10-03-02 14:59
No 363894
Well,built a shaker table for this one.Has a 3 inch stroke,180 strokes a minute or 3 per second.Geared down a motor from 1725 rpm,converted rotary motion to linear with crank/rod.
Used 2g PdCl2,10g CuCl2,500g MeOH and 150 g crystal clear sparkly double distilled safrole.Premixed Pd with half MeOH for 2 hours.Premixed all others idividually for 10 minutes and dumped into standard 2 litre pop bottle vessel.Pressurized with O2 from a tank.Sessions were 12 minutes,purge and re pressurize with O2.Coffee colour.First hour,pressure drop 2 psi per session,after an hour or so the colour went a bit olivey and she started gobbling 3.5 to 4 psi per session.Left for 2 hours, came back and psi drop of 9.Did a fewe more sessions, 3 to 4 psi drop, then time for bed. Overnight 8 hours she dropped 19 psi and started looking a bit burgundy.Over the day got more burgundy and then darker,and started smelling sweet..actually quite a nice smell. .O2 consumption dropped ,exteneded sessions to half hour of Shaking With Extreme Prejudice and psi would drop only 1.5 or 2. Jesus what a hungry bitch.Figured she was done.Total SWEP 12 hours.Sitting 11 hours.Total psi drop 170 psi,assume some leakage per gauge check..so 160 or so psi drop.Interesting psi did not seem to make a difference..do 40 psi and would drop 3 psi,next session 32 psi and would drop 3 psi.At the end it looked just like cherry cola, c-o-l-a cola ;)
Dumped into 1 l d H2O, turned to hot chocolate with little burgundy swirls.146 grams of red,very red,I mean Ferrari red oil dropped out.Dropped G D sep flask so use the funnel trick/finger stopper.Washed alcohol twice with 150 g toluene,mixed with oil, and washed oil/ toluene 2 X 250 g H2O.H2O took up some chocolate.Dumped in 150 g peanut oil,Distiiled under vac toluene and mix went back to cherry cola.Forgot to grab a bit of oil to see if reacted with bisulphite.Put in freezer and head to bed. Will report on Pd recovery and results in couple days.If it doesn't work don't care about saf,just happy to get Pd back.Any comments critiques questions?? Want to try Ritter's? IPA .
Piece of advice don't buy digital LCD pressure gauge..methanol vapour gets in and absolutely melts the shit out of it.Took her apart and looks like was stuck in an oven
(Chief Bee)
10-03-02 15:05
No 363896
Dumped in 150 g peanut oil,Distiiled under vac toluene and mix went back to cherry cola.Forgot to grab a bit of oil to see if reacted with bisulphite.Put in freezer and head to bed. Will report on Pd recovery and results in couple days.If it doesn't work don't care about saf,just happy to get Pd back.Any comments critiques questions?? Want to try Ritter's? IPA .
Have you ever tried sentence structuring? Or easy conceptualization of the ideas you are voicing?
What was your intention with the post? You described what you did (badly), but didn't report yields, boiling point, identity of product etc.
(not quite as irritable lately)
10-03-02 23:28
No 364110
I agree with Rhodium, this could have been an interesting post.
Shall we assume english is not his native tongue?
Here's a quick re-hash...
Built a shaker on a table. It has a 3 inch stroke, 180 strokes a minute or 3 per second. I geared down a motor from 1725 rpm,converted rotary motion to linear with crank/rod.
I Used
2g PdCl2,
10g CuCl2,
500g MeOH and
150g crystal clear, double distilled safrole.
Premixed Pd with half MeOH for 2 hours. Premixed all others idividually for 10 minutes and dumped into standard 2 litre pop bottle vessel. Pressurized with O2 from a tank. Sessions were 12 minutes, purge and re pressurize with O2. Coffee colour.
First hour, pressure drop 2 psi per session, after an hour or so the colour went a bit olivey and she started gobbling 3.5 to 4 psi per session. Left for 2 hours, came back and psi drop of 9. Did a few more sessions, 3 to 4 psi drop, then time for bed.
Overnight 8 hours later. it dropped 19 psi and started looking a bit burgundy. Over the day it got more burgundy and then darker, and started smelling sweet..actually quite a nice smell. .O2 consumption dropped, extended sessions to half hour of Shaking With Extreme Prejudice and psi would drop only 1.5 or 2. Jesus what a hungry bitch. Figured she was done.
Total SWEP 12 hours. Sitting 11 hours. Total psi drop 170 psi, assume some leakage per gauge check..so 160 or so psi drop. Interesting psi did not seem to make a difference.. did 40 psi and would drop 3 psi, next session 32 psi and would drop 3 psi. At the end it looked just like cherry cola, c-o-l-a cola ;)
Dumped into 1L dH2O, turned to hot chocolate with little burgundy swirls. 146 grams of red, very red, I mean Ferrari red oil dropped out. Dropped G D sep flask so use the funnel trick, finger stopper. Washed alcohol twice with 150 g toluene, mixed with oil, and washed oil/toluene 2 X 250gm H2O. H2O took up some chocolate. Dumped in 150 g peanut oil, Distiiled under vac, toluene and mix went back to cherry cola. Forgot to grab a bit of oil to see if it reacted with bisulphite. Put in freezer and went to bed.
Will report on Pd recovery and results in couple days. If it doesn't work I don't care about saf, just happy to get Pd back.
Any comments critiques questions?? Want to try Ritter's? IPA .
Piece of advice don't buy digital LCD pressure gauge.. methanol vapour gets in and absolutely melts the shit out of it.Took her apart and looks like was stuck in an oven.
(Stranger)
10-04-02 11:16
No 364255
My apologies for not being overly verbose, as I had very little time to type in my accomplishment.Perhaps I should have waited until the necessary time was available to properly explain my procedure..I erred,forgive me .As well, you may notice I said that I would report back fully when complete.And to fully describe my device would take much time and space.I had only distilled off the toluene,and felt that to report it's boiling point would have been moot.Than I went to bed.
Next afternoon I got to the oil distillation.
The results that you may or may not be interested in:on my vacuum,safrole boils at 155 C.Had a few drops of safrole,then at 175 to 180 C recovered 115 grams of pale yellow ketone smelling oil.Used sodium bisulphite to test for the presence of ketone and it coagulated up quickly and perfectly.Then,as time permitted,the water and alcohol was boiled off to recover palladium chloride and a little unidentified junk to be separated at a later date.
(Hive Bee)
10-04-02 23:00
No 364427
If safrole boils at 155, ketone boils at 195-200. What kind of pump are you using? Of course, this is a completely different rxn, but the best solvent for the alkyl nitrite wacker is methanol. My guess is that the rate will be slower with IPA as solvent. Try it, though. Kinetics are a bitch to predict.
If you only recovered 115 g of ketone and a few drops of safrole, you are losing about 40 g of oil somewhere. You say you recovered 146 g oil. You probably had a lot of crap left over in your distillation flask (polymerized ketone). Get a better pump and you'll recover all of it but a few grams. Also, don't you so much fucking peanut oil! If you know anything about thermodynamics, this causes insane boiling point elevation. For that amount of oil, I use about 10 g of safflower (or peanut) oil.
To determine how much of the pressure drop what due to leakage, run the exact same experiment with only methanol in the bottle to see how much leaks out.
(Newbee)
10-05-02 07:49
No 364618
Didn't your solution get red hot? I've had 2 explosions last weekend due to this using 1g/100g ratios catylist/oil. I can only imagine your srv had to get super hot. Probably within the first 3 hours at those ratios. Are you cooling the srv or something? Because the 2 explosion here both occurred at just under 25 psi at the apex of the temperature climb. It must have got at least 55c. So, what did you do - keep it cool to keep it from exploding or did it not just turn exothermic at all(?)? BTW, the best yields have always resulted from running it as hot at possible. Also, those 2litre pop bottles hold ~9.5 grams 02 at 45 psi with ~340ml liquid in them (if you sqeeze all atmosph air out first).
(Stranger)
10-05-02 11:55
No 364683
I will not use so much peanut oil next time.My vacuum pump is a Gast rotary vane,on the gauge around 26 to 26.6 "Hg.
And yes, there is more ketone in the flask as I can smell it.I have other things to get to this weekend,so I plan on getting the rest out within a few days.
(Stranger)
10-05-02 12:02
No 364687
My reaction did get exothermic.I did not measure the temperature but it always felt warm to the touch.Once the absorption of oxygen slowed,it was cool-as could be expected.One thing that may help is that my basement is fairly cool.As for your explosions,sorry to hear but I don't know what I'm doing right or wrong.Perhaps it is the fact that my pressures are not so high?Will be trying another one fairly soon and will keep closer track of it.This first one was just to see what happened.
Also lab_bitch: the drop in pressure when checking with the gauge is minimal,perhaps 1/2 psi.
(Hive Bee)
10-05-02 23:36
No 364966
No offense, but your vacuum pump sucks. You are only pulling around 100 torr, and that is by no means sufficient to distill ketone. Get a fridge service pump. They are very easy to aquire and pull down to 0.025 torr.
(Stranger)
10-08-02 14:50
No 366204
exothermic
This swim uses only O2 wacker reaction. (its a karma thing)
In all the dreams pdcl cupric chloride remained pretty much near abient with heat needing to be applied to get any thermic reaction.
Yet this one never dreams above 50gm Olefin at a time so my views are tainted in the small field.
"Sometimes I sits and thinks, and sometimes I just sits." Satchel Paige