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selsel
June 17th, 2002, 12:57 PM
i searched everywere for a way to form SnCL2 or SnCL4 and i would like someone to tell me a way to make it withought to much mess.The only material i got is 95% Sn.

I want to use it as a catalyst to form tetrameric acetone peroxide

rikkitikkitavi
June 17th, 2002, 01:55 PM
SnCL2 is made through dissolving Sn in HCl. It is a strong reducant(oxidizes to Sn(IV)).

SnCl4 can be made by reacting SnCl2 and Cl2 in solution, or Sn and Cl2-gas. Other oxidants can probably be used to, but I dont know if they (or their reduced form) might interfer in the process of making tetrameric AP. SnCL4 hydrolyses easily to basic Sn(IV) compounds wich preciptates in neutral solutions, preventen by addition of some HCL.

/rickard

megalomania
June 18th, 2002, 12:47 AM
Here is a more detailed purification procedure to prepare quality stannous chloride, SnCl2, from "Organic Synthesis Collective Volume 3":

The most active and dependable form of anhydrous stannous chloride is prepared as follows: In a 600-ml. beaker is placed 204 g. (189 ml., 2 moles) of acetic anhydride (99–100%) and, while the liquid is stirred by hand, 226 g. (1 mole) of commercial C.P. crystalline stannous chloride dihydrate is added. This operation should be performed in a hood, for the heat of the reaction is sufficient to cause the acetic anhydride to boil. After about 1.5 hours, the anhydrous stannous chloride is filtered on a large Büchner funnel, rinsed with two 50-ml. portions of dry ether, and dried overnight in a vacuum desiccator. The yield is quantitative (189 g.). The product may be kept in a tightly closed bottle until it is wanted. The product secured by dehydrating crystalline stannous chloride in an oil bath at 195–200° is satisfactory in many instances but is not dependable.

Incidentally, this is in the wrong section. I have moved it to Chemistry Related.

selsel
June 19th, 2002, 09:11 AM
well excuse me for bad english...

I will make my question more simple for the tin tetracloride catalyst.
All i need is an easy to find or manufacture a catalyst (not absolutely tin cloride) that will form a tetrameric acetone peroxide explosive compound.
i posted the topic about SnCL2 because it is the only catalyst i found after some research,maybe somebody knows if there is an other one?
thanks.

selsel
June 21st, 2002, 10:31 AM
I tried to dissolve Sn in HCL but it dint.
Any ideas what went wrong
The HCL was 12% and the Sn 95%

Polverone
June 21st, 2002, 12:44 PM
What's the other 5% that isn't Sn? If you're starting with lead-free solder as your tin source, it often contains silver, and although I haven't experimentally tested this I would guess that silver chloride formation could really slow down your reaction rate.

Is your starting material etched/attacked at all, or does there seem to be absolutely no change? Are you heating the acid or just mixing it with the metal?

Here's a couple of other random ideas: try first dissolving the metal in sulfuric acid, since you can heat sulfuric acid to much higher temperatures than hydrochloric (the metal should melt well before the acid boils), converting the sulfate to carbonate via metathesis with sodium carbonate, and then using hydrochloric acid on the carbonate.

Or try adding hydrogen peroxide to your HCl. I know that the rate of attack on copper is greatly increased if you do this, though I don't know if it will have an effect on tin.

selsel
June 22nd, 2002, 11:10 AM
the 5% of my tin is antimony.
i just droped the tin in hydrochloric acid an it is still in there but i have not try to heat it because is dangerous(toxic fumes).
I had a thought that some metal oxides could work as catalysts like iron oxide but i want to know if it works on tetrameric AP before i try this so i can be sure for the final product.

ikbendirk
May 12th, 2004, 04:55 PM
I am able to get some SnCl3.. would this also work to catalize the tetrameric rxn?
or should i try to use it as precursor to sythesise SnCl4 some way?

megalomania
May 13th, 2004, 01:28 AM
Well, it would seem a stretch if tin trichloride works, but I suppose some experimentation is in order on your part to find out.

frogfot
May 13th, 2004, 11:16 AM
Ain't SnCl3 an ion? So, since tetramer formation needs an Sn2+ or Sn4+ to be catalysed, I'd guess SnCl3- wouldn't be able to do same thing (cause it have different shape..) Though I may be totally wrong..

Btw, some reduction reactions (like nitro group to amine) uses SnCl2, which then oxidises to SnCl4. Since SnCl2 is very easy to prepare, this would be a method of choice (unless one likes the reaction between chlorine and molten Sn :rolleyes: )

Rosco Bodine
May 13th, 2004, 11:35 AM
Pure tin is needed .

There are lead free fishing sinkers made of pure tin .

These can be dissolved in excess hot HCl ,
and the resulting solution boiled down until concentrated to
a syrupy goo of hydrated tin chloride which solidifies on cooling .
This material will deteriorate from exposure to air and moisture ,
so it should be kept dry in sealed containers .

Small broken chunks of the material may be dissolved in water and
used as the catalyst for tetrameric AP . The aqueous solutions
are unstable on long keeping due to hydrolysis , so the catalyst
solution should be freshly made up in small quantities as needed .

The catalyst solution is very reactive on contact with the
peroxide / acetone mixture , making an audible frying sound
as a tiny stream from a syringe contacts the vortex of the
rapidly stirred mixture . So the introduction of the catalyst
solution should be done cautiously and with turbulent stirring .

The tetrameric AP is slightly more powerful than the trimer ,
and it is much less volatile in storage , subliming at perhaps
one half to two thirds the rate of trimeric AP . The density
and hardness and reflectivity of the crystals of tetramer is
also higher than for the trimer .

ikbendirk
May 13th, 2004, 12:07 PM
frogfot, you're right.. SnCl3 is an ion, so the material adressed as SnCl3 is probably SnCl2 . 2 H2O... uhm.. this one could be used as a catalyst too right :rolleyes: ?

K9
May 13th, 2004, 03:27 PM
That is most probably SnCl2.2H2O. I see from a website (http://www.uvi.edu/SandM/che251.htm) that their method of preparation for tin (III) chloride is - "tin(III) chloride: Dissolve 113 g SnCl2.H2O (free of iron) in 250 ml conc. HCl, then add pieces of mossy tin, and dilute to 1 L with distilled water".

But SnCl2.2H2O will work effectively as a catalyst for the prodcution of tetrameric acetone peroxide.

nbk2000
May 13th, 2004, 07:47 PM
It's also been used as a chemical smoke agent, particularly in mixes with CW agents, to visualize the agent dispersal.

organikum
August 25th, 2004, 05:05 PM
Anhydrous SnCl4 production:

Have a look here:
https://www.the-hive.ws/forum/showflat.pl?Cat=&Number=511779

There is a description of apparatus and method.
The tin needs not to be absolut pure 95%+ , the chlorine not absolut anhydrous, drying through CaCl2 is ok.
Stannic chloride hydrate precipitates and can be filtered off, better is distillation of the SnCl4 whats a liquid with a boiling point of about 120 deg.C.

Bugger
August 25th, 2004, 05:40 PM
As a chemical smokescreen producing agent, TiCl4 is the compound of choice used by the military. Both TiCl4 and SnCl4 are hydrolysed to the highly opaque dioxides and HCl when dispersed as vapors or aerosols in moist air, but they would not work in perfectly dry air, as in cold desert climates. Although no doubt SnCl4 could be used, its much greater molecular weight (due to the Sn) is a disadvantage, as regards both the bulk weight of the chemical, and the length of time the SnCl4 and the SnO2 produced by hydrolysis can remain suspended in air. A much cheaper and lighter (than both of these) compounds that could be tried is SiCl4.

Bugger.

me234
August 26th, 2004, 02:20 AM
It's most likely already been seen, and NBK has been here already, so it may not be my place to say, but...
Ikbendirk, it's 'I', not 'i'.

Pb1
August 26th, 2004, 09:32 PM
Lost in the recent forum outage:

SnCl2 + 2HCl + 1/2O2-> SnCl4 + H2O

Just bubble O2 into a solution of SnCl2 and HCl.