I have been trying to synthesize some Antimony chloride.
I think i managed it.
My procedure: first i added 2g of Antimony powder to a solution of 10ml 10% h2o2 + 10ml 20% hcl with a little gentle heating most of the Antimony
dissolved and i had a pale yellow solution of what i assumed to be Antimony chloride.I left this in the beaker for about a week,today i decanted it
into a small bottle and labelled it,then a strange thing happened i dropped the beaker into the bowl in the sink (which was full of cold clean
water)and a white precipitate formed in the water and all round the inside of the beaker.
anyone know what this might be?merrlin - 11-8-2009 at 11:41
Your accidental process sounds similar to the preparation of oxide sols through the dilution/pH reduction of acidic solutions containg metal cations
and hydrogen peroxide.ammonium isocyanate - 11-8-2009 at 11:56
Antimony chlorides decompose on prolonged contact with water, so a one-step aqueous preperation won't work. My best guess is that the compound you
have is antimony oxychloride, the white powdery substance that results from the hydrolysis of antimony trichloride.
The prep of antimony trichloride I suggest would be to burn antimony powder in air, forming antimony trioxide, and then react it with concentrated
HCl, removing the water quickly by applying heat, vacuum, or both.itchyfruit - 11-8-2009 at 12:30
Owell another one not gone according to plan
So i presume the yellow solution is just slightly contaminated hcl and not my Antimony chloride, best relabel that then!!! chloric1 - 11-8-2009 at 14:27
No you had it! Antimony trichloride is stable in concentrated HCl. When diluted the oxychloride is precipitated. IRC antimony trichloride boils at
like 235 Celsius. You only need some antimony oxide and HCl in excess. Distill this and the first thing to come over is constant boiling 20% HCl.
Later, the temperature is raised and the SbCl3 comes over. Any SbOCl3 can just simply redissoved in conc HCl to repeat the whole process. Antimony
is a metaloid which has properties intermediate between bismuth and arsenic. Like a metal, its chloride can be isolated from aqueous HCl. Like a
nonmetal the chloride is mainly covalent and hydrolisized easily in dilute solutions. itchyfruit - 11-8-2009 at 14:45
Cool,it's nice to get something right for a change
I don't know what i'm gonna do with it yet but i'm sure it'll be handy for something!!!ammonium isocyanate - 11-8-2009 at 16:20
Got any anhydrous HF? Well, I kinda hope not, but you could always generate a little. Anyways, you could distill over the antimony trichloride,
chlorinate it while molten with Cl2, and then dissolve that in anhydrous HF (produced from alkali or alkali earth fluoride and concentrated H2SO4) to
make HbSF6. Of course I don't actually recommend you try the reaction. It's really dangerous. But kinda cool to think about. After all, HSbF6 is
20,000,000,000,000,000,000 stronger than 100% sulfuric acid!itchyfruit - 11-8-2009 at 17:04
I have some Cryolite(the proper stuff from Greenland)it's over 30years old but it is fluorine ish (F6)at the end of the formula.
But you right i don't think i should be messing with it.
Just out of interest what would anyone want something that strong for?ammonium isocyanate - 11-8-2009 at 17:14
Forming carbocation salts. HSbF6 is so strong that it will protonate hydrocarbons to form stable carbonium ions (after emission of H2 or CH4).itchyfruit - 11-8-2009 at 17:34
Nothing complicated then not_important - 11-8-2009 at 19:07
Three old inorganic preparations books, all of which include SbCl3
Useful, although some of the experiments are outdated and others are considered a bit dangerous nowadays. They will at least give ideas on what to
expect, such as the instability of SbCl3 in water.
Taoiseach - 11-8-2009 at 22:50
Destillation of SbCl3 is troublesome. You need to catch it at the right time, otherwise all you get is a mixture of HCl and SbCl3 again. I was unable
to get dry SbCl3 using destillation. Trace amounts of SbCl5 make it nearly impossible because it liquifies the SbCl3 at quite a low temp (maybe
60-70°C) so you dont even notice when the SbCl3 comes over. I dont know if SbCl5 is formed when HCl+H2O2 is used, but it is always a byproduct of the
reaction of metallic Sb with Cl2.
I suggest you dont bother trying to destill and instead precipate it right from the solution. Dry HCl gas should do the trick. Cool the solution and
bubble dry HCl through it. This is a convenient method that works with most chlorides.
not_important - 11-8-2009 at 23:27
Quote:
[uote]I suggest you dont bother trying to destill and instead precipate it right from the solution. Dry HCl gas should do the trick. Cool the solution
and bubble dry HCl through it. This is a convenient method that works with most chlorides.
However it often doesn't work with chlorides that form complexes with Cl-, and thus HCl, as SbCl3 does. Dissolving Sb2O3 or Sb2S3 in concentrated
aqueous HCl gives a transparent solution of SbCl3 in the acid, without SbCl5. If using elemental Sb + Cl2, use a setup similar for making PCl3,
collect the product from that and add a little powdered Sb to it, heat it enough to melt the SbCl3 if needed, and stir for awhile, then distill.
I dont know if SbCl5 is formed when HCl+H2O2 is used ...
It does. SbCl5 forms alongside SbCl3 if antimony powder is solubilized in H2O2-containing hydrochloric acid (E. Salkowski, Ch.Ztg. 40 [1916] 449).woelen - 12-8-2009 at 04:57
I have a book of Vanino (German, 1920's), which tells that SbCl3 can best be made by having a slow flow of dry chlorine gas (dried by passing it
through a tube of anhydrous CaCl2 or bubbling it through conc. H2SO4) over finely crushed antimony. An almost horizontal tube is used with the
antimony in it, the tube being connected to a two-holed flask. One hole of the flask is connected to the tube, the other is connected to a slow
chlorine generator. While the antimony reacts, a liquid compound is formed, which slowly runs through the tube into the flask. When all antimony has
reacted, then the product is in the flask and it can be distilled to purify it (getting rid of dissolved chlorine and SbCl5).
I never tried this method myself, but it looks interesting and feasible for a home chemist with some decent glassware.itchyfruit - 12-8-2009 at 15:52
That sounds like it might me within my capability's, i made some progress with my fume cupboard today when i get it finished i'll give that a go,after
phosphorous chloride off course itchyfruit - 27-8-2009 at 14:33
what happens to antimony pentafluoride if it is not kept under nitrogen?
