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AJKOER
Radically Dubious
Posts: 3026
Registered: 7-5-2011
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Quote: Originally posted by CuReUS  | | Quote: | | And yes I plan to gas this with Cl2 in an oil bath above the boiling point of SCl2 but below S2Cl2...say 120C. The SCl2 vapors that continuously form
will combine with SO2 & excess chlorine over a hot activated charcoal bed in making SOCl2. Which will then be purified and used in the making of
alkyl chlorides. |
I think you didn't read my post,S2Cl2 can make alkyl halides from alcohols,you don't need to convert it to thionyl chloride
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Here is a link to page 191 of "Small-Scale Synthesis of Laboratory Reagents with Reaction Modeling" by Leonid Lerner that discusses purifications
issues with respect to SOCl2.
Link: https://books.google.com/books?id=VqosZeMjNjEC&pg=PA191&...
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Comments per another source on safe paths to SOCl2:
"The oxidation of SCl2 by atmospheric oxygen has been investigated using activated charcoal as the catalyst. The reaction has been discussed in terms
of two reactions. Firstly, the irreversible oxidation of SCl2 to SO2Cl2 :
SCl2 + O2 --> SO2Cl2
and secondly, the reversible reaction between the SCl2 and the SO2Cl2 to form SOCl2 :
SCl2 + SO2Cl2 <--> SOCl2
This oxidation has been investigated at the temperatures 193°C, 138°C and 320°C, and the equilibrium constant of the reversible equilibrium
reaction has been determined for each temperature. From the temperature dependence of this equilibrium constant it is found that the reaction is
exothermic to the extent of 18 kcal.
(Yield of SOCl2 at 193°C : ~73%) "
Link: https://www.thevespiary.org/rhodium/synthetikal/www.syntheti...
While not cited in the original work which dates back to 1947, I would suspect, in actuality, some radical based chemistry via uv radiation creating
active species of oxygen, chlorine and sulfur noless (atomic oxgen, singlet oxygen, S2O, SO, S2Cl, for example, see recent paper "Photochemistry of a
Volcanically Driven Atmosphere on Io: Sulfur ... " available at https://www.google.com/url?sa=t&source=web&rct=j&... pages 81 to 85 in particular) in the referenced action of "atmospheric oxygen" on
SCl2 forming SO2Cl2.
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Some comments by Atomistry (http://sulphur.atomistry.com/sulphuryl_chloride.html ), on SO2Cl2 preparation to quote:
"Chlorine and sulphur dioxide will only unite under some accelerating influence. It was by the interaction of these gases in sunlight that sulphuryl
chloride was first obtained by Regnault in 1838.
Bone charcoal or activated wood charcoal is a convenient accelerator, combination occurring instantly. If the vessel in which the reaction is carried
out is cooled to 30° C., the sulphuryl chloride is condensed and may be drained away as rapidly as it is formed. The terpene hydrocarbons, especially
pinene and limonene, also certain ethers, phenols and esters, are effective catalysts, as also is camphor.
The formation of sulphuryl chloride is favoured by low temperature and its decomposition by high temperature:
SO2 + Cl2 ⇔ SO2Cl2.
Both these reactions are .catalysed by the foregoing catalysts. For the efficient preparation of the chloride, the dry reacting gases are brougght
together at ordinary temperatures in the presence of a catalyst such as "Norit," a highly activated powdered carbon. The mixture is then cooled to
-10° C. to ensure complete combination, filtered from the catalyst and carefully distilled, the heat being applied to the liquid for as short a time
as possible. "
[Edited on 21-5-2015 by AJKOER]
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byko3y
National Hazard
Posts: 721
Registered: 16-3-2015
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I can't seem to find the result of the reaction
Na2S + S2Cl2 -> ?
Does anybody know good books about sulfur compounds, especially sulfur halides? (gmelin's?)
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