vessel went 150ml labgrade etoh, 1gpdcl2 goodstuff! prestirred for 2 hours then added 5gcucl dihydrate, 100ml fractionally distilled starting material premixed with 100ml meoh and 5 ml dh20, mixed for an hour sealed up and added 40 psi set regulater and let it run for 12 hours because of the lesser pressure (usually 45-60 psi) in a 70c room. with highspeed stirring and a 3in eggbar it stirred well.
the mix was extracted had a blackish green color and spelled spicy/sweet put in a 2liter sep and added 1ltr dh20 with 50ml hcl 37% the black oil fell out and was collected.
85ml of it swimfs dream was so real! so he tasted the stuff! it was the stuff he buchnered this 3x through celite, then mixed with 300ml tolene, that he had washed the aquous level with 150ml/2x then buchnered 2x
he noticed no tar in the workup and it was a nice reddsish color with a green yellow tint, he decided to skip any washes since it was a small amnt and already looked good.
this was fractionally distilled and after collecting the tolene 25ml peanut oil was added, and vaccum was attached.
approx 2ml forerun was collected and thrown out. then at 125c(strong vac) it began to flow and it was soo beautiful (you know how dreams can be) almost clear with a golden tint,
definately the stuff!
92 ml total!
too bad this was only a dream, noone can make mdp2p that otc! and the o2 dosent work without dmf and a shaker! this must bee true since only a few bees on the new board have done it, they must all be lying myself included! but i dident lie my dream was like that.
frost over and out!

FarQ

  • Guest
Re: o2 is the shit
« Reply #31 on: October 15, 2000, 07:05:00 PM »
If it needs to be re-epoxied then that sort of defeats the purpose, as one could just epoxy a better steel vessel that would be much safer and more practical for other applications as well.
The real test for this will be after several runs to see how the coating stands up.
The way frost does things I am sure we will have an answer within a couple of weeks.

Frost,
With that size base on the vessel. How big do you think you could scale up before stirring became in-effectual?


"ML"

frost

  • Guest
Re: o2 is the shit
« Reply #32 on: October 15, 2000, 07:22:00 PM »
i believe it depends on the stirring power of the hotplate some are srtonger than others with a strong one and removing the pump piece 1kg could be achieved with 4inch eggbar. and 1:2 safrole to solvent ratio with 60-80psi it could bee done! the coating held up in the dream but after many maybe just buy another?
frost :)

Osmium

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Re: o2 is the shit
« Reply #33 on: October 16, 2000, 04:13:00 AM »
1. Prestir the PdCl2 and CuCl2 together for a few hours.
2. No additional water needed in this reaction.
3. The poly versions (I guess the tank is made from PP)  are probably much cheaper and should work just as well.
4. It only works good for small batches, O2 absorption is too slow when you fill it to the top with the reactands.

KrZ

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Post deleted by KrZ
« Reply #34 on: October 16, 2000, 09:25:00 AM »

Fuchem

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Re: o2 is the shit
« Reply #35 on: October 16, 2000, 01:12:00 PM »
Take a sodakeg to an industrial finish house. Tell them you are working with high temp corrosives. Ask them about vitrified coatings (duraglas, quartzite, etc) it's not cheap, but not too expensive either. Tell them you are a chemical engineering student working on your masters project and you would appreciate any discounts they would provide or even offer to assist doing the shit work/prep work.


"To be the sum of all parts, in one place, at one time" - Andrew Graybeal

scram

  • Guest
Re: o2 is the shit
« Reply #36 on: October 16, 2000, 02:03:00 PM »
You nigga's are so Kool when I'm high!  This is going to be a kickass devise. KRZ, how much water do you think needs there to be per 100g oil? If your getting 80% yields, thats amazing. I'm only getting about 35% based on weight/weight but I can't say for sure that's correct since this is a very impure nondistilled product going into the al/hg which could be accounting for much lower yields due to impurity and a false impression of actual ketone content.

Osmium

  • Guest
Re: o2 is the shit
« Reply #37 on: October 16, 2000, 02:20:00 PM »
KrZ, read that 1969 ref again in case you still don't know it inside out  ;) . It clearly says that reducing the water content speeds up the reaction. Exactly my observation too.

If water was necessary for the reaction it would be necessary in molar amounts. Adding 5ml of H2O to a 100ml safrole reaction isn't even 0.5 mole. Maybe you can tell us why water is needed in the reaction at all. Everybody knows that the product of the MeOH Wacker is the ketal, which is hydrolysed in a few seconds, maybe minutes afterwards as soon as you quench the reaction with acidic water. If only a half a mole of water is present per mole of alkene you end up with some ketal or semiketal anyway, meaning you have to hydrolyse the rest during the workup. Now please show us where in your opinion during the Wacker reaction sequence water is needed. I don't know who came up with that BS idea that water is needed here. I did it without, all reagents of the highest grades available to me back when I did that experimentation, and guess what, it worked. With way less than 0.1mole of H2O/mole alkene.
But of course I live in Europe, the place where amine hydrochlorides are acidic (contrary to the meth board parallel universe, where amine hydrochlorides are neutral....). Maybe that explains it all.  ;)

Fuchem

  • Guest
Re: o2 is the shit
« Reply #38 on: October 16, 2000, 03:10:00 PM »

http://www.blome.com/ds220.htm


http://www.tycon.com/


http://www.indobase.com/web/aquadra.htm


http://business.vsnl.com/aquadra/products.htm

This lists the Fo-Poxy formulations.

http://business.vsnl.com/aquadra/coldweld.htm

More Fo-Poxy info.
Perhaps ceramic glaze could bee used. Pour it into container, slosh it about, pour out, toss into the oven. I don't know if a home oven is capable of the heat required. If not, bring it down to an industrial heat treating company and see if they will fire it for you. I've had a HT shop heat all manner of weird stuff for me. I've never had to pay. Just told them I'm a mad scientist and working on my mad scientists degree. Smaller stuff they throw in with one of their batches if it's the right temp, others they do a special run for me. The guys get a kick when they see me coming wondering what the hell I'm up to now. One of them calls me "the nutty professor".
Fuchem


"To be the sum of all parts, in one place, at one time" - Andrew Graybeal

frost

  • Guest
Re: o2 is the shit
« Reply #39 on: October 16, 2000, 04:29:00 PM »
osmium,
swinfs new to the organic chemistry thing, but he's learning at a fast rate, he's always added 5ml/100ml to the o2s if using something otc like heet won't there be a few mls of h2o present anyway? the reason he asks is when doing a nitro amination there has to be some h20 present to form the amine so isnt it coming from the meoh. ;D  also dident spiceboy from what he had learned from you use 5ml in his experiments or did he just add that on his own? i hear thar stirring won't work from your debate with KrZ on the oldboard, but spiceboy reported good results with the eggbar as well as KrZ. i'm assuming its  working because of the eggbar and the large flat area and only 200ml alcohol to 100ml safrole will force the o2 into the mix. if totally anhydrous conditions are used how fast would conversion occur at 45psi? this will bee tried next.also what causes the yellow oil phenomenon? the stuff that looks like ketone but will freeze, i used to get it alot at first. thought it was iso nut it would aminate(low yields) is it some kinda iso/ketal azeotrope it would come over at the same temp as ketone. this happened when using air and orbital shaker. and has happened only once with o2 and stirring.

thanks for the wisdom,
frost