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blogfast25
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Quote: Originally posted by Rainwater  |
Moving on from there, i have some stannous chloride(dihydrate)
Not sure if it can be made anhydrous by heating above 250c
But if it can that is a much lower reaction temperature than 330c
The second problem is thermodynamics indicates it will be more exothermic than silver chloride.
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It will not be possible to dehydrate SnCl2.2H2O by mere heating: the hydrate will hydrolyse badly without some kind of
protection, like from NH4Cl or thionyl chloride.
But I can't see greater exothermicity being much of a problem.
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Rainwater
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Out of that list, it looks like the only salts that can easily be made anhydrous are
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Name ΔG ΔH ΔS ΔG = 0 when T =
AuCl3 -557.97 -466.90 333.38 -1673.66 C
CoCl2 -322.77 -231.38 334.59 -964.66 C
HgCl2 -595.09 -496.22 361.96 -1644.09 C
MnCl2 189 275 313 604.24 C
NH4Cl 8.71 220.00 775.00 11.2
NiCl2 -353.70 -253.01 368.61 -959.55 C
PbCl2 -188.67 -90.79 358.32 -526.54 C
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I'm going to try to optimize the NH4Cl process because that's the same stuff I put on my roses to make them red and I have plenty in stock. It's
relatively nontoxic and the reaction is easy to control. And mostly because I don't have any of the others.
Using mineral oil, nothing. No gas production of any kind, 50ml of baby oil, 2g of aluminum foil, 6g of NH4Cl, 24hours at 190c with stirring. Not one
bubble collected
Oil turned dark.
At 330c i started distilling the oil, and gas production began. Solids where highy reactive to water.
Next test will be directed at making a cheap disposable apparatus designed to cool the gasses below 190c and collect crude product for sublimation.
"You can't do that" - challenge accepted
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Rainwater
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After several experments this is the cheapest appratus that worked
It goes without saying the appratus and all components must be dry before assembly, this should be performed with adequate ventilation and gas capture
equipment.
This reaction is very well controlled but must be executed with extreme caution. Products are highly reactive with water. Side products are dam near
explosive with water, boiling it instantly.
The entire reaction in the described appratus took less than 5 minutes once started. Multiple products are formed including 1 or more unknown
compounds which react violently with water
Products:
ammonia gas
Hydrogen gas
Anhydrous aluminum trichloride
Unknown solid, liquid at 220c for a limited time. I Guess it decomposes
BoM
(1) steel food can
(1) soda can
Aluminum foil/shavings
high temp sealant, im using hvac rated "duckseal"
Metal pipe, atleast 1/4in diameter
Acetone based cleaner
Ammonia chloride 30g
Step 1) cut the bottom off the soda can and discard the rest, ensure the soda can fits into the food can
Step 2) Clean the plastic liner out of the steel can and soda can with acetone.
Step 3) drill hole into center of food can lid and soda can bottom, the diameter of the pipe used
Step 4) place pipe into center of can and loosly pack foil/shavings around it
Step 5) insert soda can over pipe, your making a bowl
Step 6) fill bowl with salt.
Step 7) place food can top over pipe and seal appratus very well.
The apparatus is burried in a sand bath with the salt at the top.
Heat is applied from the bottom. Ensuring the aluminum will be
At sufficient tempature (350c)before the salt begins to decomposes(330c).
aluminum should be in the appratus lose enough to create large surface area and maximum exposure
The outlet pipe shoud enter a cooled flask to collect the solid product.
Be prepared for large quantities of hazardous gas.
Weight of the aluminum should 3 times or more exceed the weight of ammonia chloride used. If not the output product will be contaminated with
reagents. This is due to the endothermic nature of the primary reaction cooling the aluminum below the requires tempature.
When this happens reagents pass through unreacted and contaminate the product.
The additional thermal mass of the aluminium as well as the reactor arrangement in a sand bath ensures the aluminium temperature exceeds 350c for the
duration of the reaction. By bottom heating quickly a temperature gradient will form, ensuring the proper tempature is maintained to prevent
contamination of the final product.
After the appratus has cool it can be neturalized by slightly opening the top can and dunking the entire appratus in an extream
excess of water.
My bests yield was 15.71g with minor contamination.
After sublimation 11.42g was recovered.
30g NH4Cl ÷ 53.491 g/mol NH4Cl * 2mol AlCl3 ÷ 6mol NH4Cl * 133.34g/mol AlCl3 = 24.93g maximum yield
11.42g ÷ 24.93g = 45% yield
Lots of room for improvement, great source of anhydrous ammonia.
Edit: fixed typo
[Edited on 26-12-2022 by Rainwater]
[Edited on 26-12-2022 by Rainwater]
"You can't do that" - challenge accepted
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blogfast25
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Note that the first letter of a chemical element symbol is always a capital letter: H, N, A, O, Fe etc etc.
Nice write up.
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sceptic
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Nice documentation!
Anhydrous copper (II) chloride dissolved in acetone should be reduced by aluminium to copper and aluminium chloride. Based on this data it looks like copper chloride might have retrograde solubility in acetone, so cooler temperatures should increase solubility, as well as
reducing acetone losses to evaporation. I've tried a similar experiment with copper chloride in propylene carbonate, and it turned from a dark brown
solution to clear, which leads me to think that it did form aluminium chloride.
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unionised
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I'm pretty sure that acetone will react with AlCl3.
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sceptic
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I would have thought so too, but Rainwater apparently used it successfully for extraction.
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Rainwater
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It did react but after distillation
"You can't do that" - challenge accepted
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