PMK Oil Synthesys From PMK (CAS 28578-16-7 Wax Form) Large Scale

[Selassi]

1kg P
1kg water
150gr NaOH

Mix and melt at 85/90 for 1hr

450gr Phos and again 1,5hr at 85/90

After should be immediate separation from the layers

 

[Katty Korner]

1kg P
1kg water
150gr NaOH

Mix and melt at 85/90 for 1hr

450gr Phos and again 1,5hr at 85/90

After should be immediate separation from the layers

SelassiThis seems way more dense than the starting post. 1 kilo of pmk glycidate, 1 kilo of water (which iirc is one liter) and 150 grams naoh seems much denser than other posts.

It'd be much nicer if it was that dense, instead of requiring gallons for a few kilos.

Anyone care to say if this can be done at this density, or concentration of reagents?

 

[btcboss2022]

Hello,

Here is my last achievement make it to crystallize naturally in the molecular form of the crystal itself. More pure impossible!! ;-)
Seems handmade but trust me are naturally formed!

 

[Tweaker]

Hello,

Here is my last achievement make it to crystallize naturally in the molecular form of the crystal itself. More pure impossible!! ;-)
Seems handmade but trust me are naturally formed!

btcboss2022Very nice work. What process do you use to remove the black tar like impurity? Even on snow white crystals it appears on subsequent recrystalizations and the end product becomes quite dark.

 

[btcboss2022]

Very nice work. What process do you use to remove the black tar like impurity? Even on snow white crystals it appears on subsequent recrystalizations and the end product becomes quite dark.

TweakerIn the acid stage during the acid base washing process.

 

[btcboss2022]

Okay thanks sounds like powder is the way to go. I have a sample amount of powder the conversion method is identical to wax?

TweakerYes exactly the same.

 

[Paranoia]

Yes exactly the same.

btcboss2022Coming next in a few weeks @btcboss2022 ice sample lab test https://analisis2.energycontrol.org/ for meth purity and eniantometer R.S

 

[lemon]

I've been trying this for a while and I came to the conclusion that I was most likely scammed.
When I add NaOH whole solution get dark and it just stays like that, after heating nothing happens, just after adding too much of acid then glycidate reappears again. After heating I get dark red oil which quickly became solid when cold. Even when heating glycidate just in water i get same dark red oil.
I already wasted 200g of this and even tried reduction with it and nothing...
I even don't know if this is PMK glycidate or chinese scammed me.
About solubility: it's insoluble in water and highly soluble in IPA

 

[UWe9o12jkied91d]

I've been trying this for a while and I came to the conclusion that I was most likely scammed.
When I add NaOH whole solution get dark and it just stays like that, after heating nothing happens, just after adding too much of acid then glycidate reappears again. After heating I get dark red oil which quickly became solid when cold. Even when heating glycidate just in water i get same dark red oil.
I already wasted 200g of this and even tried reduction with it and nothing...
I even don't know if this is PMK glycidate or chinese scammed me.
About solubility: it's insoluble in water and highly soluble in IPA

lemonHow long did you reflux with 3M NaOH?

 

[Loki12]

I've been trying this for a while and I came to the conclusion that I was most likely scammed.
When I add NaOH whole solution get dark and it just stays like that, after heating nothing happens, just after adding too much of acid then glycidate reappears again. After heating I get dark red oil which quickly became solid when cold. Even when heating glycidate just in water i get same dark red oil.
I already wasted 200g of this and even tried reduction with it and nothing...
I even don't know if this is PMK glycidate or chinese scammed me.
About solubility: it's insoluble in water and highly soluble in IPA

lemon@lemon
Who have you purchased this from? If it was one of the vendors advertising here you should name them, to clarify the situation.
1. Did you heat the mixture with NaOH and reflux it like the above user asked? Can you please describe your method further, step by step, what you actually did? (ex. I added 100g of x to 50g of y, refluxed at X for Y time)

Maybe there is nothing wrong, why are you posting the glycidate in water, this is hilarious??
We need to know if you proceeded with the reaction, what background do you have? Have you researched the reaction, do you know what is supposed to happen even or what is supposed to look like?
Saponification and chem texts was linked somewhere in this thread if I am correct, please read, understand the reaction, have an idea of what to expect, then proceed with it.
Not only is chemistry dangerous, but without a general idea of what you are doing, you will only waste product, possibly you will poison yourself with the conc. HCL or the DCM used in this reaction, please take care.

 

[Jordan Belfort]

I've been trying this for a while and I came to the conclusion that I was most likely scammed.
When I add NaOH whole solution get dark and it just stays like that, after heating nothing happens, just after adding too much of acid then glycidate reappears again. After heating I get dark red oil which quickly became solid when cold. Even when heating glycidate just in water i get same dark red oil.
I already wasted 200g of this and even tried reduction with it and nothing...
I even don't know if this is PMK glycidate or chinese scammed me.
About solubility: it's insoluble in water and highly soluble in IPA

lemonBrother, you can redo the failed reaction.

Take 1L hot water, use 500 gram caustic, on the hot lye one kg of the glydicate and I don't know pour slowly 1.5L hydrochloric acid it will 100 percent come. Then oil goes to the bottem once successfully turned you don't need to reflux

 

[Jordan Belfort]

I've been trying this for a while and I came to the conclusion that I was most likely scammed.
When I add NaOH whole solution get dark and it just stays like that, after heating nothing happens, just after adding too much of acid then glycidate reappears again. After heating I get dark red oil which quickly became solid when cold. Even when heating glycidate just in water i get same dark red oil.
I already wasted 200g of this and even tried reduction with it and nothing...
I even don't know if this is PMK glycidate or chinese scammed me.
About solubility: it's insoluble in water and highly soluble in IPA

lemonWhats the cas number of the glydicate, if its the low hield p then this method doesnt work you will burn the oil

 

[bblanco]

But Uhm did you started with wax or powder ? Simple small test. 5gr naoh in 75 Mill water disolve ,add 5gr wax melting, reflux an Hour add hcl or h2so4 and reflux gentle 3h.. then should be ok

 

[Davidrobinson]

Can anyone help me out ,
I messed up my pmk sap and hydrolysis well I messed up one and don’t know which one.
I messed the temps up , I ran the sap at 52 degrees instead of 60 and then ran the hydrolysis at 70degrees instead of 80.
I put around 4.4kg of powder in and got ou near enough the same in a orange dull oil.
Does anyone know if the oil is salvageable , my thinking was the hydrolysis was messed up , doesn’t sap happen straight away even at room temp.
Does anyone know if I can just run the sap and hydrolysis again on the oil.
Thanks

 

[Jordan Belfort]

Can anyone help me out ,
I messed up my pmk sap and hydrolysis well I messed up one and don’t know which one.
I messed the temps up , I ran the sap at 52 degrees instead of 60 and then ran the hydrolysis at 70degrees instead of 80.
I put around 4.4kg of powder in and got ou near enough the same in a orange dull oil.
Does anyone know if the oil is salvageable , my thinking was the hydrolysis was messed up , doesn’t sap happen straight away even at room temp.
Does anyone know if I can just run the sap and hydrolysis again on the oil.
Thanks

kangarooIf you add enough caustic, you can add a acid like HCL and keep stirring, the reaction will go on itself.

 

[Win Win]

Hello,

After check and test the methods posted in the thread http://bbzzzsvqcrqtki6umym6itiixfhn...-methyl-pmk-glycidate-conversion-to-pmk.2013/ I decided the post the best method for me:

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.
2. Put in the reactor 7L of H2O
3. Add while stirring 1,2kg of sodium hydroxide
4. While the H2O and the sodium hydroxide are mixing and getting temp put 5kG of wax PMK to melt by low heat.
5. When PMK is melted add it to the reactor and put the mixture at 80 °C reflux during 1 hour stirring.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.
7. Stop stirring and put the mixture at 25 °C.
8. Discard the water top layer.
9. Put again in the reactor the oil top layer.
10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.
11. Add 10 liters of DCM (from freezer preferably).
12. Let it get separated around 10-15 min.
13. Evaporate DCM from the bottom layer.

PMK oil (MDP2P; cas 4676-39-5) yield is 3,72kg.

btcboss2022May i know the ration of iterm 10? Thank you

 

[btcboss2022]

May i know the ration of iterm 10? Thank you

Win Win???Is the point 1!

 

[Win Win]

Hello,

After check and test the methods posted in the thread http://bbzzzsvqcrqtki6umym6itiixfhn...-methyl-pmk-glycidate-conversion-to-pmk.2013/ I decided the post the best method for me:

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.
2. Put in the reactor 7L of H2O
3. Add while stirring 1,2kg of sodium hydroxide
4. While the H2O and the sodium hydroxide are mixing and getting temp put 5kG of wax PMK to melt by low heat.
5. When PMK is melted add it to the reactor and put the mixture at 80 °C reflux during 1 hour stirring.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.
7. Stop stirring and put the mixture at 25 °C.
8. Discard the water top layer.
9. Put again in the reactor the oil top layer.
10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.
11. Add 10 liters of DCM (from freezer preferably).
12. Let it get separated around 10-15 min.
13. Evaporate DCM from the bottom layer.

PMK oil (MDP2P; cas 4676-39-5) yield is 3,72kg.

btcboss2022May i know this ratio of this (10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.)

 

[btcboss2022]

May i know this ratio of this (10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.)

Win WinOMG is in the point 1!

 

[Win Win]

OMG is in the point 1!

btcboss2022Mean the ration same with iterm 1 right

 

[Win Win]

Hello,

After check and test the methods posted in the thread http://bbzzzsvqcrqtki6umym6itiixfhn...-methyl-pmk-glycidate-conversion-to-pmk.2013/ I decided the post the best method for me:

1. Put 47,5 liters of H2O in the reactor and add 2,5kg of sodium bicarbonate, stirring until complete dissolution, take out the mixture and keep it.
2. Put in the reactor 7L of H2O
3. Add while stirring 1,2kg of sodium hydroxide
4. While the H2O and the sodium hydroxide are mixing and getting temp put 5kG of wax PMK to melt by low heat.
5. When PMK is melted add it to the reactor and put the mixture at 80 °C reflux during 1 hour stirring.
6. Add 3,25kg of HCL 37% in small portions, once all added keep the mixture at 80 °C reflux during 1 hour stirring.
7. Stop stirring and put the mixture at 25 °C.
8. Discard the water top layer.
9. Put again in the reactor the oil top layer.
10. Add the H2O and sodium bicarbonate mixture, stirring 2-3 minutes.
11. Add 10 liters of DCM (from freezer preferably).
12. Let it get separated around 10-15 min.
13. Evaporate DCM from the bottom layer.

PMK oil (MDP2P; cas 4676-39-5) yield is 3,72kg.

btcboss2022No.10 add how many h20 and how many sodium bicarbonate solution?

 

[btcboss2022]

Incredible

 

[blackburn]

 

[axecap168]

Btcboss2022, please help I followed your recipe for synthesis of pmk 28578-16-7 powder to mdp2p and after refluxing oil separation occur but there was still some white cloudy stuff in the oil and as the oil cooled the white cloudy stuff became thicker like soggy cereal and left me with very little oil.
Has anyone seen this happen before?
What did I do wrong btcboss2022?
Can anyone help me with this?
I have attached some photos.

 

[btcboss2022]

Btcboss2022, please help I followed your recipe for synthesis of pmk 28578-16-7 powder to mdp2p and after refluxing oil separation occur but there was still some white cloudy stuff in the oil and as the oil cooled the white cloudy stuff became thicker like soggy cereal and left me with very little oil.
Has anyone seen this happen before?
What did I do wrong btcboss2022?
Can anyone help me with this?
I have attached some photos.

axecap168OMG! Should be destiny or something similar hahhaah
I never had any issues in more than one year with that process and last week happened me the same with a 15kg powder batch(was the last 15kg of a large batch so same product)
I'm at 99% sure that is about storage and storage time, in my case I stored in a bucket with lid around 6 months.
I isolated that solid that seems a kind of polymerization of the original stuff.

I tested with what product it gets solved:
Water: No
Acid water: No
Alkali water: Practically nothing
DCM: No
Methanol: Practically nothing
Acetone: No

Strange right? It only gets liquid at high temp or with hot water similar to the original stuff so the only 2 options are:
- Unreacted product ( very improbable after hundreds of times of performing the same process also with the same batch, and it must be solved in alkali water too)
- A kind of polymerization due the storage time and conditions.

You can try more time at 90C with the HCL but I guess it wont works.

What I did( don't means that is the solution or that you must do the same)

I added water stir it and later DCM and all in a separator funnel.
You will have the top layer water, middle layer the solid and bottom layer the DCM+PMK oil later later evaporate DCM.
It is a slow separation and I did it 3 times with DCM.
Obviously the yield is much lower than normally but better this than nothing.

I'm sorry couldn't help you more I had the same problem and I tried to fix it as best I know using the common sense and my previous experiences.

Possibly a chemist would help you in a better way.

 

[axecap168]

Btcboss2022, please help I followed your recipe for synthesis of pmk 28578-16-7 powder to mdp2p and after refluxing oil separation occur but there was still some white cloudy stuff in the oil and as the oil cooled the white cloudy stuff became thicker like soggy cereal and left me with very little oil.
Has anyone seen this happen before?
What did I do wrong btcboss2022?
Can anyone help me with this?
I have attached some photos.

axecap168Belfort, thats correct reaction with HCL.