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Daffodile
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[*] posted on 18-3-2019 at 20:09


Anyone done the cyanamide-hydrazine aminoguanidine synthesis?

Just tried it but got no/ negligible yield.

I know my Calcium Cyanamide was decent quality, and my Hydrazine Sulfate was as well at some point (bottle is two years old, however the sample has become quite acidic).

Problems emerged when the pH would not increase substantially during the reaction, as it should with formation of free base Aminoguanidine.

I also accidentally let the thermometer come out of the solution, so the temperature increased to boiling for several minutes.

The Bicarbonate was added as a mostly-dissolved slurry. It all dissolved in the filtered reaction mixture and effervescence persisted for several minutes.

No precipitate formed.

I'm stuck. Any ideas where this could have gone wrong?
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FeedMe94
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[*] posted on 26-3-2019 at 01:33


Can i recrystalize ETN with Isopropyl alcohol or acetone ? Should i also add bicarb or ammonia ?
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Herr Haber
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[*] posted on 26-3-2019 at 05:02


Quote: Originally posted by FeedMe94  
Can i recrystalize ETN with Isopropyl alcohol or acetone ? Should i also add bicarb or ammonia ?


Yes, yes and yes.
Acetone is not as bad as people say.
You can crash your ETN in water with a little bit bicarbonate.
You can also use bicarbonate if there's enough water + solvent before crashing.
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FeedMe94
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[*] posted on 26-3-2019 at 08:22


I had some ETN made 6 months ago. I just recrystalized it using hot acetone and the crushed it into cold water with some drops of Ammonia Water. Got some ETN back but a lot of oily substance was at the bottom. I added more water and turned all into ETN. The ETN i got is like crumble , not like the one without recrystallization which was like flour
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[*] posted on 26-3-2019 at 11:17


More water next time ;)
Redissolve the crumble!
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FeedMe94
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[*] posted on 26-3-2019 at 12:53


Redissolve in acetone ? Can i recrystalize the old batch and a new one together ?
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Herr Haber
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[*] posted on 27-3-2019 at 04:43


Well I suppose you are not going to grind this crumbe into a mortar and pestle ! :P
So yeah, redissolve with the new batch, it's the same molecule so it doesnt matter. The worst you can do is purify further.

Would I be correct to assume some of that crumble adhered to the walls of the recipient you crashed it in ?
If so, definitely not enough cold water. Use acetone to clean the container, pour it straight in cold water. Do not scrape it !
ETN isnt soluble in water so it'll always be better to use more water than less. Filtration will be slower but who cares ?

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[*] posted on 28-3-2019 at 14:22


Someone got an english synthesis of copper Glycinate perchlorats?
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FeedMe94
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[*] posted on 29-3-2019 at 03:59


Yesterday i made some PETN and recrystalized it. I also recrystalized some old PETN i had. The difference i found is the the old PETN is like free flowing and the new PETN acts like kinetic sand. Whats going on?
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[*] posted on 29-3-2019 at 05:49


Can I make nh40h/methanol/dcm extraction solvent by mixing nh4oh with methanol / dcm azeotrope distilled from paint stripper? I guess I'm wondering how miscible nh4oh is with the azeotrope of methanol and dcm. I'd rather not wash out the methanol just to add it back.



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Laboratory of Liptakov
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[*] posted on 29-3-2019 at 12:08


@FeedMe94 error is in solvent, which content some the fat or else grease impurities.



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[*] posted on 29-3-2019 at 13:38


Quote: Originally posted by Laboratory of Liptakov  
@FeedMe94 error is in solvent, which content some the fat or else grease impurities.


I dont think so because the other PETN i recrystalized i used the same Acetone, its 99.6%.
Anyway i recrystalized it again as you told me and i will wait for to dry
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[*] posted on 30-3-2019 at 06:39


Quote: Originally posted by snooby  
Someone got an english synthesis of copper Glycinate perchlorats?


snooby,

Haven't got one handy but can speculate a method that should probably work via metathesis reactions from NH4ClO4. React Ca(OH)2 with NH4ClO4 in aqueous medium to form solution of Ca(ClO4)2 and filter out excess unreacted Ca(OH)2. Heat to drive off excess byproduct NH3. Treat solution with CuSO4 to form Cu(ClO4)2 and filter out byproduct low solubility CaSO4.

Treat solution of Cu(ClO4)2 with glycine, heated together 2 hours and allow to stand for up to a week for crystals to form. (lit)
Evaporation with heating to the point of initial crystallization and then cooling should speed up the process.

Nickel and Cobalt analogues could have interest also. Betaine analogues also could have interest and may form similarly.

[Edited on 3/30/2019 by Rosco Bodine]
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[*] posted on 30-3-2019 at 11:04


@Rosco Bodine
If it works, your post is one of the most valuable in the past few months. Your described method is cheap, simple, safe, and available components. She looks brilliant.....Cu(ClO4)2 is keys formula for a lot nexts attempts...:cool:...LL

[Edited on 30-3-2019 by Laboratory of Liptakov]




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[*] posted on 1-4-2019 at 22:31


Tetrazole lvr on YouTube has had success with this. Says it works just as well as CHP. Only problem is I can’t find copper perchlorate :). Check out his videos.
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[*] posted on 2-4-2019 at 01:25


Yes, success with copper-glycine-perchlorate is great. (CGP).
Advantage of CGP are neutrals crystal. But CGP has difficulty preparation. CHP s very easy preparation. But is partially unstable for free NH3/4 free bond. However CHP is basically stabille. His energetic properties are same after 1/2 year. In detonator, or in glass close jar. Confirmed.....:cool:...LL




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[*] posted on 3-4-2019 at 23:34


Im about to make some impact firecrackers with KCLO3 , Dark Al and Sulfur. My sulfur has impurities in it. What is the best way to purify it ?
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[*] posted on 4-4-2019 at 04:48


Quote: Originally posted by FeedMe94  
Im about to make some impact firecrackers with KCLO3 , Dark Al and Sulfur. My sulfur has impurities in it. What is the best way to purify it ?
Recrys from CS2. If no CS2, then toluene is ok.



Useful sites:
Balance Chemical Equation: http://www.webqc.org/balance.php
Molecular mass and elemental composition calculator: https://www.webqc.org/mmcalc.php
Solubility table: https://en.wikipedia.org/wiki/Solubility_table
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[*] posted on 7-4-2019 at 09:33
ETN using H2SO4/HNO3


Sorry if I'm floggin a dead horse, but..
I am attempting to follow H2SO4/HNO3 parameters suggested by Microtek, and generally agreed to give a good yield:

Quote:

"18 ml H2SO4 (96%), 12 ml HNO3 (62%) and 3 g erythritol, I got a yield of 6.3 g (85 %). The acids were mixed first, then cooled to ca. 0 C. The erythritol was ground to a very fine powder and gradually added by sprinkling into the stirred acids, keeping the temperature under 5 C. Stirring and cooling was maintained for 30 minutes after the end of addition, and the mix was then dumped into 500 ml of rapidly stirred ice water. Product was then filtered and washed again a few more times before being neutralized with NaHCO3 soln."


I doubled the amounts and used a little less E (wanting to keep it thin so I can use my stirrer). Only difference is that my acids did get up to maybe 20 C. during initial mixing, but cooled back down before adding E. Mixture remained easily stir-able using magnetic stirrer. Temp rise with incremental addition of E was very easily manageable. When I crashed it, I did see flakey precip in the ice cold water, though most of it collected at the top. Filtered and partially dried, I only got maybe 30% more than the E I put in. I tried a burn test (letting it melt first) of a few small flakes, seems to deflag, not detonate. I'm guessing it was a fail, but not sure why.




[Edited on 7-4-2019 by twelti]
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[*] posted on 7-4-2019 at 10:25


My experiences is, that E must be absolut dry. Fine powder E heat on 100 C by 10 minute in thin layer on some pan. If is not perfect dry, yields are for example 2/3 against dry E. Only experiences. Reason can be else.....:cool:...LL



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[*] posted on 7-4-2019 at 10:55


Quote: Originally posted by Laboratory of Liptakov  
My experiences is, that E must be absolut dry. Fine powder E heat on 100 C by 10 minute in thin layer on some pan. If is not perfect dry, yields are for example 2/3 against dry E. Only experiences. Reason can be else.....:cool:...LL


Forgot to mention, I did grind the E for 1/2 hour in morter/pestle to very fine, and left overnight in a small baggie with dessicant. Maybe not long enough?

Now finished reX, using denatured alcohol. Most (3/4? ) did dissolve in the 50-55 degree EtOH. Filtered it before crashing into stirred cold water. That small amount of filtrate looked fairly crystalline. After crashing, and cooling for 45 min, final filter, got only 2.5 g (very slightly wet). This final product is white, clumpy, and almost "silvery" looking. Not silvery color but silver sheen, if that makes any sense. I have pics, not sure what the forum policy is...
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[*] posted on 7-4-2019 at 11:28


Your entire procedure is OK. Consistency looks as mica is OK. Sometimes is impossible say, where is error. In procedure was the step of increase temperature on 25 C by 30 - 60 minute? Without mixing? It is final step, when is all E converted on tetranitrate. Without this step arises mixture of Dinitrate, trinitrate and tetranitrate of erythritol. Dinitrate and trinitrate are dissolve in water. Tetranitrate not.



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[*] posted on 7-4-2019 at 12:26


Quote: Originally posted by Laboratory of Liptakov  
Your entire procedure is OK. Consistency looks as mica is OK. Sometimes is impossible say, where is error. In procedure was the step of increase temperature on 25 C by 30 - 60 minute? Without mixing? It is final step, when is all E converted on tetranitrate. Without this step arises mixture of Dinitrate, trinitrate and tetranitrate of erythritol. Dinitrate and trinitrate are dissolve in water. Tetranitrate not.


Hi, LL, in other threads using acid/salt, the allow the temp to come up at the end, to maybe 25 C plus or minus 5. Some also are using longer nitration times.. Does that apply to the HNO3 route do you think? Thanks. I see that is what you asked.

[Edited on 7-4-2019 by twelti]
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[*] posted on 7-4-2019 at 13:14


Not. After mixing, for example 30 minute, is necessary increase temperature on 25 C and mixing run again. Or only stay, without mixing nd hold temperature on 25 C for time next 30 minute.



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[*] posted on 7-4-2019 at 13:17


Why are you sure you have failed? Most nitro esters just burns, but only detonate from inpact. Thats why its called secundary explosive. So in case if you havent tried it, go do some hammerblowntests. Maybe the etn is just fine.
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