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Organikum
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I used a 150W halogen (about 7€ or so) with the glass removed and it worked just fine (toluene/TCCA).
I believe the cheapest lamps work best for they offer no kind of inbuildt UV protection.
[Edited on 31-5-2007 by Organikum]
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evil_lurker
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Toluene run #3
I had to abort this run after about 1/3rd a mole of TCCA was converted into CL2.
In it I used 600g of toluene and a 20K light w/ 1 g of hexamine added.
The result?
Fucking SNOW!!!!
I'm guessing that the hexamine absorbed the HCl formed, which became insoluble, and well the rest is history.
So, it would seem that hexamine is NOT a good catalyst and does not need to be used... or at least if it is used, in tiny tiny amounts.
[Edited on 11-6-2007 by evil_lurker]
Not all chemicals are bad. Without chemicals such as hydrogen and oxygen, for example, there would be no way to make water, a vital ingredient in
beer.
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evil_lurker
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After a complete tear down, rinsing, and oven drying cycle of all flask equipment Run #4 has begun.
The metal halide lamp is inufficiant to heat and react the flask at the same time. Therfore the floodlight was used as a heat source. I figure there
is in the neighborhood of some 40,000 lumens hitting the flask with about 20,000 being the correct spectrum to initiate the reaction you can see the
blue tint above.
Chlorine production seems to have stabilized for the moment, all the leaks are out of the system, and clouds of HCl are coming out the exhaust tube
and being blown off into the night by the exhaust fan.
All in all this run is looking very promising.
Not all chemicals are bad. Without chemicals such as hydrogen and oxygen, for example, there would be no way to make water, a vital ingredient in
beer.
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evil_lurker
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Success... the light works!!!
Run #3 started off with a standard 12 mole theoretical load. Using a 50-50 solution of HCl and water, approx 200mls was put into the reaction flask so
estimate that there was 10 moles of Cl2 left in the chlorine generator when run #4 was begun.
Run #4 initial charge was 613 grams of toluene and the weight of the contents of the flask had increased by a whopping 154g over the last run.
Provided that a mole of chlorine gas weighs in at @ about 35.5g, that means approx 4 moles of chlorine were absorbed and reacted...
Since I am unable to determine how much chlorine was in the initial charge, I am guessing that yields are in the 80% plus range based on chlorine
input.
The crude product will be distilled later today after I get a nap and the fraction boiling over the 170-180ºC range will be collected.
Not all chemicals are bad. Without chemicals such as hydrogen and oxygen, for example, there would be no way to make water, a vital ingredient in
beer.
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jimmyboy
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nice - i hope the yield was high..
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garage chemist
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I hope the toluene was distilled before use.
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evil_lurker
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| Quote: | Originally posted by garage chemist
I hope the toluene was distilled before use. |
It was straight out the freaking can.  I've distilled some out of the can
before, and its indeed 99%+ pure.
I'll probably break down start using distilled in the future, but I'm rather short on reagent storage bottles at the moment so it will just have to
wait till a later time.
Anyways, I distilled the crude reaction product. There was significant darkening which resulted in quite a bit of high boiling tarry material left in
the flask.
Total isolated yield was 374g of cystal clear material boiling between 174-182Cº or roughly 2.95 moles.
Not all chemicals are bad. Without chemicals such as hydrogen and oxygen, for example, there would be no way to make water, a vital ingredient in
beer.
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garage chemist
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Distillation is not necessary because the toluene is not pure enough, it is necessary because the can is made of iron. When iron is present in the
reaction, the aromatic nucleus will be chlorinated instead of the side chain, no matter if you irradiate with light or heat to boiling.
Lets hope there wasnt enough iron in there to completely screw up the reaction.
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evil_lurker
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There was definately some iron contamination due to darkening of the reaction mix and decomposition of the reaction product in the distilling flask..
however, this could be at least partially caused by the ceramic packing and reflux (I used a 250mm vacuum fractionating column) and large amounts of
residual HCl dissolved in the crude RP... I'm sure that distilling at atmospheric did not help things one bit either.
I do believe that I have benzyl chloride in rather decent purity as only about 30-40 ml or so came over between 150-174ºC (chlorotolune b.p.
160-162ºC, benzyl chloride b.p 179ºC).
The next batch I run will definatly be distilled prior to running, but as I said before I need some new reagent storage bottles.
Any suggestions for glassware cleaning?
Not all chemicals are bad. Without chemicals such as hydrogen and oxygen, for example, there would be no way to make water, a vital ingredient in
beer.
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