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Topic: Nitrating reactions using nitrate salts rather than nitric acid  (Read 7431 times)

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Offline nj_bartel

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Nitrating reactions using nitrate salts rather than nitric acid
« on: November 24, 2009, 02:42:48 AM »
Are there any drawbacks to generating the nitric acid in situ, other than requiring additional conc sulfuric acid?

Offline Borek

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #1 on: November 24, 2009, 03:16:01 AM »
Mixture will be always less acidic.
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Offline nj_bartel

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #2 on: November 24, 2009, 03:23:14 AM »
Is the maintenance of that incredibly high level of acidity necessary for most applications, as long as you're maintaining a solution acidic enough to have a significant portion of nitronium ion?  It's not like diluting with water at any rate.

Offline 408

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #3 on: November 24, 2009, 08:58:54 AM »
Damned if I can find the section in the Organic Chemistry of Explosives that covers this.
But if you look it is in there, somewhere.

Usually it allows less water content in the nitration compared to using 70% nitric/100% H2SO4.  But some mechanical issues as it makes the reaction thicker.

Offline nj_bartel

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #4 on: November 24, 2009, 10:13:55 AM »
Thanks :)  Mechanical issues are better dealt with than the pain of distilling nitric acid!

Offline 408

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #5 on: November 24, 2009, 01:49:46 PM »
You obviously have never distilled 100% nitric using a big beaker, a sandwich baggie, and a shot glass ;)

It also depends what you are nitrating, as it does have increased potential for hotspots to develop....

Offline nj_bartel

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #6 on: November 24, 2009, 01:53:10 PM »
That sounds very fun :D  I was under the impression you couldn't distill to 100% with nitric though - you need to distill then dessicate, correct?

Offline 408

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #7 on: November 24, 2009, 02:09:47 PM »
Not if you distill out of concentrated sulfuric.  Large beaker with KNO3 and H2SO4 (excess sulfuric for heat transfer) in the bottom.  Centred in this beaker is a shotglass in the style of a mini wineglass  }-<  (angle ascii 90degrees CCW to see the needed type of shotglass).  A sandwich baggie is placed over the beaker, in a cone style, such that one corner is directly over the shot glass.  Then rubber band the baggie to the beaker, fill the baggie with ice and water, and leave the contraption in a ~50C water bath.  After a few hours you will have a shotglass of 100% nitric. 

Make sure the baggie is compatible with nitric first from online tables.  I cannot remember what type I used, but suffice to say, if it breaks, you will have a bad day from adding water to hot acid :P   :o

Offline nj_bartel

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #8 on: November 24, 2009, 08:30:47 PM »
I love that setup!  So simple  :)

Offline billnotgatez

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #9 on: November 26, 2009, 05:17:44 PM »
Quote
I love that setup!  So simple

Are the safety precautions simple?

Or are we doing this in the scary mode?

Offline 408

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Re: Nitrating reactions using nitrate salts rather than nitric acid
« Reply #10 on: November 26, 2009, 06:33:27 PM »
Ventilation/respirator; 100% nitric fumes insanely
Gloves
Goggles

Latex gloves are instantaneously dissolved by warm 100% nitric acid.  I will tell you this to avoid having to learn it the way I did  ;)

Multiple baggies are recommended, just in case one tears/gets punctured.

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