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Author: Subject: PETN recrystallisation procedure for LOW density
Etanol
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[*] posted on 5-6-2024 at 22:58


Quote: Originally posted by pjig  
I think for “simple detonators etc” a low density material would be sufficient to kick off other materials.

PETN is quite sensitive to detonation. If you are not planning to make a non-primary detonator, then I see no reason to strive for low density. The higher the density, the higher the brisance and efficiency of the detonator.

Quote: Originally posted by pjig  
a two stage press , dense base , simi dense layer and a primary to complete.

Yes

Quote: Originally posted by pjig  

The Re crystallization process of the hot acetone + Petn and a pinch of urea, taken and crashed into cold water created a wet sand like low density material that reduces into a very fine material.

If this is recrystallization of pure PETN, then I see no reason to add urea. Urea is too weak a base. Ammonia is much better.

Quote: Originally posted by pjig  

Even dry acts like it wants to cake up like wet due to the fine particles.

This is due to the needle-like shape of the particles.

Quote: Originally posted by pjig  

First, in this form of avalanche Re crystallization is this process enough to remove unwanted byproducts, and acids? Second is it stable for long term storage ?

I do not understand you.
For the recrystallization of pure PETN for the purpose of crystal modification, urea is not required.
For recrystallizing dirty PETN to remove acids and other impurities, urea does not work. Such PETN will not be stable.
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Microtek
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[*] posted on 7-6-2024 at 07:53


The function of urea in this context is not to act as a base, but as a NOx scavenger. The same reaction can be employed to remove NOx from RFNA. During decomposition of PETN in storage, NOx is evolved which increases the rate of further decomposition. By incorporating small amounts of urea in the PETN crystals, this feedback loop can be broken.
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pjig
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[*] posted on 8-6-2024 at 08:52


Im speculating about crystal formation and its ability to release its waste acids , other slow crystal growth , or immediate upon a crash (avalanche method) . I believe the slow method is more effective in purifying and density. The trade is manipulation to reduce large crystals (shave) to desired size (for its function ).

Now the ease of the fast crash method is appealing, (fast results) but I’m not 100% sure it’s as effective at removing trace acids(hense the use of urea) , and it reduces to a very fine particulate. I assume that is low density. It takes on a unique caking problem due to crystal structure.

The fast crash material also presented another weird trait . It almost seems (under normal pressures ) to go max density when pressed and it’s need for more initiating power required. Making it less predictable with normal priming methods.


Any experiences or results other have to back this up or explain unique processes?
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[*] posted on 9-6-2024 at 01:41


You could do both. First a slow crystallization for obtaining a pure product, then redissolve in fresh solvent and crash precipitate for fine powder. From my perspective, the main advantage of fine powder is the smaller critical diameter and better performance at the microscale. I prefer crystallizing by addition of water to the neutralized acetone solution. Then I can adjust temperature, agitation and speed of addition to tune the crystal size and morphology to the application.
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[*] posted on 9-6-2024 at 11:59


Excellent ideas.. ty

As per your crystallization process are you doing this at higher temps, rm temp , or cold to precipitate out your solution? Stirring will obviously aid in the shaving process ( how long are you continuing to stir after all water is added and precipitation is done ?

[Edited on 10-6-2024 by pjig]
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Etanol
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[*] posted on 9-6-2024 at 13:12


Quote: Originally posted by Microtek  
First a slow crystallization for obtaining a pure product,

It is better not to dilute the acetone solution with water, but by a mixture of 40% alcohol and 60% of water. Then yellow resins and pentaeritritol trinitrate remain in the solution.
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[*] posted on 13-6-2024 at 01:37


@Etanol: My PETN does not contain the impurities you mention, possibly because I synthesize it from 100% HNO3 rather than mixed acid.

@pjig: I usually do the precipitation close to the boiling point of acetone, then maintain stirring until it has cooled most of the way to room temp.
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[*] posted on 14-6-2024 at 20:54


Ty microtec
The hot PETN acetone solution instant crash may have some undesirable variants (less sensitive forms of the petn family . This Leaving the final product less sensitive to initiating, but in a way, safer for an industrial level where munitions may call for insensitivity . Unfortunately for sensitive initiators it is counter productive. Soi assume a slow process is more desirable for the precipitation being more sensitive . Never seen the oily yellow derivatives, but that may be from the heating after nitration process to max yield, and destroy impurities . Losses from the “cold only “ process is minimal in small scale production… not worth the risks and potential near ddt temps if residue resides on sides of reaction glass . Just my 2 cents
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