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Author Topic: separation of nitroethane and 2-nitropropane?  (Read 96 times)

NeilPatrickHarris

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separation of nitroethane and 2-nitropropane?
« on: December 25, 2010, 11:15:34 PM »
i have a product that is 90+% nitroethane and <10% 2-nitropropane but the bp's are so close that this is going to be very difficult to isolate the nitroethane, any ideas?

Wizard X

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Re: separation of nitroethane and 2-nitropropane?
« Reply #1 on: December 26, 2010, 01:16:36 AM »
Fractional distillation (http://en.wikipedia.org/wiki/Fractional_distillation) with a longer fractionating column (http://en.wikipedia.org/wiki/Fractionating_column)  and very controlled heating.

Fractional distillation is the separation of a mixture into its component parts, or fractions, such as in separating chemical compounds by their boiling point by heating them to a temperature at which several fractions of the compound will evaporate. It is a special type of distillation. Generally the component parts boil at less than 25 °C from each other under a pressure of one atmosphere (atm). If the difference in boiling points is greater than 25 °C, a simple distillation is used.

However, you can also use it as is (90+% nitroethane and <10% 2-nitropropane) and condense with benzaldehyde.
 
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

NeilPatrickHarris

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Re: separation of nitroethane and 2-nitropropane?
« Reply #2 on: December 26, 2010, 02:08:45 AM »
i have a pretty long vigreux, i'll just have to be very slow and patient with the heat, not distilling to dryness.

actually i was interested in using the EtNO2 for in-situ ethylamine generation via al/hg.  the presence of 2-nitropropane in that scenario worries me

crazyboy

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Re: separation of nitroethane and 2-nitropropane?
« Reply #3 on: December 26, 2010, 02:28:34 AM »
How did you get the nitroethane? I am very interested in obtaining some but have been unsuccessful. I have ~30g of 2,4,5-trimethoxybenzaldehyde that I would like to utilize.

akcom

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Re: separation of nitroethane and 2-nitropropane?
« Reply #4 on: December 26, 2010, 07:00:22 PM »
I would suggest azeotropic distillation, but I couldn't find any information on nitropropane azeotropes.

RoidRage

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Re: separation of nitroethane and 2-nitropropane?
« Reply #5 on: December 26, 2010, 07:20:03 PM »
Quote from: crazyboy on December 26, 2010, 02:28:34 AM
How did you get the nitroethane? I am very interested in obtaining some but have been unsuccessful. I have ~30g of 2,4,5-trimethoxybenzaldehyde that I would like to utilize.

Go for mescaline then :D ... Even if you end up getting some nitroethane, don't waste it on that benzaldehyde...You can get to TMA's through essentials oils ;)

akcom

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Re: separation of nitroethane and 2-nitropropane?
« Reply #6 on: December 26, 2010, 07:23:48 PM »
He would need 3,4,5 TMB for mescaline
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