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Author Topic: Ammonia Purification  (Read 156 times)

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Mycilius

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Ammonia Purification
« on: Yesterday at 07:18:22 AM »

I'm working on a method of ammonia extraction from a cleaning solution. The only listed ingredients for the cleaner were "ammonium hydroxide" and "surfactant", this is the most specific information on the product I could find as an MSDS sheet was surprisingly nowhere to be found even on the company website.

From my own research I've made up a setup for extracting ammonia
https://drive.google.com/open?id=0B3lmcYL898TkZDdBZ01CZlVvblE

Before setting this up I ran a small test to see if the surfactant would interfere with the extraction, the long and short of that being simply "no" as while it does foam a bit it would not cause a problem in a sufficiently large flask. However, there was something that I ran into during this test that stopped me in my tracks, the vinyl tubing I used for the test turned a sort of light yellow as well and became somewhat soft as it heated up. The tubing I used was recycled from a past experiment where I used it to carry chlorine. This discoloration I'm fairly certain is caused due to the vinyl tubing being a polymer plastic and the reactivity surrounding the C=C double bond with the NH3 passing through reacting somewhat.

My concern is over how the tubing will fare in these conditions over the course of the extraction which I plan to let run for several hours at a time. I have not locked down a precise temperature yet but it appears that I won't need or want the temperature to rise above 100C in the boiling flask.


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AWK

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Re: Ammonia Purification
« Reply #1 on: Yesterday at 08:11:57 AM »

This is a simple distillation. The only problem is good cooling. I advice receiver and then rinser - both cooled in ice-salt cooling bath.
Note - boiling temperature should be below 100 C. Expect foaming of distilled solution.
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Mycilius

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Re: Ammonia Purification
« Reply #2 on: Yesterday at 09:23:21 AM »

I honestly had not thought of running it like a simple distillation as I had thought the surfactant would have came over with the water/ammonia solution. If I used a simple distillation setup would the water just carry the ammonia over like a steam distillation while leaving most of the surfactant behind?

The whole reason why I had planned a setup like the one shown in my last post was because I had thought to heat the solution enough to drive off the ammonia gas while leaving much of the water and surfactant behind only to bubble the ammonia through fresh distilled water. If I could get away with using a simpler setup as I think you are suggesting I would definitely spring for that.
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Re: Ammonia Purification
« Reply #3 on: Yesterday at 10:40:24 AM »

I honestly had not thought of running it like a simple distillation as I had thought the surfactant would have came over with the water/ammonia solution. If I used a simple distillation setup would the water just carry the ammonia over like a steam distillation while leaving most of the surfactant behind?

The whole reason why I had planned a setup like the one shown in my last post was because I had thought to heat the solution enough to drive off the ammonia gas while leaving much of the water and surfactant behind only to bubble the ammonia through fresh distilled water. If I could get away with using a simpler setup as I think you are suggesting I would definitely spring for that.
Household solutions do not contain more ammonia than 10 %, hence you distillation start at ~50-70 C. Vapors will contain more ammonia than solution, hence small amount of water is needed in receiver at the beginning. During repeated distillation you may use previous diluted ammonia from the rinser. Good cooling (ice+salt) of receiver and rinser is absolutely needed (eventually use the second rinser with diluted H2SO4 without cooling) - boiling point of concentrated ammonia is ~30 C.
The residue after distillation still may be used for cleaning.
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Mycilius

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Re: Ammonia Purification
« Reply #4 on: Yesterday at 02:08:33 PM »

Thank you for your help, I've only been doing this for around two years so I'm sure my inexperience shows.
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