Simple steam distillation of P2P

GhostChemist

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Reagents and materials:

  • 145 ml of unrefined P2P obtained through the reduction of P2NP with borohydride
  • 300-400 ml of a 10% aqueous solution of potassium carbonate
  • 4 liters of distilled water
  • 500 ml (100 g of sodium chloride) of a 20% aqueous solution of sodium chloride
  • 1-liter, 2-liter, 500 ml, and 250 ml flasks
  • Beakers
  • Funnel
  • 2-liter separatory funnel
  • Ball-shaped condenser
  • Glass adapters
  • Teflon steam tube
  • Heater

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Performing the purification process of P2P through steam distillation

The flask for steam distillation is filled with P2P to be purified, and then it is half-filled with a pre-prepared solution of potassium carbonate. Fig 1
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A steam condenser is connected, and the entire setup for steam distillation is assembled. The amount of steam from the steam generator should be greater than what would be produced during the regular boiling of the P2P in the flask (i.e., the flask containing P2P should be smaller in volume than the steam generator). Fig 2
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The mass in the distillation flask is adjusted to achieve a uniform and constant boiling without hydraulic shocks (small boiling stones made of ceramic or glass are added to the flask to prevent bumping; in case of hydraulic shocks during boiling, a small amount of distilled water should be added to the flask to normalize the boiling process). Distillation is continued until there is no further delivery of water with oily droplets of P2P into the receiving flask. Fig 3
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Appearance of P2P in the distillation flask during the process. Fig
4
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In the distillation flask, heavy insoluble impurities remain at the bottom. Fig 5
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The water distilled along with P2P. Fig 6
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A solution of sodium chloride is prepared to facilitate the upward floating of P2P and to enhance the separation process. The distilled water with P2P is poured into a large separatory funnel, and the prepared sodium chloride solution is added. Emulsions are allowed to settle for a certain period (at least a couple of hours). The lower aqueous layer is then drained because it contains a small residual amount of emulsified phenylacetone, which can be reused for distillation with new portions of P2P. Fig 7
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The layer containing P2P is drained into a container with silica gel for drying and further use. Fig
8
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The obtained P2P is a product with a purity of not less than 99%. The distillation process takes 2 days, and the yield is 100.02 grams, which corresponds to 68.98%. Fig 9
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Purification methods of P2P


During the production of P2P, especially when using unrefined starting reagents and solvents, there will be constant challenges in conducting further syntheses and, most importantly, in obtaining the desired product yield. To achieve the desired synthesis results, it is necessary to purify the initial P2P from impurities.

There are several methods for purifying P2P from its impurities, including purification through the bisulfite derivative and simple steam distillation. Each of these methods is suitable for specific working conditions.

Bisulfite Method. It involves P2P selectively reacting with sodium bisulfite, forming a compound in the form of a crystalline creamy mass. Fig 10
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The bisulfite derivative of P2P is obtained by adding dirty P2P (without solvents) to an equal volume of concentrated sodium bisulfite with very intense stirring until complete crystallization. Fig 11
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The bisulfite derivative of P2P is insoluble in diethyl ether, making it easy to wash away impurities. It can also be rapidly washed with butanol, in which the bisulfite derivative of P2P is also poorly soluble. However, due to the acidic properties of alcohols, decomposition will occur with the release of P2P, which will need to be separated again from the mother liquors. After washing, the bisulfite derivative of P2P is added to a solution of potassium or sodium carbonate, where P2P is liberated and can be separated from the alkaline solution, washed with an aqueous solution of sodium chloride, filtered if necessary, and dried with silica gel. Fig 12
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The P2P obtained by this method meets the commercial specifications stated in the Safety Data Sheet (SDS).

The processes of P2P interaction with sodium bisulfite and the interaction of the bisulfite derivative with carbonate proceed according to Scheme 1.
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A drawback of this method is the problematic crystallization, especially for large volumes exceeding 1 liter. Additionally, obtaining sodium bisulfite and washing the obtained derivative can be challenging when using alcohols. The yields when using alcohols are 40-50% of pure P2P, and it also requires re-isolation from mother liquors.

Steam distillation. Steam distillation is a simple but time-consuming method for purifying high-boiling substances. In this study, heavily contaminated P2P, obtained from the unre-crystallized P2NP through sodium borohydride reduction, was purified using steam distillation. Steam distillation of the unrefined P2P is recommended to be conducted in the presence of potassium carbonate for additional impurity removal.

The distillation process can be intensified by using steam generators with at least a small pressure and volumetric capacity. For continuous and constant production, the distilled water (if no color change and impurities are present) separated from P2P is recommended to be recycled back to the distillation cycle for preparing the potassium carbonate solution, reducing overall losses of expensive and scarce P2P.

During the design of a steam distillation setup for large volumes of P2P (5 liters and above), the throughput capacity of the condenser should be carefully considered to avoid pressure fluctuations from the steam generator that could lead to explosions.

P2P obtained by Steam distillation method has a purity of not less than 99%. The yield of P2P is 68%.

When combining methods by obtaining the bisulfite derivative, followed by its decomposition with a potassium carbonate solution and steam distillation, P2P purity of 99.9% or higher can be achieved, but yield of P2P is 40-50%. This was confirmed by appropriate analytical methods such as TLC and refractometry. Fig 13
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Spoiler:

The release of P2P steam distillation video is expected very soon! The video materials are already being edited!!!

 
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Mo0odi

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So great hope your success continues
 

EileiterBurner

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Hut ab, ich muss echt sagen finde es echt bemerkenswert mir welcher Hingabe und Leidenschaft
ihr hier ans werk geht. ----- RESPEKT Jungs ----- 🤘

Sowas findet man nirgendswo im netz.
Bald ist es soweit, freue mich schon drauf meine ersten Versuche mit euch zu teilen. :kühl:
 

rothschild33

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This is some top notch instruction!

Is Fig 13 also P2P? It looks so clear compared to other ones.

What happens if you use rotovap on a mixture of water and P2P, will the evaporated water carry P2P with it too the same way as steam distillation?
 

Lordoftheshard 2

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Easy steam generator pressure cooker on a gas hotplate. So you can adjust the pressure of the steam being pumped into the flask also use flasks with side necks and run the steam through the side necks
And scalling up is easy if doing bulk just need to use 10l and 20l rbf
 

rothschild33

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I keep seeing comments on how one should steam distill p2p instead of vacuum distill. Is there a reason for this?
 

GhostChemist

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Steam distillation is more safer than direct vacuum distillation
 

Akashic

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@GhostChemist would it be acceptable to use sodium bicarbonate in place of potassium bicarbonate In this procedure? Im speculating potassium is going have better cleaning ability than Na bicarb, or maybe another base that could be used?
 

choose

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If P2P Is in toluen, Is there way to extract it without evaporation or vacuum destilation of solvent? I mean some simple extraction. The goal of this question is that I dont have access to vacuum pump and vapors can lead to unessesary attention.

Thanks for replies in advance
 

WillD

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The best choice for you is to use this further in toluene without extracting. Since all other methods will require evaporation or will be difficult with the poisonous vapors. Just choose the synthesis with toluene if you know about the amount in the solution.
 

OrgUnikum

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Add methanol and distill out the toluene as methanol/toluene azeotrope which has a boiling point of about 55 °C, what should be low enough for all purposes.
 

choose

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Can I use isopropanol?
 

OrgUnikum

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Probably not. Azeotropes are specific to single compounds and do not generally apply to groups like if one alcohol then all alcohols. This does not work.
 

OrgUnikum

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Adding Potassium Carbonate solution to the flask with the dirty P2P is a very bad idea and makes absolutely no sense except one intends to kill a lot of P2P on purpose. P2P is highly succeptible to base catalyzed autocondensation, say the P2P condenses with itself forming a polymere, in the extrem it turns completely to the infamous "red tar" otherwise the red goo is well known, or pink to dark red discolorations.
P2P is much more stable towards acids.
If you want to raise the boiling point of the water in the flask use table salt.
Also tilting the flask with the P2P by up 45 degrees or even more if you use a long-necked flask (recommended) helps to prevent water splashing into the condenser in case of hard "bumping" or too much steam. The bumping can be completely omitted when the P2P flask is heated not from below but only from the sides (bottom third of flask unheated). Many heating mantles have double heating exactly for this, one heating for upper part, one for lower part, you use both for quick heating up and only the upper part in distillation which avoids the bumping. Mostly. Don't tell me you knew this. Nobody knows this anymore. So much got lost in time since the hey-days of chemistry....
 

GhostChemist

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Potassium Carbonate added to the ketone hydrosulfite derivatives for producing and purifaing of free ketone with steam distill
 

hacke8

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Hi, sir, if you use acid to purify p2p, which acid is the highest? Sulfuric acid 98%, hydrochloric acid 37%, oxalic acid solid, phosphoric acid 85%) This is the reagent I have. 2L steam generator flask, 1L P2P flask, how many dirty P2P can be added in such a combination? Water vapor distillation is really a painful thing.
 

OrgUnikum

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The formation of the bisulfite addition product of P2P followed by separation and washing of it serves for purification, so does steam-distillation, doing both makes usually not much sense. In special the bisulfite procedure is not really very good yielding and 30% losses can be expected (with P2P). Steamdistillation is done from neutral to slightly acidic water or there will be bad losses due to self-condensation of the P2P ending in the worst case in the dreaded "red tar". Thats just as it is.
And IF you want to do both for any reason: No need to add base or acid at all, the bisulfite adduct will decompose long before the 95°C+ which are needed to steamdistill P2P, as it decomposes nicely upon heating alone.
The temperature dependence of those adducts is btw. a convenient way to separate Aldehydes and Ketones, at a certain temperature only adducts of Aldehydes will form whilst Ketones present will not form such an adduct and such the Aldehyde fraction can be almost completely removed by a simple filtration.
 

hacke8

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Dear chemist, I don't have potassium carbonate. Can I use sodium hydroxide solution instead? Is the proportion the same as using potassium carbonate?
 

OrgUnikum

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You cannot find potash? Did you consider switching to binge watching porn instead of making drugs as hobby? And have you tried to switch it off and on again? Da brain?

But yes you can use NaOH. Any hot base will polymerize a good part of the P2P, makes no difference actually.
 
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