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making d-limonene Options
 
whitebread420
#1 Posted : 11/16/2011 7:16:20 PM
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I thought i would share something with you all the might be useful. it's a procedure on extracting d-limonene from orange peels. d-limonene is a basic terpene found in a lot of citrus peels.

so this technique makes very little product, it's out of my organic chem lab workbook, so basically everything we did in there was on such a small scale... basically just scale everything up (a lot .. like 100x) and you should get a good amount

take two oranges and peel them. try to scrape off all the white stuff on the inside. you just want the outer skin. put this in a blender until it becomes a slush and rinse it out with 120 ml's of dH20 into a round bottom flask. hook this up to a glass distillation kit, and heat it up until its boiling and collect about 40-50 mls of liquid. do not let solids accidentally splatter up into the condenser and contaminate your sample. this liquid (what you collect) contains d-limonene in an oil form and water. on top you should see the oil.

from this you wanna put what you collected in a sep funnel and wash it a few times with DCM, about 10 ml's each time. collect all your washes (the bottom organic layer) and dry it with anhydrous sodium sulfate. transfer the DCM into a vacuum flask, and wash the sodium sulfate with more DCM and put that in there too. upon vacuuming, you'll be left with a crude oil witch is d-limonene. DCM is used here because it evaporates really easy in a vacuum. sorry i don't have much more details on the purity or how to further purify it... in the lab we tested it by polarimetry and refractive index and got pretty good results (close to the accepted pure values)

like i said before this makes almost nothing ... seriously like 5 ml's of oil if you're lucky and to get a good amount you would have to scale this wayyyyy up.

i hope someone finds this useful. i don't think the fruit used has to be too specific. if you have a lime, lemon, or orange tree just clean up the peels as best as possible and grind em up. i imagine if you used 50 or more oranges you can get a good amount. during the steam distillation its just important to use excess water, since there is a lot of water in the peels themselves too.
 

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Limeni
#2 Posted : 11/16/2011 10:55:16 PM

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Interesting read whitebread.

I can't see I'll be doing it any time soon...but now I don't feel so bad about paying so much for it. Laughing
 
ChickenTikka
#3 Posted : 11/17/2011 1:17:19 AM

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If it came to this surely people would just go for a different solvent, but interesting to know anyway.

Perhaps if you have loads of orange trees nearby it could be worth while.
 
 
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