Pmk wash proceding dcm wash
- Thread starter Followme38
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If starting from p-oil you should wash with dilute naoh and brine and should be a orange/red-ish clear liquid. If you want cleaner I recommend vac distillation.
If you reacted with alkali then HCl, you wash with 5% naoh then water. Will look like honey....because there is water in the oil.
DCM is not neccesary. You can obtain a fairly pure oil from the new PMK, by washing with naoh while still hot. Its good enough.
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So you have powder PMK? or the oil that solidifies at room temp? if powder don't use ethanol.
Maybe you get thick stuff because you add too much HCL? how much did you add? what are your temps? Do you get a solution with separation, the oil being on the bottom?
Maybe you get thick stuff because you add too much HCL? how much did you add? what are your temps? Do you get a solution with separation, the oil being on the bottom?
Well i have the new pmk yes also the wax kind, first i start of by mixing it at 30 degrees celsius with ethanol and water, after 1 hour i add acid twice the amount on weight of the powder, on 75degrees celsius i keep it that way for 3 hours at the 2.5 hour mark the color of the mix changes, after evaporation the oil gets like honey thick see videos.
Too much acid.
you must wash with naoh solution and water, will clean it up. It looks like you didnt wash it and also added too much acid I think. I didn't know the powder was a 2step conversion.
you must wash with naoh solution and water, will clean it up. It looks like you didnt wash it and also added too much acid I think. I didn't know the powder was a 2step conversion.
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I think you just need to wash that. Use less hcl next time..should have washed it right away. You probably got 10-15% poo in that oil thats why its thick. You get like 2.5L of dark water on the naoh washes. All of that is still in your oil I'm sure its mostly due to not washing..you seem to have it right but only add enough hcl for reaction and do the wash right away. If the oil doesn't sep and is dissolved in ethanol or something then idk i guess heat and stir to distill off ethanol then do da washy wash
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Good day my friend did as you said, i used half as hcl equel amount with powder on weight now, and washed it with naoh 5% solution the water went dirty directly reddish see picture, after that did a water wash, the oil got thin as you said, there is just to much junk in the new powder i guess yield is like 65% on weight chinese sell it like 75% yield 
)) on timing i dont know yet i did 1.5 hours saponification, and 3 hours stirring with acid on 75 degrees C. Only the oil comes out dark is this due to the new powder?
)) on timing i dont know yet i did 1.5 hours saponification, and 3 hours stirring with acid on 75 degrees C. Only the oil comes out dark is this due to the new powder?Attachments
I think each time you do a conversion it will get better. I got dark stuff first few times but now get a light-colour oil more brown/yellow or like honey. Clear.
BTW idk much about powder I'm just trying to help
You have to use quite a bit of Naoh water on your wash.. And also you have to dehyrdate you oil then it will turn clear.
BTW idk much about powder I'm just trying to help
You have to use quite a bit of Naoh water on your wash.. And also you have to dehyrdate you oil then it will turn clear.
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Oil usually comes out dark and requires VAC distillation its a standard thing, you really want your ketone to be of highest purity because impurities can mess with the synth and dramatically effect yeild but I think with practice from pmk you should be goos to go without VAC distill just practice your purification.
If your new yeild is the same oil you showed in the previous post then you might not be able to get that oil clean that easy.. Its much easier when its still hot directly after the conversion IMO.
If your new yeild is the same oil you showed in the previous post then you might not be able to get that oil clean that easy.. Its much easier when its still hot directly after the conversion IMO.
Yes i did a single naoh wash only, but i dont know how it will come out with 2 washes and how much wash do you use normally lets say on 50gr oil how much wash and as you say yes without vacuum destillation its dark, and later on when you try to clean it after it cools down its impossible almost to clean as you say. yield is also low something like 50% oil you get out of it older pmk was like 58-60% oil
1eq NaOH and excess acid. 80*C approximately for boiling with acid, with alkali, the reaction is best done at room temperature and longer. 75-85% oils usually. Saponification stage - you need to take the equivalent of sodium hydroxide, make it a solution and cool. Add to glycidate and leave with stirring overnight.