Sciencemadness Discussion Board

NMP from paint stripper

spong - 18-10-2010 at 02:58

I was spending far too much time thinking about where I could find DMF and then I noticed that a few paint thinners use NMP which works just as well in most situations. I bought a tin of polystrippa paint/varnish remover (the DCM free version) and planned to vacuum distill it from the thick syrupy goop.
The thinner:


Into the flask (yes I'm using boiling stones under vacuum, yes they did not work very well and there was plenty of bumping :P)


The setup with my fridge pump I snagged from a bin at uni :D:


The goop first starting to boil:


It didn't boil as nicely as that the whole way through, most of the time it would bump and form big bubbles but none made it into the condenser. Firstly something came over at about 60C, my fridge pump isn't THAT good, I'm guessing it was something else in the thinner, too high for water, perhaps a fragrance. It had an orange scent I think so that could be it. The boiling point then stayed around 80-90 for the rest of the distillation which is most likely NMP.

First drips:


The finished (for now) product:


The fragrance will have to be removed somehow, perhaps a fractional vacuum distillation if my fridge pumps are up to the task. Can someone do their best to describe the scent of NMP? I can smell something aminoniaish but there's some fake orange/citrus smell in there too (not limonene, that smells amazing :D)


[Edited on 18-10-2010 by spong]

HexJam - 18-10-2010 at 06:43

Great post, think I might try this myself!

mr.crow - 18-10-2010 at 09:54

Very Good

NMP can also substitute for DMSO and doesn't turn stinky over time.

spong - 18-10-2010 at 18:12

After leaving the bottle overnight, two layers have formed, they're very hard to notice but I had worried about that when I poured it into the flask, it didn't pour like a pure substance. The top layer, I'm pretty sure is limonene, it doesn't smell as nice as limonene but that's probably because it's mixed with NMP fumes. I moved a small amount of each liquid into a test tube, water was added which caused an obvious separation of the layers, the cloudy water/NMP in the bottom and the limonene on the top. The top layer was removed, it burned just like limonene, sooty orange flame, quite flammable. The bottom layer had the water boiled off and burned with a clean, weak blue flame. I'm going to do some reading and make sure no azeotropes of water/NMP are formed but if not I'll do the same on a larger scale, boiling the water off then vac distilling the NMP over.
The label did say 60% NMP (There is no MSDS for this product), I had assumed the rest was polymer but they mean 60% NMP and 40% limonene, the polymer doesn't count apparently. It's the same with 87% DCM and 13% MeOH in another paint stripper.
EDIT:
I removed the limonene from the rest of it, around 30ml water was added to the mix in a separatory funnel, the bottom layer was kept and the limonene drained off into another jar until I find a use for it.
Mix before water (the border between the layers is just barely visible)


After addition of water:


Separated:


Vac distilling again(this was a huge pain in the ass, I used a capillary tube to stop bumping but the hole was a bit too big and because of the water present it would not cleanly boil for some reason, eventually the water boiled off and only the NMP was left, not much of the water was separated though, it will have to be dried thoroughly with a dessicant before use)


Finished:


When I distill the rest of the can I think I'll skip the addition of the water and just try to separate the layers, either carefully in a funnel if the limonene is not soluble in the NMP or by fractional vacuum distillation if it is.

[Edited on 19-10-2010 by spong]

Magpie - 18-10-2010 at 18:17

Nice work, spong. This looks like an interesting solvent that may I may well need sometime. Does anyone know what US brands of paint stripper use NMP as solvent?

Magpie - 19-10-2010 at 09:37

FYI, here's one US product, complete with orange dye, citrus smell, esters, gel, and an MSDS:

http://www.wmbarr.com/citristrip/default.aspx

I have no idea how difficult it would be to isolate NMP from all the other additives in Citristrip.

mr.crow - 19-10-2010 at 11:23

Gorilla PVC Glue in the states also uses NMP

You can mix the glue with water to get rid of the plastic resin, boil off the water and vac distill.

Eclectic - 19-10-2010 at 11:34

isopropanol and salting out works for separating the NMP from the methylcellulose? thickener.

entropy51 - 19-10-2010 at 11:36

Ye gods and little fishes!

Screen names for the members I can understand, but now screen names for the chemicals?:D

A thread about a useful chemical on a chemistry forum, and nowhere was anyone polite enough to mention that ugly word "N-Methyl-2-pyrrolidone ", which is what I think you guys are talking about. If you must use acronyms, at least define them the first time used.

Magpie - 19-10-2010 at 13:08

Yes, I had to look it up too, by searching paint strippers. NMP is all over this board so I thought I must be the only one who doesn't know what it is.

BTW entropy, you will be glad to know that I'm now tending a little batch of sulfanilic acid per Brewster.

entropy51 - 19-10-2010 at 14:34

Quote: Originally posted by Magpie  

BTW entropy, you will be glad to know that I'm now tending a little batch of sulfanilic acid per Brewster.
Yes! I finally ran a Brewster prep before Magpie.:D

I'm sure you will get a higher yield, however.:(

Did you distill your aniline first? If not, your product may be a tad off-color.

spong - 19-10-2010 at 17:02

Quote: Originally posted by Magpie  
FYI, here's one US product, complete with orange dye, citrus smell, esters, gel, and an MSDS:

http://www.wmbarr.com/citristrip/default.aspx

I have no idea how difficult it would be to isolate NMP from all the other additives in Citristrip.

That sounds almost identical to the one I had, NMP (or n-methyl-pyrrolidone to you entropy :P) limonene, orange dye and thickeners.