# Pmk wash proceding dcm wash



## Followme38

Hello was wondering how to proceed with a dcm wash on a ketone, and what are the steps and ratios on pmk to make it cleaner, and is it possible to perform is on with a water bath


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## Gale

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.


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## Followme38

Gale said:


> 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.



GaleProblem is the new pmk oil, the steps are different also i get a honey like oil all the time wich is unusable


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## Gale

Followme38 said:


> Problem is the new pmk oil, the steps are different also i get a honey like oil all the time wich is unusable



Followme38

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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## Followme38

Can you write down exact steps for me tried everything by now and still not getting good oil but rather some honey like substance, dark brown..


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## Followme38

Lets say i begin with 50 grams of powder what are the exact steps with what chemicals to obtain good oil with the new pmk old pmk was like gold this one is different


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## Gale

Followme38 said:


> Lets say i begin with 50 grams of powder what are the exact steps with what chemicals to obtain good oil with the new pmk old pmk was like gold this one is different



Followme38So 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?


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## Followme38

Gale said:


> 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?



GaleWell 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.


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## Gale

Followme38 said:


> After 1 hour i add acid twice the amount on weight of the powder



Followme38Too 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.


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## Gale

what was your yeild?


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## Followme38

Gale said:


> what was your yeild?



GaleYield was like 72% on weight, and yes did not wash after, how much acid is needed and how much water ethanol at first part?


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## Followme38

And timing and degrees if you have suggestion


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## Gale

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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## Followme38

Gale said:


> 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



GaleGood 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?


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## Gale

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.


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## Gale

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.


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## Followme38

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


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## Followme38

And how much alkali and acid do you use? and do you have proper timings and temperature what is best?


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## William Dampier

Followme38 said:


> And how much alkali and acid do you use? and do you have proper timings and temperature what is best?



Followme381eq 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.


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## William Dampier

For acid - if there is indicator paper (pH-metr), control with it pH (<= 3)


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## Gale

Followme38 said:


> and later on when you try to clean it after it cools down its impossible almost to clean as you say.



Followme38Its more difficult because you let it sit with a bunch of rxn impurities and it causes some damage I'm fairly sure.

Will says to stir overnight but try different durations to see what works best.. Again idk powder.


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## Followme38

Gale said:


> Its more difficult because you let it sit with a bunch of rxn impurities and it causes some damage I'm fairly sure.
> 
> Will says to stir overnight but try different durations to see what works best.. Again idk powder.



GaleThis is the wax i guess that comes out light yes if you stir it at room temperature not hot, when its hot the color changes quite a bit, and acidifying stage also different, what was your yield? Also like 50% i guess based on oil so 100gram wax yields 50ml of oil give or take.


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## Gale

I would assume the powder should come out cleaner. Oil usually come out very dark from the wax but over time method improved and now have cleaner results, mainly due to washing procedure. Yeild is about 60% but could be higher maybe.


Please go over the process closely for the first rxn.

Can you post video of your new yeild


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## Followme38

Gale said:


> I would assume the powder should come out cleaner. Oil usually come out very dark from the wax but over time method improved and now have cleaner results, mainly due to washing procedure. Yeild is about 60% but could be higher maybe.
> 
> 
> Please go over the process closely for the first rxn.
> 
> Can you post video of your new yeild



Galei have washed it 3 times it does not get any lighter see picture, tried every possibility, did not vacuum distill it, my yield is 60% on weight after 50 grams of powder my final weight is 30 grams, tried it for 4 times now yield does not go up i think this new powder is much lower quality compared to the pmk last year that came out golden always, the reaction is ok but after a while the oil gets darker and darker, how much noah do you use at the beginning? and how much acid 37% on weight of wax/powder? i add a picture with wax extraction at the right powder on the left i kept my temperature like 78-80 degrees


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## Gus_Fring

Gale said:


> 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.



Galei promise i did that...but same resulkt...this brwn dirty oil.... what im doing wrong?
so... it seems i have the same problem as many people has... the new ETHYL GLY is hard to get proper results...i have the same issue as other posts here, this brown dense oil which looks very dirty... the recipe i followed:

-MIX 1.4 LT water and 240 gr NaOH and 1 kg eth-gly-pmk at 80º for an hour
- add 650g HCL at 80º mix an hour too (is not too muich hcl?)
-then separator
-then brine wash+ water wash 2 times 
-separator
-then vacuum distill (not done yet because i didnt be sure that ive made ok) 
-then separator , thats to remove acidity (why...i already did the brine.... dont know)
-then again 500 ml water and separator
-the vacuum distill till all water goes
-voila


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## Gus_Fring

Gale said:


> 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



Galehow much HCL you would use?


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## Bennyboy88

Gale said:


> Its more difficult because you let it sit with a bunch of rxn impurities and it causes some damage I'm fairly sure.
> 
> Will says to stir overnight but try different durations to see what works best.. Again idk powder.



Gale


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## Bennyboy88

Do you mind sharing your method for the wax. It great appreciated. Thx in advance


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## William Dampier

Those who get the oil dark, try the stage with alkali at a temperature of 20*C, and within 12 hours or more.


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## Albert

Hello everybody,
I am new to the forum.
I had a similar problem I think.
After hydrolyzing PMK glycidate cas: 13605-48-6 for an hour and a half with HCL at 80 C degrees, I separated the oil from water in a separatory funnel and then cleaned from residual water with zeolite 3A for a whole night.
After finishing the process, I added methanol to the PM and left the oil in a closed flask at room temperature for several weeks.
The mixture became brown and you can see several crystals at the bottom.
How long do you think PMK oil can be kept at room temperature and can the situation be corrected?


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## Albert

It is important to note that at the end of the pmk glycidate hydrolysis process, the oil turned out a beautiful yellow like honey and turned brown only after a few weeks.


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## G.Patton

Albert said:


> After finishing the process, I added methanol to the PM and left the oil in a closed flask at room temperature for several weeks.
> The mixture became brown and you can see several crystals at the bottom.



AlbertHello. Did you use dark glass flask and dark place (like a cupboard)? Was this flask closed tightly, without air exposure?


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## Albert

G.Patton said:


> Hello. Did you use dark glass flask and dark place (like a cupboard)? Was this flask closed tightly, without air exposure?



G.PattonIt was a transparent glass flask, in a room where the sun penetrates through the window (quite a bright place) but no direct sunlight.
It was quite hermetically sealed.


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