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Author: Subject: Does anyone know the melting points of nitrated xylene?
fdnjj6
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[*] posted on 7-8-2020 at 10:31
Does anyone know the melting points of nitrated xylene?


I'm going to be doing a mononitration of what I think is toluene. I couldn't monitor the temperature of the distillation but there was crap that boiled over when the oil bath was under 110C and the liquid was boiling at 110-140C. At 140C it was actually bumping though. I assume it was mainly toluene but since I got my toluene from mixing a bottle of carb cleaner with water, and separating the layers, and distilling, I don't know the purity.

I'll carry out the nitration anyway since it seems to be mostly toluene. The MSDS only says toluene, acetone, and methanol are in there as well as CO2. I don't trust it though since I'm pretty sure there was something else in there which was very irritating to my eyes and throat! I'm kinda pissed. The toluene smells like toluene but since xylene and toluene smell similar and have bascially the same density, I can't figure out if there is a lot of xylene in there.

I'll carry out the nitration and should be left with a yellow oil and no initial solids. If there are solids, I'll filter them off. Then I have to chill the yellow oil to -10C - -20C and the para nitrotoluene should crystallize out.

I know the melting points of all of the nitrotoluenes but besides dinitroxylene, I can't find any other metling points of xylene. It seems like xylene nitration needs a catalyst too. I'm just hoping I get pretty pure para nitrotoluene.
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[*] posted on 7-8-2020 at 15:25


trinitro-p-xylene (TPX)m.p. 140.9 °C


....see,

https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6147648/#B8-mol...




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fdnjj6
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[*] posted on 7-8-2020 at 18:57


Sorry I should've clarified. I know the melting points of di and tri nitro xylene but I can't find the melting points of mono nitroxylene. The conditions and temperatures that the mono nitrotoluene will be synthesized at should form mono nitroxylene as well... unless I'm wrong but that's what the patents I found seem to tell me. They never mention melting points though.
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fdnjj6
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[*] posted on 7-8-2020 at 20:13


God damn it I found it. I don't know why but I have this curse that I find answers after I post about them. I literally spent about an hour searching for data but as soon as I post something, I find it using some other keywords I haven't used before.
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[*] posted on 7-8-2020 at 20:28


fdnjj6,
Can you post the answer it might help in the future for someone else.
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[*] posted on 8-8-2020 at 08:39


ortho- nitroxylene MP 7-8˚C



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fdnjj6
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[*] posted on 8-8-2020 at 16:36


Thank you!
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fdnjj6
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[*] posted on 8-8-2020 at 16:44


There are a lot of isomers but the ortho nitroxylene melting points I found are
3-nitroxylene: 15C
4-nitroxylene 29C
Dinitroxylene is 93C not sure about other isomers of it though.

Since I couldn't use my thermometer to properly determine the temp of the toluene distillation, I'm not 100% certain of what I have. The MSDS says only acetone, methanol, and toluene but there is definitely some other shit in there that dried out/irritated my throat for 1.5 weeks. Don't use SuperTech Carb Cleaner!

The oil bath temp was monitored and the temperature of the oil bath was only a bit higher than toluene's bp so it should be toluene. It's impossible for me to know if I have xylene in there so I'll just carefully nitrate it and go through the whole procedure and test the melting point of my product. If it melts below 45C, that's bad. Above 55C, that's bad. I'll wash and recrystallize and try again and if it still isn't at 50 ish C, that's bad. I just wanted some nitroxylene melting points in case it ends up being the wrong mp and then I have some melting points to look at and compare.
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