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gl92038
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[*] posted on 20-1-2012 at 13:34
SnCl4


Hello, I have a simple question. At what temperature reaction between tin and chlorine to produce SnCl4 takes place? :)
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[*] posted on 20-1-2012 at 17:11


So thats spoonfeeding, but I feel like it today as I was helped so much with references...

At what temperature in air I suppose? Don´t know, if you want to know search a little bit, Google and such :)

This is how you make anhydrous SnCl4:

Take a small diameter to height vessel , zylindric so to say where a gasdispersingtube goes to the bottom and another from the top out. You can make this with a rubber-stopper with two holes, but wrap the fucking stopper in teflon tape, seriously not just a little bit but 5 to 10 times around. Or the rubber gets eaten and chlorine all over is no fun.

The dispersingtube you hook to your chlorine generator, dry, dried, conc. H2SO4 dried chlorine. The outlet you hook to a suckbackpreventervessel and then to a vessel to scrub the chlorine, don´t remember what I used then. In the processing flask you fill chloroform or DCM, leave some headspace. Into the chlorinated solvent comes tin. Tin leaves made by simply melting 99% tin solder and let it dropping on the floor. Tiles are preferred a carpet might be not so good. Just stuff so much tin in that the gas gets more dispersed on its way up but is not blocked.
Add a mini, mini, mini, drop of Mercury. Or a mercury salt.
Make sure everythings tight, fire up the chlorine generator (you can say a short prayer before if you like to) and here we go.
Hg makes for some small amalganation and chlorine eats the tin even in the cold no problem. When almost all of the tin is gone - there are some residues, you´ll see - shut the generator down. Clean the lines but seal the flask from the air. Put the flask in the freezer. Put a distillation flask in the freezer. Prepare distillation setup. Shortway distillation. Open the colden flask with the SnCl4, hold your breath, as HCl fumes evade. Transfer to distillation setup. Distill solvent- Change receiving flask and distill the SnCl4. Your distillation setup must be closed except for a vent equipped with a CaCl2 drying tube yes? After distilling put the SnCl4 in a glas-vessel which fits for the volume and can be hermetically sealed, say grounded glass stopper and wrap this with teflon tape. Store in the freezer.

Everytime you open it you´ll have the tears of success.

I made about 250ml SnCl2 in a afternoon and had only two days problems breathing, so that was good.


The procedure is curtesy of Hyperlab/Antoncho IIRC.

/ORG
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gl92038
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[*] posted on 20-1-2012 at 21:36


Thank you so much for the help. :)
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AndersHoveland
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[*] posted on 20-1-2012 at 21:59


Actually chlorine reacts with tin (Sn) foil at room temperature to make the clear liquid SnCl4.
I have actually done this. Be sure that the chlorine is free from moisture, otherwise the liquid will quickly hydrolyse into solid white metastannic acid.

The reaction of SnCl4 with ammonia forms ammonobasic tin(IV) chloride, SnCl3NH2.
Reactions of tin(IV) halides with ammonia derivatives. Part I. The reaction of tin(IV) chloride with liquid ammonia, E. Bannister and G. W. A. Fowles; J. Chem. Soc., 1958, 751-755


[Edited on 21-1-2012 by AndersHoveland]
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[*] posted on 21-1-2012 at 04:34


Quote: Originally posted by AndersHoveland  
Actually chlorine reacts with tin (Sn) foil at room temperature to make the clear liquid SnCl4.
I have actually done this. Be sure that the chlorine is free from moisture, otherwise the liquid will quickly hydrolyse into solid white metastannic acid.

......

Sure it does. Just not always so eagerly in the beginning as one would like it. Doing the reaction in a chlorinated solvent with a pinch of Hg as starter makes things just considerably easier, in special the workup.

And I would believe it being safer, solvent working as heat mediator and stuff.

regards
/ORG
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dann2
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[*] posted on 21-1-2012 at 10:08


Hello,

Spoon feeding on this board is frowned upon.
But nobody said you couldn't use a tube!

Some info. on SnCl4 here:
http://www.oxidizing.110mb.com/chlorate/makesncl4.html

You can make the SnCl4:5H2O stuff using Aqua Reiga (I am told) in the link.

Dropping SnCl4 into water from a height is fun and gives pretty patterns in the water.

Dann2

[Edited on 21-1-2012 by dann2]
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[*] posted on 21-1-2012 at 12:30


The chemistry of hydrolysis of SnCl4 with water is fairly complex, more so than that link mentioned.

I suppose one could do the reaction of Sn with Cl2 in chloroform, but I did not have any problems just reacting the solid metal foil with the gas. Mercury is really quite unnecessary.

[Edited on 21-1-2012 by AndersHoveland]
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dann2
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[*] posted on 22-1-2012 at 10:18



How do you turn Anhydrous SnCl4 into SnCl4:5H2O ?

Cheers,
Dann2
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