btcboss2022

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May I ask what method you use to crysyalize the final product?
CuriousonionBefore crystalize you must get the freebase, for freebase I use NaBH4 method and to crystalize the freebase there are a lot of methods.
 

RotterdamNL

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Have you hear about your conversion (from first page this topic) made in 316l ss? I ask becouse in reaction before adding hcl - its sodium salt form, and IF somebody add Acid maybe ph is 2-3
, not strong 1 and hcl maybe dont eat 316 or little eat. Citric Acid if Works I think is the best route for 316 steel
 

btcboss2022

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Have you hear about your conversion (from first page this topic) made in 316l ss? I ask becouse in reaction before adding hcl - its sodium salt form, and IF somebody add Acid maybe ph is 2-3
, not strong 1 and hcl maybe dont eat 316 or little eat. Citric Acid if Works I think is the best route for 316 steel
RotterdamNLIn my case I use a glass reactor. In acidification stage citric acid should work in molar ratio equivalent.
 

G.Patton

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@btcboss2022 Interesting fact, I've counted your yield 3.72 kg in accordance with molar equation, and have got a curious result that it's 105% yield. Theoretical 100% yield is 3557g.
There are to options why it happens: the yield oil isn't pure, your description/calculation mistake.
 

btcboss2022

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@btcboss2022 Interesting fact, I've counted your yield 3.72 kg in accordance with molar equation, and have got a curious result that it's 105% yield. Theoretical 100% yield is 3557g.
There are to options why it happens: the yield oil isn't pure, your description/calculation mistake.
G.PattonPossibly wasnt enough pure at that times, were the firsts synthesis using that method and I didnt have the same knowledge than now, it was long time ago.
But the oil that I got weight that for sure anyway hahaha with impurities possibly but all them cleaned in the next processes so no problem.
Nowdays I have other working methodollogy.
I will weight it again next time I do it and we can compare.
Thanks.
 
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G.Patton

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Possibly wasnt enough pure at that times, were the firsts synthesis using that method and I didnt have the same knowledge than now, it was long time ago.
But the oil that I got weight that for sure anyway hahaha with impurities possibly but all them cleaned in the next processes so no problem.
Nowdays I have other working methodollogy.
I will weight it again next time I do it and we can compare.
Thanks.
btcboss2022
Nowdays I have other working methodollogy.
Can you share us new one?
 

AKWA

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Can you share us new one?
G.PattonThought to ask the same but frankly I feel like if he wanted to share he could have already done that right around the time he found this new method.
I’m not stressing though, he has contributed valuable data already on his previous conversions and I feel that’s already enough.
 

btcboss2022

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Can you share us new one?
G.PattonI have to be honest, and I like to be clear.
The truth is that I don't find it fair to share every improvement, change, or method for free (something I have often done willingly).
It's for a simple and logical reason: every improvement or change, at least in my case, represents a significant investment of time, money, and effort.
I am not sharing procedures or documents that I found (which I appreciate from those who do, and I don't criticize it, quite the opposite).
In this case, what is being shared is the final result of hard work, and I believe that making it freely accessible to everyone devalues and distorts that work.
I could share info in private way with who helped and help me and with people who publish some of their works too but no publicly.
Anyway, no one can say that I haven't answered a question about the procedures I have published, both privately and publicly. One thing doesn't exclude the other.
Similarly, I would say that all the important or basic procedures are published on the forum, and anyone who wants to could do them without needing anything else. In fact, I have done many of them myself.

As I always say, this is my personal opinion, and anyone is free to think otherwise and do what they want or believe without any problem.
Even thinking about the easy and obvious idea that I am selfish and only doing it for money/business, etc., when if that were the reality, I assure you I would have stopped doing this a long time ago.
Taking advantage of the situation, I have the step-by-step live guidance service where I provide all the details, improvements, etc... ;-) (as if I wouldn't, right? hahah)
and by the way, its price is well below its value in the underground cost in Europe, at least, if you can find such a service, which is the most difficult part, I believe.
Now, looking at it with hindsight, honestly, I would have paid almost any price to have access to something like this. It's clear that I have learned a lot, and no one can take that away from me. However, all the time, effort, and money I would have saved would be almost incalculable, I would say.

My opinion may be liked more or less, but it is entirely coherent, sincere, and common sense. Besides, I continue to write, express opinions, give tips, and answer questions – that's not the issue. I think it has been well understood. Personally, I appreciate everything you do.
 

Win Win

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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.
btcboss2022Hi sir can i use this method
1. Add 100 ml of ethanol to 100 g of PMK powder and then add 100 ml of distilled water and then seal and stir at room temperature for 90 minutes until it becomes a little powdery.
2. Filter the liquid (weigh the powder) and add hydrochloric acid at a ratio of 1:2
3. Pour the powder into the reaction kettle, add hydrochloric acid, start stirring, raise the temperature to 75 degrees, and stir for 3 hours. You will see a dark oily substance.
4. Take out the oil and use it for the next step.
 

Win Win

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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.
btcboss2022I want to ask if this recipe works.
 

subzero

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What is best yielding acid to use for this method?
HCL, Phosphoric... ?
 
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undefinied0

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Please, someone help I might have made a mistake.

I followed everything up to point 12, but the bottom DCM layer was very cloudy, white, and thick. I discarded the upper aqueous layer, which was slightly brownish. In one of the pictures, the separating funnel contains the lower white DCM layer that I kept.

From reading the comments, I saw that they suspected spoilage. Mine had also been standing for about a year but was vacuum-sealed in a relatively cool place at around 20 degrees Celsius.

In another comment, I read that it's worth adding phosphoric acid because it's likely too basic. I checked with an indicator, and it indeed showed blue.

After adding the phosphoric acid, I mixed it and slightly raised the temperature, but the DCM is still in it, so I didn't raise the temperature enough for it to evaporate. This is what it looks like now, as shown in the second picture.

What would you suggest, what should be the next step?
 

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G.Patton

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Please, someone help I might have made a mistake.

I followed everything up to point 12, but the bottom DCM layer was very cloudy, white, and thick. I discarded the upper aqueous layer, which was slightly brownish. In one of the pictures, the separating funnel contains the lower white DCM layer that I kept.

From reading the comments, I saw that they suspected spoilage. Mine had also been standing for about a year but was vacuum-sealed in a relatively cool place at around 20 degrees Celsius.

In another comment, I read that it's worth adding phosphoric acid because it's likely too basic. I checked with an indicator, and it indeed showed blue.

After adding the phosphoric acid, I mixed it and slightly raised the temperature, but the DCM is still in it, so I didn't raise the temperature enough for it to evaporate. This is what it looks like now, as shown in the second picture.

What would you suggest, what should be the next step?
undefinied0
I discarded the upper aqueous layer, which was slightly brownish.
Are you sure that it was aqueous layer? Cuz it looks like you discarded your PMK layer. Water layer can be on the bottom in case of over-saturated solution with density bigger that PMK DCM layer.
 
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undefinied0

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Are you sure that it was aqueous layer? Cuz it looks like you discarded your PMK layer. Water layer can be on the bottom in case of over-saturated solution with density bigger that PMK DCM layer.
G.Pattonhmm sounds good..it can be sadly.. but is it possible to extract so much pmk from the aqueos layer what i kept
accidentally, after adding poshporic acid to it? it looks to much for me there must be some DCM too but even with that.( start with 50g glycidate and end with 70ml theoretically PMK with DCM in it and it's only from the aqueos layer)

and Is the color okay?
 

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G.Patton

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hmm sounds good..it can be sadly.. but is it possible to extract so much pmk from the aqueos layer what i kept
accidentally, after adding poshporic acid to it? it looks to much for me there must be some DCM too but even with that.( start with 50g glycidate and end with 70ml theoretically PMK with DCM in it and it's only from the aqueos layer)

and Is the color okay?
undefinied0Probably there are some glycidate in water but not so much. I don't understand your English, to be honest. Please, reformulate your question clearly.
 

undefinied0

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Probably there are some glycidate in water but not so much. I don't understand your English, to be honest. Please, reformulate your question clearly.
G.PattonThank you for the answer! I apologize if I didn't express myself clearly. So, my question is: I apparently discarded the PMK layer and kept the aqueous layer. However, how is it possible that I was able to extract so much PMK from the aqueous layer by adding phosphoric acid? The total amount of PMK I started with was 50g, and after discarding the PMK layer, I extracted 70ml of PMK from the aqueous layer. Does this mean that what I prepared is not very pure, or is it possible to get this much PMK oil from 50g?
 

Loki12

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Thank you for the answer! I apologize if I didn't express myself clearly. So, my question is: I apparently discarded the PMK layer and kept the aqueous layer. However, how is it possible that I was able to extract so much PMK from the aqueous layer by adding phosphoric acid? The total amount of PMK I started with was 50g, and after discarding the PMK layer, I extracted 70ml of PMK from the aqueous layer. Does this mean that what I prepared is not very pure, or is it possible to get this much PMK oil from 50g?
undefinied0In the post above you mentioned that 70ml you extracted from the aqueous layer, most likely had DCM in it also. So subtract the DCM content buddy, then go ahead and vacuum distill whatever is left after you evaporate that DCM. Most likely your yield will not be as high as you think. However with slight modifications, an experienced cooking enthusiast should be able to get yields between 70-80% of dirty PMK from the glycidate. This is ofc less after performing vacuum distillation.

Usually when you count your yield, you do not add the volume of solvents to the product, get rid of the solvent first and then weigh what is left.
 

G.Patton

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Thank you for the answer! I apologize if I didn't express myself clearly. So, my question is: I apparently discarded the PMK layer and kept the aqueous layer. However, how is it possible that I was able to extract so much PMK from the aqueous layer by adding phosphoric acid? The total amount of PMK I started with was 50g, and after discarding the PMK layer, I extracted 70ml of PMK from the aqueous layer. Does this mean that what I prepared is not very pure, or is it possible to get this much PMK oil from 50g?
undefinied0
However, how is it possible that I was able to extract so much PMK from the aqueous layer by adding phosphoric acid? The total amount of PMK I started with was 50g, and after discarding the PMK layer, I extracted 70ml of PMK from the aqueous layer.
70 ml of PMK oil with DCM?

You can't make a pie with two apples out of one apple.

You need to repeat procedure and check the layers carefully on each step.
 

undefinied0

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I repeated the process with 150g glycidate as you and G.Patton said added the leftover aqueos layer from the last reaction got 100ml PMK after DCM evaporation but I didn't vaccum distill so maybe even less than 100ml.Thank you both for your advice!
 

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