Organikum - 24-11-2004 at 05:11
The Ullmann writes that styrene can be separated/purified by complexing it with coppersalts.
Does anybody know which salts are usable and in special how the styrene is freed again?
Distillation of styrene under STP leads to bad losses from polymerisation, so this would be a nice method for pure styrene for those without a good
source of vacuum.
Any help welcome.
vulture - 24-11-2004 at 09:39
An equilibrium constant would be nice, so that we can compare it with other ligands.
But I'm pretty sure strong ligands like NH3 should displace it.
Ref: Styrene Coppersalts Separation
solo - 24-11-2004 at 11:54
Organikum Here is a nice article on ligans and cooper complexes which may have some assistance in your
quest.....solo
get it here.........Cooper
___________________________________________
Copper 1996
Diane R. Smith
Coordination Chemistry Reviews
172 (1998) 457–573
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 458
2. Copper(I) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 458
2.1. Mononuclear complexes with macrocyclic ligands . . . . . . . . . . . . . . . . . . . . . . . 458
2.2. Mononuclear complexes with acyclic ligands . . . . . . . . . . . . . . . . . . . . . . . . . . 461
2.3. Dinuclear complexes with macrocyclic ligands . . . . . . . . . . . . . . . . . . . . . . . . . 470
2.4. Dinuclear complexes with acyclic ligands . . . . . . . . . . . . . . . . . . . . . . . . . . . . 473
2.5. Tetranuclear complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 476
2.6. Cluster complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 477
2.7. Polymeric complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 478
2.8. Supramolecular complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 484
3. Copper(II) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 488
3.1. Mononuclear complexes with macrocyclic ligands . . . . . . . . . . . . . . . . . . . . . . . 488
3.2. Mononuclear complexes with acyclic ligands . . . . . . . . . . . . . . . . . . . . . . . . . . 499
3.2.1. Nitrogen coordination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 499
3.2.2. Oxygen coordination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 512
3.2.3. Nitrogen and oxygen coordination . . . . . . . . . . . . . . . . . . . . . . . . . . . . 513
3.2.4. Nitrogen and oxygen coordination . . . . . . . . . . . . . . . . . . . . . . . . . . . . 523
3.3. Dinuclear complexes with macrocyclic ligands . . . . . . . . . . . . . . . . . . . . . . . . . 526
3.4. Dinuclear complexes with acyclic ligands . . . . . . . . . . . . . . . . . . . . . . . . . . . . 533
3.4.1. Nitrogen, sulfur and oxygen coordination . . . . . . . . . . . . . . . . . . . . . . . . 533
3.4.2. Nitrogen and sulfur coordination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
3.4.3. Nitrogen and oxygen coordination . . . . . . . . . . . . . . . . . . . . . . . . . . . . 542
3.5. Trinuclear complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
3.6. Tetranuclear complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 553
3.7. Hexanuclear complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 556
3.8. Cluster complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 557
3.9. Polymeric complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 558
4. Mixed valence complexes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 564
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 565
Mephisto - 24-11-2004 at 13:42
Too bad, Ullmann gives no source to this statement.
I found an example, which you might think is too impracticable for clandestine chemists. Nevertheless it is probably worth to read the introduction in
the patent (TIFF-pictures). USPTO-Link.
Abstract
[color=darkgreen]Styrene (I) was purified by formation of a co.ovrddot.ordination compd. with CuCl (II). A 40% I-60% PhEt mixt. (400 g.) was cooled
to -15° and mixed with 100 g. II at the same temp. After 24 hrs. the ppt. was sucked dry and washed with pentane. The ppt. was then mixed with
pentane and the temp. raised to 35°. I was released and could be sepd. by distg. Lower straight chain alcohols are used as catalysts in the
absorption.[/color]
Purification of styrene. Atkinson, Edward R.; Mark, Jacob G.; Rubenstein, David. (W. R. Grace & Co.). (1961), US 2973394
19610228 Patent language unavailable. CAN 55:99260 AN 1961:99260 CAPLUS (Copyright 2004 ACS on SciFinder (R))
Organikum - 24-11-2004 at 18:34
Oh! Thanks to all!
-15°C is in reach of my fridge I hope and decomposition by plain warming sounds ok.
I will give this a try first.