Pmk wash proceding dcm wash

[Gale]

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.

 

[Followme38]

This 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.

 

[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

 

[Followme38]

i 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

 

[Gus_Fring]

i 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

 

[Gus_Fring]

how much HCL you would use?

 

[Bennyboy88]

 

[Bennyboy88]

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

 

[WillD]

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

 

[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?

 

[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.

 

[G.Patton]

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

 

[Albert]

It 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.