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Author: Subject: Preparation Of CuCl And Problems Drying
SimpleChemist-238
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[*] posted on 20-2-2015 at 11:14
Preparation Of CuCl And Problems Drying



A simple way to make CuCl without a HCl complex or sodium salts

I have been revisiting copper compounds in hope to discover something unknown to me and have found a interesting thing. I was looking in YouTube for videos on how to make copper 1 chloride but everything thing was very expensive based on yields. Most methods involved copper chloride complexes and 4 different salts.

I was at a gun show over the weekend and purchased a 1oz copper coin just for chemistry and for this reaction.

Take any amount of copper 2 chloride (About 20g for me.) and add copper metal to it. I tried it with a solid copper penny and it did not work. A piece of copper with a large surface area is best, for me this was a 1oz Cu coin.

Biol the mixture of copper 2 chloride and copper metal until the mixture turns black. Then let it cool and filter the copper 1 chloride out. Repeat the processes until the solution is no longer green.

I have been having problems drying it but a hot air gun on 300F works best. For best shelf life store under N2 gas. CuCl is a white insoluble powder and oxidizes in air and water.

[Edited on 20-2-2015 by SimpleChemist-238]




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[*] posted on 20-2-2015 at 11:24


An easier way is just heat copper (II) chloride to 700°C for ten or so minutes under nitrogen. If you lack either a good heat source or nitrogen gas, just go to a welding shop, they can easily supply both. I'm friends with quite a few welders, so I can do this for free (although I already have both heat and N2), but you could just pay them a few bucks and they'll do it in a few minutes. If it's still green, either heat it more, or rinse away the soluble copper (II) chloride.



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[*] posted on 20-2-2015 at 11:29


And an even easier method for preparing CuCl is adding ascorbic acid to a hot solution of CuCl2.
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[*] posted on 20-2-2015 at 11:37


Yeah but then you have to dry it, and oxidation will inevitability occur. If you have the nitrogen and torch, decomposition would be way faster and make a purer product.



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[*] posted on 20-2-2015 at 17:52


One method of preparing copper I chloride that results in coarse crystals that oxidize slowly because of their size is to simply place copper in ammonium chloride solution and seal the bottle and leave to stand for several months. I discovered this accidently many years ago when I left a large copper soldering-iron tip in dilute ammonium chloride solution in a jar and forgot about it for months. When I re-discovered it the copper was covered in colourless rhombic dodecahedral crystals of lustrous cuprous chloride. I didn't immediately recognise it but some simple chemical tests and the tendency of the crystals to slowly oxide to an insoluble copper chloride didn't leave too many options. I keep meaning to try this again under more carefully controlled conditions with copper wire in ammonium chloride, bromide and iodide. An interesting feature was that the clear solution did not smell of ammonia nor did there appear to have been any build up of pressure which you expect if the ammonium chloride was simply acting as a HCl doner.
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[*] posted on 20-2-2015 at 18:00


Quote: Originally posted by Boffis  
I didn't immediately recognise it but some simple chemical tests and the tendency of the crystals to slowly oxide to an insoluble copper chloride didn't leave too many options.

The crystals slowly oxidized to an insoluble copper chloride? Copper (I) chloride is insoluble, if it oxidized, it would not be an insoluble copper chloride.




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[*] posted on 20-2-2015 at 18:23


Quote: Originally posted by Molecular Manipulations  
Quote: Originally posted by Boffis  
I didn't immediately recognise it but some simple chemical tests and the tendency of the crystals to slowly oxide to an insoluble copper chloride didn't leave too many options.

The crystals slowly oxidized to an insoluble copper chloride? Copper (I) chloride is insoluble, if it oxidized, it would not be an insoluble copper chloride.


Rubbish! CuCl is indeed insoluble but so is the pale green oxidation product. You have obviously never tried drying CuCl.
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[*] posted on 20-2-2015 at 18:45


You're quite right, I've never dried wet copper (I) chloride because mine never gets wet.
But if you want to "rubbish" me you might as well try to be right.
One of copper (I) chloride's oxidation product is indeed insoluble but it's not strictly a chloride.
6 CuCl + 3/2 O2 + 3 H2O → 2 Cu3Cl2(OH)4 + CuCl2.

[Edited on 21-2-2015 by Molecular Manipulations]




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[*] posted on 20-2-2015 at 19:16


Just curious here, why must this be done without any compounds containing sodium?



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[*] posted on 30-5-2015 at 11:06
CuCl(I) from CuO _ copper chloride (I) from copper oxide(II) by reduction with sodium sulfite


Hi , i wanted to share a receipe i saved a year ago... (sorry my english is not very good^^)

It should lead to a sufficient purity for home chemists (surely not for a pro lab ;) )

Chemicals:
CuO(min 77%, industrial grade)
HCl 30% (industrial)
Na2SO3 (min 98%)

Steps:
1) CuO(excess) + 2HCl > aqueous CuCl2 and the remaining CuO
2) 2CuCl2 + Na2SO3 > Na2SO4 + 2CuCl
3) Quick vacuum filtration under inert gas (if you can)
4) Washing and drying under inert gas.
5) Storage under inert gas + parafilm.

------------------------

1) In a beaker, put 129g CuO (1.257mol) and 200ml of water. Add 265ml 30%HCl (2.51mol) and stir well. Wait a little bit and measure the pH, it sould be 4-5. Then, filter the solution and place the aqueous CuCl2 into a large beaker. Prepare a solution of 165g Na2SO3 (1.3mol) in 600ml of water (heat if not dissolve entirely).

Préliminary to the step2, prepare your inert atmosphere filtration unit. It could be a reversed funnel or a plastic bag connected to your source of inert gas. Prepare a little bit of cold ether or glacial acetic acid to wash the product. And prepare an erlenmeyer (150-250ml are ok) and the two holes stopcock, the first hole for inlet inert gas and the second for nothing :D. Begin to heat a bath at 80-90°C.

2-3-4) In one step, pour the aqueous Na2SO3 into the CuCl2 solution. Stir, wait 10seconds and begin the filtration with the inert gas outlet the closest as possible to the buchner. When it becomes a cake, wash whith cold ether or acetic acid to remove the remaining water, and continue to dry as possible. Transfer quickly your product into the erlenmeyer, place it on the bath and flow inert gas through to drain condensation and protect the product from oxidation. Wait 2-3hours to get it dry. Rem : the flow of gas must be very slow and use a pasteur pipet to bring the gas.

5) Plug the erlen and seal with parafilm. Then take something like a plastic bag, place your erlen and vacuum it, then fill with inert gas and knot the end.

Yield? I don't know but sufficient, Weighing the product = more exposition to O2.

Purity ? > yes i know min77% CuO is not cool (I didn't have Cu2O at that time), it's for this reason i made a solution of CuCl2 with large excess of solid CuO.

Ether or acetic acid ? Acetic acid is better because partial pressure of O2 is very low into it. Non purified Ether contains peroxides+O2 and oxidize your Cu(I). I tried first with acetic acid but it's a hell to dry the product.The next time i washed it with ether and yielded a clean white dry product.

PS : Anyone tried the synthesis from Cu2O ?

where to find inert gas ? Ar (from hardware store) or N2 from welding store.


Any remark is welcome.
Enjoy!

[Edited on 30-5-2015 by ledob86]
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[*] posted on 30-5-2015 at 11:27


Quote:
CuO(min 77%, industrial grade)


That probably means 77 w% copper.

Good luck with dissolving that CuO in HCl: not all grades willingly do that.

Starting from commercial CuSO4 + NaCl should work too.

[Edited on 30-5-2015 by blogfast25]




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[*] posted on 30-5-2015 at 12:01


I didn't encountered problems with dissolving the CuO. And yes it was probably 77% bw

Next time i'll try with Cu2O and HBr to make CuBr(I) with the same manner for drying. It should give a purer product than when using sodium sulfite because of the probable presence of Na2SO4 in the final product.
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[*] posted on 30-5-2015 at 14:06


Quote: Originally posted by ledob86  
77% bw



77 % by weight OF COPPER. "77 % bw" means of cuO.




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