Newbee P-Benzo wacker ?

[BlingBling]

Just wondering something here.

A friend called me from his hot air balloon and asked me if I knew why his organic/ketone matter solidifies once cooled.

I wasn't to sure on what to tell him. He told me he was distilling a wacker, 300ml's of organic/ketone left, all fractions but the ketone remained.

He used an oil bath, for he is able to judge the bath temp by way of thermometer, and how erect he is.

He never went over 141c, and finaly threw his hands up in the air and yelled "mannnnn what the fuck!!!"

So, he decided to remove the 300mls out of the 1L flask, and transfer to a 500ml flask, then proceed using a vigeroux column to prevent bumping.

WELLLP, when he poured the (60°c) THICK organic/ketone out of the 1L, it kinda came out like mollases, but a little faster. A shit load stuck to the side, and luckily he had some DCM in the balloon or he would of lost the few ml's that may have otherwise got tossed.

Im thinkin crack kills.


Does anyone else decide to play with their P-Benzo organic/ketone mid stride during a fractional distillation?  Same consistancy? Are you lying? Please, share with me.

I am not interested in what your black tar looked like before the safrole was removed.. im talkin, mdp2p and Organic CRAP that can suck it for hours!

Also, while im a little roll here, how many 10% Naoh washes can you give without decomposing your goods? I would like to try 100, and mayyyybe, just maybe, a distillation can take place without worying about excessive bumping.. please?

[Rhodium]

Read

Post 370929 (missing)

(Rhodium: "Recovery of solidified/tarry MDP2P", Newbee Forum) and the other posts in that thread.

[SPISSHAK]

What kinda crack are you smokin' ?
Sounds like some good stuff, let me try some.
That shit you wrote was damn near incomprehensible.
But if you're offering I'll toke, btw if ya want sum candy, you know wut's up.

[BlingBling]

Rhodium, I thought about taking polmerized shit and letting it sit in DCM, why I never actually did it, beyond me. I would think if enough DCM was added, it would eventually break down, and be distilable again. It kinda hurts when I think about it. Even if it just ended up being a learning experience. 

What about the 10% washes? How many do you think you can do before you begin doing more damage than good?

The thought of washing the organic/ketone till it's practially light green is a happy thought I have in a happy little place.

It makes sense that eventually the 10% naoh washes will clean it up quite a bit, as 4+ washes keep resulting in a dark polar layer. How many more washes can you do? Has anyone ever washed their ketone/organic collection 10+ times? 20+ times? I think it would eventually be an easier task as the layers become more visable from the hydroquine being removed with the washes.

When re-distilling ketone for 100% purity, the distillation goes smoother than Spisshak's ass. (a bit rugged) It would be nice to wash up the organic/ketone to the point where the washes aren't visably showing signs of hydroquine removal. If it's possible. I dont want to try it if ultimately im going to damage my oil. Has anyone tried this???

[Rhodium]

You don't need to add DCM to be able to distill partly polymerized, solidified ketone. If there is still any free MDP2P in there, it will cause the solid to melt when heating it in the distilling flask. It could be of very much use though if you want to transfer it from one flask to another.

The base washes - it is effective as long as the washes are more colored than the organic solution itself. After that, it is mostly just a waste of time. It doesn't matter if you so wash the ketone 143 times with 10% NaOH, it won't become significantly purer after the first 3-5 washes. Let's say that each wash removes 80% of the base-soluble impurities present in the organic layer. Then the amount of these impurities left after a certain number of washes is like follows:

0: 100%
1: 20%
2: 4%
3: 0.8%
4: 0.16%
5: 0.03%

As you see, there is not much use carrying on after doing three washes. Also, there is also a whole lot of colored impurities which are NOT soluble in aqueous NaOH anyway, so trying to remove all the color through washing is futile.

[SPISSHAK]

When you wash do you go staight to NaOH? or do you wash first with saline or bicarbonate?
The reason behind this is that the first wash has a nasty tendancy towards emulsions, you can also overcome this by gently swirling the two layers of the first wash in the sep funnel, as opposed to shaking which may result in an emulsion, also if your washing with base it's helpful to use dcm or another appropriate non-polar to seperate the phases and keep the organic layer a little dilute since it's in contact with a strong base which can do nasty things to it.
And my ass is as smooth as silk.

[BlingBling]

I see! Good thing I asked.

I didn't think that the NaOH washes were that effective. I suppose after 3, it would be a waste.

How is it that plain old h2o gets discolored when added? What about excessively washing with saline and bicarbonate? Another waste of time??

>>When you wash do you go staight to NaOH? or do you wash first with saline or bicarbonate?

Sometimes, depends on what's closest. Lately the DCM collections haven't been pooled in with the organic collection, but set aside to be distilled at a later date. I notice alot less emulsion, but have thought about what you said when doing this. I can see how the addition of DCM could be of use when determining which layer is which, and making the consitancy of the organic matter a little more manageable.

Upon distillation of the DCM collections that were gathered over 3 wackers, I expected about 100-125 ml's at most. I was impressed when 250ml's came over. It proved that DCM is similiar to a car pool that transports kids from point A-Z. A valuable chemical that I love to smell on occasion.

I suppose either way you look at it, you will have that emulsion to deal with. The DCM collections got a NaOH wash regardless, how the two are mixed, appears to determine how much emulsion you will have to play with.

I found that a beaker and a stir bar is a great way to minimize emulsion, gently stirring, but enough to mix both layers nicely. Not as nice as your smooth ass, but nice.

Thanx for the help, saved me a pointless time consuming experiment. (and alot of NaOH)

[Rhodium]

I didn't think that the NaOH washes were that effective. I suppose after 3, it would be a waste.

How is it that plain old h2o gets discolored when added? What about excessively washing with saline and bicarbonate? Another waste of time??

Don't quote me on "80%" being the exact figure, but it is at least somewhere between 50-90% (that doesn't matter really, with 50% extraction efficiency the numbers would be 100% -> 50% -> 25% -> 12.5% -> 6.25% -> 3.1%, that is five washes to remove over 95% of what can be removed. With the extraction efficiency being 90%, only two washes would be needed for 99% removal (100% -> 10% -> 1%).

The purpose of the sodium hydroxide washes is to remove the bulk of the hydroquinone and other acidic contaminants, while the purpose of the carbonate is to "pre-wash" the solution with a weakly basic solution so that certain surfactants like alkyl carboxylates are removed prior to the NaOH washes as to lower the risk of creating intractable emulsions. Brine washes of the non-polar layer dries it crudely by osmotic suction.