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PHILOU Zrealone
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Hydrolysis is not always fast or critical; there are many hydrolysable compounds that are isolable and storable.
You simply have to wash-dry (with a volatile solvent - or with a sequence of volatile solvents that is/are unreactive towards your compound) them as
fast as possible and avoid prolongated contact with the air or water. K-6 should be handlable and not so fast at hydrolysis if stored well.
Heat and pH are wel critical for such sensitive compounds during the solvent and water removal ... so better cool and at reduced pressure than warm
and at atmospheric pressure.
NTNHT should be hydrolysable by water traces because it is a derivative of the putative very unstable N,N',N"-trinitroguanidine ... in their scheme
they imply it turns into K-6 by splitting off the nitroimino moeity and replacement by an oxygen atom...this means:
O2N-N=C(Ring) + H2O --> O=C(Ring) + H2N-NO2 (nitramide)
H2N-NO2 --> H2O + N2O (*)
So traces of water will be reformed autocatalytically and traces of water will remain in a stationary state of concentration (one molecule of water is
used and one is formed).
(*)H2N-NO2 also forms NH3, HNO3, HNO2, NH2OH, NxOy when in contact with water.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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underground
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Quote: Originally posted by PHILOU Zrealone  | Hydrolysis is not always fast or critical; there are many hydrolysable compounds that are isolable and storable.
You simply have to wash-dry (with a volatile solvent - or with a sequence of volatile solvents that is/are unreactive towards your compound) them as
fast as possible and avoid prolongated contact with the air or water. K-6 should be handlable and not so fast at hydrolysis if stored well.
Heat and pH are wel critical for such sensitive compounds during the solvent and water removal ... so better cool and at reduced pressure than warm
and at atmospheric pressure.
NTNHT should be hydrolysable by water traces because it is a derivative of the putative very unstable N,N',N"-trinitroguanidine ... in their scheme
they imply it turns into K-6 by splitting off the nitroimino moeity and replacement by an oxygen atom...this means:
O2N-N=C(Ring) + H2O --> O=C(Ring) + H2N-NO2 (nitramide)
H2N-NO2 --> H2O + N2O (*)
So traces of water will be reformed autocatalytically and traces of water will remain in a stationary state of concentration (one molecule of water is
used and one is formed).
(*)H2N-NO2 also forms NH3, HNO3, HNO2, NH2OH, NxOy when in contact with water. |
I understand PHILOU Zrealone, thanks a lot for your precious help, i really appreciate that
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underground
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I was wondering, how H2SO4 can be used to make k-6, as long as H2SO4 destroy RDX and i guess it will do the same with K-6. Except that, also RDX
participates through this process!
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underground
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Today i tried to make some k-6 but in case of urea, i used the same moles of UN, and in case of HNO3, i used the same moles of H2SO4/NH4NO3 and then i
just follow the procedure according to the pdf.
I used 18.4gr of UN, 60gr H2SO4, for HNO3 i used 93.4gr H2SO4 and 76.67gr of dry NH4NO3 (total H2SO4=153.4gr) and 10.4 gr of Hexamine.
I mix 153.4gr of H2SO4 and 76.67gr of AN and let it to cool into an ice/water bath. When all of AN was dissolved i slowly add 18.4gr of UN and i let
it at about 30minutes with addition stirring every 5 minutes. I then add the Hexamine and let it for more 30minutes with addition stirring every 5
minutes also.
I then just drop the mixture into 750ml of water and i saw something like it was going to form, but unfortunately i did not take nothing 
[Edited on 24-3-2014 by underground]
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VladimirLem
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| Quote: Originally posted by underground |
I then just drop the mixture into 750ml of water and i saw something like it was going to form, but unfortunately i did not take nothing
[Edited on 24-3-2014 by underground] |
hi
i dont have much knowledge of chemestry, but i guess H2SO4+nitrate salt is too weak...this isnt crappy ETN...it seems to be too "exotic"/complex to be
made with nitrate salts...i know this sounds weird, but the more powerful the most explosives are, the more you need high purity/dry chems (oleum,
acetic anhydride, P2O5)
if you have a destillery, go for pure HNO3 and try the way of the pdf....im interested in that syn too 
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underground
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| Quote: Originally posted by VladimirLem |
hi
i dont have much knowledge of chemestry, but i guess H2SO4+nitrate salt is too weak...this isnt crappy ETN...it seems to be too "exotic"/complex to be
made with nitrate salts...i know this sounds weird, but the more powerful the most explosives are, the more you need high purity/dry chems (oleum,
acetic anhydride, P2O5)
if you have a destillery, go for pure HNO3 and try the way of the pdf....im interested in that syn too
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VladimirLem i do not have destillery, that is why i used this method.
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caterpillar
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What is the problem with distillator? Conc nitric acid do not react with steel. You may make distillator, using simple coffee pot. On the other hand,
you can do without it, using nitrate salt + sulfuric acid. This mixture is more powerful nitrating agent, than usual mixed acid. I'm not sure about
AN + H2SO4, but KNO3 or NaNO3 + H2SO4 works good. And you may use Ca(NO3)2- this salt has two advantages. CaSO4 is quite insoluble, therefore after
reaction you'll get mixed acid. And most likely CaSO4 extracts some water from H2SO4 and therefore increases concentration of mixed acid.
Women are more perilous sometimes, than any hi explosive.
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underground
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Why not AN ? There is not much difference between AN and KNO3 or AN and NANO3.
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hissingnoise
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| Quote: | I mix 153.4gr of H2SO4 and 76.67gr of AN and let it to cool into an ice/water bath. When all of AN was dissolved i slowly add 18.4gr of UN and i let
it at about 30minutes with addition stirring every 5 minutes. I then add the Hexamine and let it for more 30minutes with addition stirring every 5
minutes also.
I then just drop the mixture into 750ml of water and i saw something like it was going to form, but unfortunately i did not take nothing
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That's because hexamine decomposes in H2SO4 . . .
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underground
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| Quote: Originally posted by hissingnoise | | Quote: | I mix 153.4gr of H2SO4 and 76.67gr of AN and let it to cool into an ice/water bath. When all of AN was dissolved i slowly add 18.4gr of UN and i let
it at about 30minutes with addition stirring every 5 minutes. I then add the Hexamine and let it for more 30minutes with addition stirring every 5
minutes also.
I then just drop the mixture into 750ml of water and i saw something like it was going to form, but unfortunately i did not take nothing
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That's because hexamine decomposes in H2SO4 . . .
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What about this paper
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hissingnoise
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| Quote: | | What about this paper |
OK! It should've read; "Hexamine hydrolyses in sulphuric acid soln.."
The researchers used anhydrous mixed acid which is practically beyond the reach of the chemistry hobbyist . . .
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underground
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My H2SO4 was boiled so the max concentrations could be achieved. Also the rest chemicals was dried into a desiccator bag with CaCl. More anhydrous can
not be...
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fredsci93
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Recently I made some K6 according to that Chinese paper, I am currently looking for the write up I did, what I do remember was I used equal parts by
volume sulphuric acid and yellow fuming nitric acid plus some pentoxide (~2g) to account for any excess water however the necessity of this I think is
dubious and not mentioned in the paper, then I added urea over ~30 minutes limiting the temp bellow 15C,
The next step entails adding the hexamine which is ridiculously exothermic, it took ~5h and 5+ kilos of ice to keep the reaction at ~0C (always
<5C) and if the hexamine was added in too large a portion it would run away and kill the entire reaction by spraying the room with the reaction.
but after the reaction, I cleaned it up, dissolved it up in acetone and crashed it out (I remember using to much solvent, oops) the final powder
weighed 7.36g but I could have done better (crude yield from the paper adjusted for size was 12g), I have some photos as well.
The product detonates to shock with alot of effort and won't detonate to heat, because of this I don't think it could only be RDX (I have not been
able to detonate it by shock before) or be a nitrourea. If I get the chance I'll do a proper test
The whole process is pretty great for nitric acid efficiency, you get similar efficiencies to the K process (if you get the reported 12g not 7.36g)
only without the high operating heat and the explosive (its a 65/35 mix of RDX/K6) is superior to even the Bachman process product (5-10% HMX?), I
recommend giving it a try (the link was posted u_underground in this thread)
btw: The first photo was from an accident I had while preparing the compound, this lead to no product just filled the room with deadly gas and got me
really mad, also the hexamine contained 1% paraffin as it was unpurified and the urea was fertilizer grade (both were powdered in a blender before
use)
[Edited on 24-3-2021 by fredsci93]
Attachment: Synthesis+of+Keto-RDX+and+its+Characterizations+Calculation (3).pdf (1.1MB)
This file has been downloaded 1149 times
[Edited on 10-11-2021 by Polverone]
 
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Nitrosio
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Attachment: Keto5.pdf (13kB)
This file has been downloaded 506 times
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fredsci93
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Synthesis repeated with a much larger scale plus (some) characterisations
I decided to repeat the procedure for K-6 now that I have some ethyl acetate for separation. The synthesis went well however before I go into detail I
will preface by saying I had a mishap during this particular reaction, during the addition of urea my ice bath was not salted enough and the temp was
~-2c, this was totally inadequate for stoping runaway reaction, my reaction mix reached 10C then would not stop slowly increasing in temperature and
within 10 minutes the temp had reached 19C!
Large amounts of gases were being released, at this point, I made a new salted ice bath and was able to control the temp however during this transfer
a small amount of water entered the reaction, along with poor stirring this contributed to my sub-par yield (stirring was totally manual which left
periods of no stirring, however during hexamine additions the stirring was nearly continuous)
to 136.5mls of Anhydrous nitric acid ~140mls of technical grade 98% sulphuric acid was added on an ice bath
The mixture should be transferred to a salted Ice bath before 40g of ethanol recrystallized urea (MUST be finely pulverized) was added in ~400mg
portions making sure the temp stays far below 10c.
The mix was aged on a new salted ice bath for 30 minutes, at this point, the mix was ~-6C. 20g of recrystallized DRY hexamine (MUST be finely
pulverized) was added in very small quantities keeping the temp below 0c (make sure to essentially sprinkle the hexamine to avoid runaway) with strong
stirring if any hissing noise is noted STIRR AS FAST AS POSSIBLE as if the hissing can continue the mix will runaway.
At this point, I needed to transfer the mix to another salted ice bath as the cooling rate was too slow, another 20g of hexamine was added in the same
manner as before.
The mix was removed from the ice bath and placed on a warm water bath to raise the temperature to 10C, (temp was maintained below 12c with the aid of
an ice bath and warm water bath (17c)) this mix was stirred for 30 minutes before being dumped into 2L of roughly crushed ice.
The mix was filtered and washed first with large amounts of water then with a ~1% bicarbonate solution then with large amounts of water (no
decomposition from the bicarbonate is evident) after drying over 50h or so with the aid of a 150W ceramic heater and 50W halogen heater/fan the mix
weighed 30.46g (about 55% of the claimed yield)
5g of the crude substance was dissolved in ~75mls boiling acetone leaving an inert off white residue (bellow measurement thresholds, looked like
~100mg) and a solution of k-6/RDX, this solution was filtered, reduced to 50mls by a 50W halogen heater/fan, cooled to room temp and placed in the
freezer for 2 hours. the crystals were collected and the solution was further reduced to ~25mls before being chilled and filtered, this was repeated
again to 10mls, the combined crystals weighed 3.97g
neither the crude mix nor pure mix was particularly shock-sensitive, however, I will note the crude mix SEEMED more sensitive (very relative)
The Crude mix smokes off leaving a small amount of residue in indirect flame and ignites and burns under direct flame with some residue, when the mix
was purified the burning qualities increased significantly, it burns quickly (much faster than the crude in both cases) in direct or indirect heat and
leaves nearly no residue.
Solubility characteristics were recorded by dissolving ~100mg of compound in ~10mls of room temp solvent and letting sit, heating if required, a
soluble compound is one that I observed to dissolve quickly at room temp, a slightly soluble compound is one which dissolved some of the compound at
room temp, or at boiling temp.
The pure mixture was soluble in acetic anhydride, acetic acid, acetone, DMSO, and MEK, it was partially soluble in ethyl acetate (only the k-6
dissolves) and methanol (took a very long time and heating), the mixture was insoluble in 99% ethanol, DCM, Chloroform and water.
There will be more to come on this as I need to wait for some solvents, however, I decided to post this now since it's been a couple of weeks since
the solvents were supposed to arrive and I thought some of you might find it interesting in its current form.
notes (all very speculative):
1: I decided not to use HDN for multiple reasons, one it's highly hygroscopic so most likely I would introduce some water, and two the paper uses more
nitric acid per gram of product when they employ HDN, I believe this is because HDN is more likely to become RDX in the given amount of nitric acid
rather than k-6 in the reaction mix as it is less susceptible to total cleavage by nitrolysis (which is required for the reaction as the reaction
proceeds as follows (TOTAL ASSUMPTION AND ONLY A PARTIAL REACTION) hexamine --> Iminodimethanol derivative HO-CH2-NH-CH2-OH (with varying levels of
nitration), HO-CH2-NH-CH2-OH + O2N-NH-CO-NH-NO2 + xHNO3 ---> Keto-RDX).
2: I decided not to use urea nitrate one because of the hygroscopicity and also because from all the syntheses of dinitrourea I have seen no one uses
urea nitrate, I assume this is because of either solubility reasons or because the urea nitrate is merely dehydrated to mononitrourea which
precipitates.
3: I used equal VOLUMES of nitric acid and sulphuric acid based on the paper on which the synthesis is based, they give molar quantities that
correspond to equal volumes, NOT masses (0.63mol H2SO4 to 0.8mol nitric acid), if you use masses the reaction will likely not work well.
4: My (slightly yellow) nitric acid was obtained by dehydration and fractional distillation of azeotropic nitric acid over an equal volume of
sulphuric acid, the collection was stoped once the temperature dropped slightly and I obtained roughly the amount I was expecting ~half the original
volume or a 70% efficiency.
5: It is not important to use white fuming nitric acid for obvious reasons as the urea will remove the excess coloration, however, this would slightly
impact yield so you might want to decolor the nitric acid before use with dry air.
6: Phosphorus pentoxide was omitted and this appeared to have no negative impact on yield and the hexamine additions seemed to be tamer this time
around, along with that during the previous run with pentoxide some dinitourea precipitated before hexamine was added whereas during this run the
solution before hexamine addition was clear apart from a small number of bubbles. so I would recommend against using pentoxide.
 
[Edited on 3-9-2021 by fredsci93]
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ManyInterests
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I'm going to making my one and only Keto-RDX synthesis in a few days and I decided to bump this thread up to report on what I'm doing (this forum is
officially my lab notes!).
I will be using HDN however. I made a dessicator with sodium hydroxide to draw off the moisture. My HDN is free of acetone as far as I know, so
hopefully there will be no acetone induced runaways. I will do what I always do in nitrations... freeze my beaker in a solid block of saltwater ice. I
will bring my mantle outside to use it to warm up the mixture to 10C when I am done with all additions.
I plan on using as much of my ~18 grams of HDN for this. Which seems mildly more sticky after I checked it just now. What could be happening?
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fredsci93
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HDN should be dried with an acidic/neutral desiccator like calcium nitrate/chloride, it gets sticky over time because it absorbs water very easily
even when semi sealed
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ManyInterests
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OK so after talking to fredsci93. I plan on using regular hexamine for my synthesis. I measured by entire yield of fuming nitric acid and it was 65ml
with a weigh of 96.92 grams at around 30C (the temp I set my room to... so room temp) which gives it a specific gravity 1.491. I could be mildly off
in how much I have, but that would be in the ~0.5 ml range, so it won't affected it that much.
My nitric acid is still quite red from nitrogen dioxide contamination. So I will need to bubble it out. I have a piece of polyvinyl tubing that I cut
and I will bubble it out with my tiny little 12v bubbler (it's really cute, like palm sized!)
Edit: Maybe the bubbling is not necessary. fredsci93 did note note that nitric acid loses its color after sulfuric acid is added. I remember my ETN
synthesis and this is true even when dealing with the azeotropic nitric acid. When I did my first ETN synthesis there was some yellowness/redness to
my acid, but after adding the sulfuric acid it all disappeared in an instant. I will mix the acids outside and in a cold water bath to deal with any
exothermic reaction.
Edit2: While the paper does state that the urea was added to the mixture at a temperature of 0-5C I will not be doing that. I will add it at the
coldest possible temperatures. I know I probably will lose a bit of end-product for this, but I would rather not run the risk of a runaway reaction
and instead keep things as cold as possible.
Assuming I get a max yield of 28 grams of end product. How much acetone will I need to dissolve all this in?
[Edited on 16-12-2021 by ManyInterests]
[Edited on 16-12-2021 by ManyInterests]
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fredsci93
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For the temp, I went with 0-5C, I don’t blame you for wanting to go with a lower temp, it probably wont hurt much and will avoid runaway a bit so
why not.
The recrystallisation doesn’t require much acetone IIRC, just heat it to 50C and add enough acetone to dissolve most of the product (some gunk is
left over) and filter the solution, as for separating K-6 from RDX, it's very difficult, I think I managed to do it based off the crystal structure of
two of my batches (RDX forms rhombic crystals keto-RDX forms more rectangular crystals, the mixed batch contained both types, the separated batch
contained a higher amount of rectangular crystals), however ethyl acetate actually dissolves both substances to a degree, I might have gotten a pure
product since I separated my crystallisation fractions, but it's hard to tell, so if you don’t have advanced tools to analyse the crystals it's
somewhat pointless to try separate them, especially since the mix is already a very powerful explosive.
[Edited on 17-12-2021 by fredsci93]
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ManyInterests
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It's good that I don't need a lot of acetone. However, I don't plan on seperating the K6 from the RDX. Keeping them together in the mixture is OK with
me. I probably will end up mixing the purified result with my ETN and to plasticize both (after taking out what I need from the ETN for my blasting
caps). (although I can't remember if I filtered that dissolved ETN to get rid of the one hair bit and a small bit of pebbles, but I did test the
result after and it was significantly more likely to pop and melt when subject to a flame. So the recrystalization did a lot to purify my result.
It'll be a while before I get a chance to set them off. I live in a crowded city and there isn't a place nearby where I can set off a crazy loud bang
without anyone noticing. Thankfully I live in a fairly large country with vast swathes of wilderness. The problem with that is finding a place to trek
that is also near a parking lot that is also not a known hiking trail. Parking a car at the side of the highway over here is illegal (and very
conspicuous) except in the case of an emergency. Still, it can be done.
[Edited on 17-12-2021 by ManyInterests]
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fredsci93
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yea, that's always the bottleneck in EM, it's very hard to do det tests, oh well just have to wait for an opportunity to present itself
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Microtek
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If you are satisfied with some of your tests being just 1-2 g of explosive, you should try Liptakovs method with coarse sawdust in a large bucket. The
sound is like dropping a bag of cement on the ground, or closing a door somewhat forcefully. With this method I can do small scale tests on the ground
floor without my kids noticing when they are upstair. Obviously, you need a lid for the bucket, or there will be sawdust everywhere.
Where I live, a suitable grade of sawdust can be bought in pet shops for rodents to nest in.
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ManyInterests
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I have cleaning grade sawdust that is quite thick and all.
But that being said. My keto-RDX synthesis ended in a massive runaway. It was my fault. I severely underestimated just how exothermic the final
addition of hexamine was and I saw my glass thermometer fly through the roof. I immediately ran back into my apartment and closed the door, watching
the massive cloud of gas emit and fly away. I hope no one noticed.
I will wait a while to let everything cool down before I can see if my beaker needs retrieving. I made several mistakes.
Firstly... holy smokes was it exothermic! I should used the quantities in the paper and not double it right away. The second thing is that I needed a
larger beaker. I used my 250ml beaker when a 500ml would have been more appropriate. But I did not have my 500ml beaker with me so I had to transfer
it from the 250ml to my 1000ml in order to prevent an early overflow. I made another regular ice bath, but the problem is I added too much water and
the 1000ml beaker just bobbed around and it made stirring hard.
My thermometer was already busted due a previous runway that burned off the numbers except for one. So I was eyeballing it all the time. I wasn't
entirely sure.
I also severely underestimated the amount of foaming it would make. I wasn't sure if would subside or what. It kinda looked like the ETN synthesis I
had done several times before, but this was an entirely different beast. Even freezing my beaker in a solid block of ice was insufficient to keep the
temperature in sub-zero ranges. While for my ETN synthesis it never broke loose from the ice block.
That being said. I am all out of fuming nitric acid and I am done with my experiments. I will be picking this hobby up for maybe another keto-RDX and
CHP synthesis, but that'll be in a year from now.
And the next time I do it it will be HALF portions, a quarter of my attempt. I was too confident and it didn't work. And in a year from now.
I feel a bit disappointed ending my experiments without a bit of RDX. But hey, my first to attempts at freebasing hydrazine didn't work out. Failures
happen. I learned. Next time I will succeed.
[Edited on 17-12-2021 by ManyInterests]
[Edited on 17-12-2021 by ManyInterests]
[Edited on 17-12-2021 by ManyInterests]
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ManyInterests
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| Quote: Originally posted by Microtek | If you are satisfied with some of your tests being just 1-2 g of explosive, you should try Liptakovs method with coarse sawdust in a large bucket. The
sound is like dropping a bag of cement on the ground, or closing a door somewhat forcefully. With this method I can do small scale tests on the ground
floor without my kids noticing when they are upstair. Obviously, you need a lid for the bucket, or there will be sawdust everywhere.
Where I live, a suitable grade of sawdust can be bought in pet shops for rodents to nest in. |
Yeah that's what I also planned on doing. I have a 5 gallon bucket full of sawdust. I also got a wooden block that I plan on inserting my blasting cap
in to detonate. One other thing I can do is play ultra-loud music (it can reach 120 decibels) to muffle the sound even further.
Or I might carry that bucket to a park where no one can hear and set it off there. It'll be a bang, but no one will hear it due to the muffling and
the distance.
Edit: I am curious as to how far I got in my synthesis. I had added all the urea, and while I did add most of the hexamine, I had one single (very
level) spoonful left of the hexamine to put in. Maybe a few grams at the most.
The consistency of the solution was extremely milky white and very frothy, almost like a milkshake. Is this is supposed to happen? If I decided to not
add the remainder and just let it sit in the icebath for however long would I still have ended up with some kind of yield? Assuming the temperature
stabilized and dropped?
[Edited on 17-12-2021 by ManyInterests]
[Edited on 17-12-2021 by ManyInterests]
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fredsci93
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haha, I'm glad someone else can attest to how ridiculously exothermic the reaction is, it took me a couple try’s to get the reaction to work, I
would advise getting a k-type thermocouple in a one ended glass tube for temp monitoring it helped alot with making sure the reaction wasn’t going
sour, but even with a k-type thermocouple it's super hard to control, I would also suggest a smaller scale, just to feel it out a bit before stepping
it up to full scale (or in my case 4x scale), but even with my experience with the reaction I got shit yields and fucked up a bunch, so I wouldn’t
be to discouraged, I might actually revist the keto-RDX synth myself, just to try get a more satisfactory yeild.
Also the nitration mix after a runaway didn’t seem to have any RDX/keto-RDX when I dumped mine into water, the high temps seem to cook the
keto-RDX/RDX, but there’s no harm in dumping the mix into water just to see if anythings in it
I currently have 3 vials full of 3 of my K6/RDX samples in acetone evaporating (one I think is mostly RDX, one I think is mostly K6 and one is a
purified mix) I'll send pictures of the vials and the samples in their respective bags once the acetone evaporates and gives some nice large crystals
For small tests I used to use a heavily insulated chilly bin, it worked ok, not great though, I have some det caps I need to test, so i'll try get
some sawdusty for that
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