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Author: Subject: ETN question
B(a)P
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[*] posted on 13-1-2021 at 11:52


A yield of 93% for ETN is quite enviable with H2SO4/KNO3, do you mind providing a little detail on your procedure please? I would be curious to know if you had issues with the contents of the reaction vessel thickening toward the end of additions? How much H2SO4:KNO3 did you use? Is the 93% yield measured from the recrystallised and fully dried product?
Thanks!

Edit: Also what H2SO4 are you using?



[Edited on 13-1-2021 by B(a)P]
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[*] posted on 14-1-2021 at 07:39


I have same question a like BaP. 93% is high yield. With KNO3. I estimate you used a bigger excess of H2SO4. Against method with HNO3.
For example, for 10g dry Erythritol is used 60ml SA 96% + 40 ml HNO3 65%. And Yield is 20g ETN after recrystallisation. Run temperature between zero to + 5C.
I forgot theoretical yield about 22g ? on 10g E.





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[*] posted on 14-1-2021 at 11:26


Quote: Originally posted by Laboratory of Liptakov  

I forgot theoretical yield about 22g ? on 10g E.



100% yield from 10 g of erythritol would be 24.75 g of ETN
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[*] posted on 14-1-2021 at 23:44


Thanks very much, B(a)P......:cool:



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[*] posted on 15-1-2021 at 11:54


OK, details.
200g H2SO4 (great excess)
65g KNO3
mixed and chilled to zero C.
Procedure was done outside at environmental approx zero C, on ice bath (no salt)
15g erythritol added in small portions over approx 2h with vigorous stirring, at first magnetic but then as the mixture thickened I had to resort to manual stirring with a glass rod (the magnetic stirbar became overwhelmed). No more that 1g per addition with 5-10 minutes of stirring between.
At the end of the addition consistency was about the same as sour cream.
When this was done, the mix was brought to an intermediate temperature of approx 10C and held there with stirring for 30 minutes.
Subsequently temperature was increased to 21C for 1h again with stirring. An ice bath was kept nearby to prevent any runaway reactions. As soon as there was any NO2 released from the mix, the mix was put on ice bath and stirred like crazy until gas formation stopped. This had to be done every few minutes.

In the end, it was crashed in a large amount of cold water. Since it was still too thick to pour, first I added 200ml ice-cold water with stirring then immediately dumped it all in 2L ice cold water. There was some heating of the mix going on with the water addition but I was quick enough to not lead to any damage.

The water/ETN/salts mix was stirred at low temperature for 1h, then filtered and thoroughly dried over 2 days.

The 93% yield is on product that was NOT recrystallized, but very dry.

(edit) The sulfuric acid used was straight drain cleaner, which in my area is very high quality (95%, no dyes, no impurities). The KNO3 was purchased last week from Duda Diesel. The erythritol is standard food-grade sweetener without any additives, purchased from Amazon.

[Edited on 15-1-2021 by stamasd]




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[*] posted on 15-1-2021 at 12:30


Great work. Is see great exces of H2SO4...95..?...98%..? On 15g E. It is better to use a spoon to remove the cream from the reaction vessel. And after individual spoons add to 2 liters of ice / water. Never rinse a reaction vessel containing 20 or even 30% cream. The temperature will rise sharply in 1 second. Others steps are perfect. Only one gram adding with long pause is maybe main key for big yield.



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[*] posted on 15-1-2021 at 14:40


Thanks for posting I too was wondering how you got such yields. I am going to try this and see if I can replicate the results.

http://www.sciencemadness.org/talk/viewthread.php?tid=155655
This thread is another apparent high yields synth with a video, I have tried this one as well may times and have yet to be able to replicate it. Normally around 65-70% yield. If anyone can replicated these results and offer some key advice I am all ears and would appreciate it!

[Edited on 15-1-2021 by Brightthermite]

[Edited on 15-1-2021 by Brightthermite]

[Edited on 15-1-2021 by Brightthermite]
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[*] posted on 16-1-2021 at 01:35


FWIW here's the effect of 300mg of the final product detonated inside a small cardboard tube using a PbN3 primary, with fairly light compression.







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[*] posted on 16-1-2021 at 01:38


Quote: Originally posted by Laboratory of Liptakov  
Great work. Is see great exces of H2SO4...95..?...98%..? On 15g E. It is better to use a spoon to remove the cream from the reaction vessel. And after individual spoons add to 2 liters of ice / water. Never rinse a reaction vessel containing 20 or even 30% cream. The temperature will rise sharply in 1 second. Others steps are perfect. Only one gram adding with long pause is maybe main key for big yield.


Thank you. I discovered yout YT channel recently, good material there. I am experimenting with 2 new sources of PIB binder and will report here if either of them is useful. Should have some results in a week.




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