10-02-03 11:34
No 462258
Hi!
I'd really like some 5-6 N hydrochloride in 2-propanol(or other suitable solvent), and gassing is no fun. I was thinking if it would be possible to simply mix 35% hydrochloric acid with IPA untill, say 50% above, 5-6 N is reached. After than one could dry the IPA with anhydr. sodium sulfate or molecular sieves. Is this possible, or will all of the hydrogenchloride be sucked up as well, rendering the IPA nearly netral?
Regards
Bandil
I just love the smell of bromine in the morning!
(Chief Bee)
10-02-03 17:04
No 462286
will all of the hydrogenchloride be sucked up as well
I believe much of it will be adsorbed to the drying agent. Gassing is probably the best way to do it.
(you can always take some more)
10-03-03 15:26
No 462382
Rhodium>
If you look here (../rhodium /equipm
Isn't the method i mentioned actually just an in-situ version of that method? The HCl gas is released, but redissolved immediately in the IPA? If we calculate, that we'll get a 40% yield as they report, dissolved in the IPA; what what would in theory differ from doing it in-situ?
Regards
Bandil
I just love the smell of bromine in the morning!
(Chief Bee)
10-03-03 16:35
No 462399
In the text they use 1:1 CaCl2/35%HCl which is a lot of drying agent, and CaCl2 binds water more strongly than for example Na2SO4. The resulting mush will also be far from "anhydrous", as the CaCl2 only binds enough water to prevent the solution from dissolving as much HCl as it did before. Also, you cannot use CaCl2/35%HCl in IPA as that will produce 2-chloropropane.
To make anhydrous HCl you also need to bubble it through H2SO4 or something after it exits the generator, as it will still carry over water vapor.
(you can always take some more)
10-03-03 17:38
No 462403
Thanks Rhodium, i see you'r point!
I suppose, there's no way out of just gassing. *sigh*
While we are at the subject; do you(or anyone else), know what the maxiumum obtainable concentration in IPA or ether is?
Regards
Bandil
I just love the smell of bromine in the morning!
(Hive Adickt)
10-03-03 18:06
No 462407
I's around 5M. Personal I drip HCl(aq) into 96% Sulfuric accid wit a press.equ. adding funel. The the gas escape throug the top (and my stopper) throug a washbottle and over in my cold stirred ether. I them dry the ether with MgSO4. Stabel for years.
(Stranger)
10-04-03 00:56
No 462455
Rhodium
The gassing technique using CaCl2/35%HCL may not work in IPA, but it works in Xylene/Toluene, right? Also, the ratio of CaCl2 to HCL is 1:1 by weight or volume?
(Chief Bee)
10-04-03 20:27
No 462589
abuse: No, it will not work to dump CaCl2/HCl directly into toluene, as it will not be anhydrous anyway. The ratio is by weight, read the *entire* document linked by bandil above.
Hest: What kind of losses are you experiencing by drying the ether over MgSO4 (instead of drying the gas in-line), and how do you determine the strength of the solution?
(Stranger)
10-04-03 23:44
No 462626
Rhode
Actually, what I meant was to use the HCL gas liberated from reacting CaCl2 with %35HCL. There was a post regarding this technique and how is was superior to the H2SO4 method, but what do I know...
(Hive Adickt)
10-05-03 16:35
No 462728
[quote]What kind of losses are you experiencing by drying the ether over MgSO4 (instead of drying the gas in-line)[ I find it easyer than drying the gas line, that's all, usual the etherr will contain some % wather.
For the strength part i mix 10mL ether with 100mL wather, stirr well and titrate the mixture with 1M NaOH and phenolphtaline.