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Author: Subject: picramic acid from picric
Rosco Bodine
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[*] posted on 2-8-2005 at 05:54


This is an area of experimentation which still interests me because of the improved density methods for DDNP and also the hydrazine / DDNP derivative lead salt which I have not tested . I also want to further refine the proportions and optimize the " dry method " preparation of the NaOH - Sulfur / hydrosulfide - polysulfide reagent , for reducing sodium picrate to sodium picramate .

I have a fresh batch of picric acid crystallizing now and hope to do some further experiments when time permits .
Actually the picric acid is itself a separate
experiment of a series I plan to do in evaluating the use of methyl salicylate as
an alternative to aspirin . It seems a bit more sensitive about the nitration times and temperatures and acid strengths than is the process using aspirin , but I believe once the optimum conditions are identified it will be a superior method .
My first experiment went well until about halfway through the introduction of the third nitro group , but I didn't go slowly enough or push the temperature high enough , or the acid mix was a bit too strong , so there was a mild runaway and boilover right at the endpoint where I had to quickly move the flask to a catch basin with a shallow layer of water to capture the overflow and save the batch .
Adjusting the conditions a bit should tame the reaction , and since the synthesis is not well known it intrigues me to formulate a reliable method . It seems to work similarly as with aspirin , but the reaction doesn't behave exactly the same and is touchier in the final stage . It will require a few experiments to identify the variables and formulate a good working method .
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[*] posted on 31-8-2005 at 03:09


The attached file is one of the listed references in PATR 2700 for Picramic Acid from the “Dictionnaire des Matières Explosives” (1902) by Daniel.

[Edited on 5-6-2013 by Polverone]

PAA REF-Page 615.jpg - 292kB
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[*] posted on 8-5-2006 at 17:22


I took the thought of reducing with ascorbic acid to heart, and tried it. Tried, meaning placing some crude slightly basic Na picrate solution (some picric acid was perhaps in there as well) adding a few prills of NaOH, and dumping in some ascorbic acid. Shake, stir, and wait. After 10 minutes of nothing, I placed it in a warm water bath. This turned the solution to the characteristic dark-red and I am positive picramic acid (salts) were produced. After leaving it for an hour, the water bath had dried, and it was heating the tube on the pan, however, it was not boiling. It was a very dark colour now, no transparency. When a drop was placed in water the color was revealed to be a dark orange/red. I suspect that is slightly over-reduced?

Either way, the ascorbic method works, and I shall do some slightly more... controlled expirementation later.




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Rosco Bodine
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[*] posted on 8-5-2006 at 18:42


Well it's good that somebody has been curious enough to try vitamin C :D I have more good ideas than time for experiments , and I love it when you fellows check it out
and prove old Rosco right ! Great minds think alike ,
I tell you that's it :D And for when I'm wrong ....
well that's just the anomalous brainfart .

I suspect your orange coloration was from either unreduced
sodium picrate , or from free picramic acid due to pH being
a bit on the low side .

I have an untested idea that it could work best if you go a bit past neutralization of the ascorbic acid first with a sodium salt like ordinary baking soda , to the point
where it doesn't effervesce CO2 on further addition
of base . The warm concentrated solution of
slightly basic sodium ascorbate is probably air sensitive
like other reductants would be , so you may want to
minimize any overt exposure to air over any long period of time , keep the stuff closed up if it isn't going to be used right away for the reduction . And it might be good to use a piece of saran wrap and a rubber band over
the top of the reduction beaker , punch a hole or cut a slit for admitting the tip of the dripping funnel , to keep fresh air off the vortex surface of the reduction mixture .
The reduction should be done very gradually , running in the ascorbate solution while it is warm , into the prewarmed sodium picrate solution , pretty warm depending on the induction temperature .....there will
be a temperature where you can probably control the exotherm by rate of addition ....so the reaction proceeds
fairly rapidly but in a controlled way . Let it keep stirring
past the end of the addition for the time it takes to start
cooling down significantly on it's own , and then let
it sit in the refrigerator or a bath of melting ice overnight .
Sodium picramate will be a very dark burgundy red
precipitated fine prismatic crystal , a very dark maroon
or oxblood color ....and it is an intense dye much more
dark colored and soluble than free picramic acid .
The crystals should be so fine it will almost look like
mud on the filter , but in strong light it will glitter profusely revealing the crystalline nature plainly .

[Edited on 9-5-2006 by Rosco Bodine]
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[*] posted on 9-5-2006 at 15:29


What are the products of the oxidation of ascorbic acid, so I can balance an equation. Would a gross exess of ascorbic acid violate the reaction, of simply make sure it gets reduced. Do we belive it could over-reduce to triaminophenol?

Either way, after I recrystallize some TNP...




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Rosco Bodine
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[*] posted on 9-5-2006 at 16:53


If I have it right , it simply loses one hydrogen
when reduced . I take it that " monodehydro " ( ascorbate ]
means " minus one hydrogen " :D ,
probably the atom and not the molecule ....
I have to be at least half right :D

This is from Wikipedia

http://en.wikipedia.org/wiki/Ascorbic_acid

Uses
Ascorbic acid is easily oxidized and so is used as a reductant in photographic developer solutions (among others) and as a preservative.

Exposure to oxygen, metals, light and heat destroy ascorbic acid, so it must be stored in dark and cold and not in a metal containment.

The oxidized form of ascorbic acid is known as dehydroascorbic acid.

The L-enantiomer of ascorbic acid is also known as vitamin C (the name "ascorbic" comes from its property of preventing and curing scurvy). Primates (including humans) and a few other species in all divisions of the animal kingdom, notably the guinea pig, have lost the ability to synthesise vitamin C and must obtain it in their food.

Ascorbic acid and its sodium, potassium, and calcium salts are commonly used as antioxidant food additives. These compounds are water soluble and thus cannot protect fats from oxidation: for this purpose, the fat-soluble esters of ascorbic acid with long-chain fatty acids (ascorbyl palmitate or ascorbyl stearate) can be used as food antioxidants.

The relevant European food additive E numbers are: E300 ascorbic acid, E301 sodium ascorbate, E302 calcium ascorbate, E303 potassium ascorbate, E304 fatty acid esters of ascorbic acid (i) ascorbyl palmitate (ii) ascorbyl stearate.

[edit]
Antioxidant mechanism
Ascorbate acts as an antioxidant by being itself available for energeticaly favourable oxidation. Oxidants (scientifically referred to as reactive oxygen species) such as the hydroxyl radical (formed from hydrogen peroxide), contain an unpaired electron and thus are highly reactive and damaging to humans and plants at the molecular level. This is due to their interaction with nucleic acid, proteins and lipids. Reactive oxygen species can 'abstract' a hydrogen from ascorbate, which becomes monodehydroascorbate and soon gains another electron to become dehydroascorbate. The reactive oxygen species are reduced to water while the oxidized forms of ascorbate are relatively stable and unreactive, and do not cause cellular damage.

Dehydroascorbic acid (DHA) is one of oxidized forms of ascorbic acid. It is actively imported into the endoplasmic reticulum of cells and generates the oxidative potential found there. Protein disulfide isomerases are known to reduce DHA back to ascorbic acid, oxidizing their disulfide bonds in the process. Therefore L-dehydroascorbic acid is a vitamin C compound much like L-ascorbic acid. As a result of different contents of crystal water (hydrated water) there are different forms of DHA: the waterfree bis-DHA and the mono-DHA*H2O. In literature often mono-DHA without hydrate water molecule is used. Oxidized forms of esterified ascorbic acids can be numbered at C(5) or C(6) atoms and the (free) chemical radical semi-dehydroascorbate or semidehydro ascorbic acid (SDA) to the group of dehydroascorbic acids.

[Edited on 10-5-2006 by Rosco Bodine]
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[*] posted on 10-5-2006 at 14:55


Some solutions were mixed, about 50mls of Na picrate soln. at RT, along with some slightly-warm sodium ascorbate solution. The solutions were dumped togeather in a erlenmeyer flask, stoppered loosely, and set on a low set hot-plate. Upon return 15 mins later, it was happily boiling slowly and was a very dark color, appearing alomst black. This was placed in an ice bath overnight, and was placed in the freezer for a bit to cool to 0 before filtering. I obtained a small (.25g) amount of sodium picramate. It is dark-red, maroonish color, and quite fine-grained. The crystalline structure is not particularily dense. I have not calculated the soluabilities, but this seems to be an OK yeild given circumstances and mistakes. Either way, it burns. :P I have yet to do a reduction with actual measuring.

I will add this to HCl in order to create free picramic acid and NaCl. This will then be acidified furthur, and a NaNO2 solution will be added at OC. If a diazo-product resembling DDNP is obtained, I dub ascorbic acid proved and worthy as a reducing agent for TNP.




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Rosco Bodine
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[*] posted on 10-5-2006 at 15:33


When you get to the diazotisation , there is a very
specific temperature window and concentration of
reacting solutions and addition rate which produces
suitably dense crystals of DDNP .....where any other
conditons only produce a low density amorphous
powder form which is not suitable for dets .

Relevant excerpt from Urbanski 3 , page 203 :

The effect of conditions of preparation have been thoroughly examined by Smolenski
and Plucinski . They found that at a diazotization temperature as recommended by
Clark , i.e. 15 C , the product pours with difficulty . Conversely , diazotization at a
higher temperature ( 25 - 45 C ) results in formation of a product with a density of
about 0.82 .

Smolenski and Plucinski prepared dinitrodiazophenol in the form of free flowing crystals by applying the following reaction conditions :

A solution of 320 g of sodium nitrite in 2 l. of water is added to a suspension of 1000 g of the sodium salt of picramic acid in 8 l. of water . Next , 6 l. of 5.5% HCl
is added dropwise for 2 hr. , stirring continuously . The initial temperature of 20 C rises to 25 C . Completion of the reaction is determined by means of starch-iodide
paper . The product is filtered off , washed with cold water and dried at 35 - 40 C . Its yield amounts to 80 % of the theoretical .


Blaster at E&W has described a diazotization procedure modeled on the above method described on the following page , with pictures .

http://www.roguesci.org/theforum/other-explosives/435-ddnp-t...

[Edited on 10-5-2006 by Rosco Bodine]
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[*] posted on 10-5-2006 at 16:52


Yes, I synthed the amorphous form. When I actually do a measured reduction, I will prepare it via the afore mentioned method.

EDIT: well, at least I thought it was amorphous. It is powdery, and fairly free-flowing, although not crystalline as was the ideal product. It did, however, burn extremely fast more like the second type. As fast as any flash I have ever created, I suppose.

[Edited on 11-5-2006 by Swany]




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Rosco Bodine
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[*] posted on 11-5-2006 at 07:34


It is something I would have to check my
patent references , but there are ways to
further process the amorphous form and
make use of it in mixed , coprecipitated
compositions , where DDNP functions as
an accellerator for deflagration to detonation
transition mixtures , useful particularly with
those polynitrated polylols which are almost
but not quite primary explosives by themselves .
Things like mannitol hexanitrate , inositol hexanitrate ,
even PETN , co-crystallized in admixture with DDNP result
in powerful det fillers which are DDT primaries
and are reportedly relatively stable and safe
enough for practical use .....although not as
storage stable at higher temps as military grade
systems , still good enough for commercial use .

DDNP in 50/50 mixture with picric acid forms a eutectic
melt a bit below the bp of H2O , which can be detonated
by compressed granular DDNP more easily than picric
acid alone , and the eutectic is more brisant than picric acid alone . Such a combination could have usefulness
in improvised dets where raw materials are a limitation
but a pretty high performance device having reasonable stability and safety could still be achieved .

DDNP also forms a reaction product with hydrazine
which is reported to have usefulness . So there
is a lot which can be done further with DDNP , even
if it is obtained as the amorphous product and not
used directly . IIRC , when a binder like dextrin is
used to form a pellet of the DDNP , it will self-confine
and undergo DDT at a certain mass quantity , going
high order after ignition even in the open , same as
is true for many other primaries which are a bit slow
on self-accelleration , but the rise is more rapid for
DDNP while it makes the transition to high order ,
so it does the job of DDT completely in subgram quantities under the right conditions of confinement ,
better say than mercury fulminate for an example of
another " slow starter " which also then climbs the
velocity ramp to DDT .
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[*] posted on 11-5-2006 at 10:00


Interesting... I happen to have some MHN on hand, and I belive I will try a co-precipitation and then attempt to detonate it as a primary, and just play with it.

Once again, after I recrystallize my TNP, I will get some numbers and figures to work with for the reduction, and hopefully results. I feel empowered. :P




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Rosco Bodine
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[*] posted on 11-5-2006 at 13:46


Here is one of the relevant patents .

It looks like the nitrated polyol like ETN or MHN
is a relatively small percentage of the DDNP composite
and is simply used as a graining binder , densifier
sort of function for the DDNP . A similar idea as
is used with bullseye smokeless powder / acetone
syrup to make AP putty , only more powerful .

Basic lead picrate mixed with nitromannite would probably
do the same trick , and would be easier to make than the
DDNP . I have never experimented with these composites .

Attachment: US2396152 DDNP - nitrated polyol mixtures.pdf (282kB)
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Rosco Bodine
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[*] posted on 11-5-2006 at 13:58


Here is another patent which relates to
the hydrazine product of DDNP ,
and analogues based on hydrazine derivitives .
There is a series of metal salts possible
from reaction of the metal nitrate with
the product from DDNP and hydrazine .

This patent is published by the same
inventor as who disclosed the azo-clathrates .

Attachment: US2728760 DDNP hydrazine product.pdf (123kB)
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[*] posted on 11-5-2006 at 22:37


Havn't seen this come up in any forum, apologies if it has but it is an excellent review of DDNP, synth and explosive properties.

Clarke, L. "<i>Diazodinitrophenol, a Detonating Explosive</i>" Industrial and Engineering Chemistry.; 1933; 25(6); 663-669. [attached]

[Edited on 12-5-2006 by Axt]

Attachment: diazodinitrophenol - a detonating explosive red.pdf (956kB)
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[*] posted on 11-5-2006 at 23:48


Two points:

"It looks like the ... ETN or MHN is a relatively small percentage of the DDNP composite"

Rosco is right as usual, while it stays a good primary with more than its weight of (per)chlorate, I found that an equally big percentage of e.g. MHN hinders DDT in many substances. HMTD and TATP need much bigger charges to reach DDT if mixed 1:1 with MHN, and even silver fulminate stops detonating in small specks.
IIRC it was a mix of MHN and tetracene that detonates from heat. Considering how bad lead picrate is as far as run-distance to detonation is concerned, I doubt LP/MHN will be a good choice.

"... only produce a low density amorphous powder form which is not suitable for dets "

This quote from Rosco I don't understand. The article Axt posted (which *was* posted before but don't ask me where) specifically says both forms have the same strength measured by sand crushing ability. The fine powder may be harder to load on automatic high-speed machines, but since we hardly make thousands of detos, I personally don't mind a fine powder. Plus, will a fine powder not make DDT easier (smaller run-distance, less needed)?
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Rosco Bodine
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[*] posted on 12-5-2006 at 01:18


For any initiator to work properly it needs to
have the ability to compress into a pellet
which doesn't re-expand but holds together
in its pressed form . Some of the crystals
actually crush during pressing and wedge
the uncrushed material in a casing . But
an amorphous powder won't usually form
a stable pellet on pressing , so it won't be
practical . The det you press today may not
fire properly after a couple of days , if the
pellet of initiator swells and crumbles as
it sits . Reenforcing caps are required for
securing the lower density DDNP in the casing
and keeping it at a density where it will
fire properly . This is exactly why I quit
experimenting with DDNP and said I was
not really impressed with it , was the difficulty
with low density material . All of my experiments
with initiators have shown that a certain " grit "
or mesh size of fine crystalline material just
always seems to work better , no matter what
initiating compound is being tested , than is
the case for powdery dustlike materials .

Now weight for weight the total power may be
the same for several grams of either material
in the sand test . But in terms of the sharpness
of an initiating impulse produced by the miniature
" ribbon charge " that is the pellet of initiator pressed
directly in contact with the column of base charge ,
there is a huge difference and advantage for the
more dense material . Initiators do act as a miniature
ribbon charge which is a basic shaped charge on
a micro scale ...so the same charge density benefit
applies , as would be the case for a brick sized
ribbon charge .
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[*] posted on 13-5-2006 at 11:31


6C6H8O6+C6H3N3O7 -> 6C6H7O6+C6H5N3O5+2H2O

Look good? That is a reaction mechanism where the ascorbic acid looses 1 hydrogen. The ratio-by weight- of ascorbic acid to TNP is 4.61:1, so I think 5:1 ascorbic acid to TNP is acceptable, no?




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Rosco Bodine
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[*] posted on 13-5-2006 at 17:24


Yeah for the theoretical , 6 moles of Na ascorbate
for each 1 mole of Na picrate .

A couple of per cent excess of the theoretical
requirement of ascorbic acid for picric acid
reduction is probably sufficient excess ,
and on that basis , use 4.7 grams of ascorbic acid
for each 1 gram of picric acid .

You can do the slightly alkaline neutralization
by using a per cent or two excess of the sodium
salt required , for each of the acids .

mole weight for ascorbic acid is 176.12
mole weight for picric acid is 229.11
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[*] posted on 14-5-2006 at 16:40


Well, it all worked. Due to a hurried addition of HCl to the diazo reaction, I belive I have amorphous product, and I will weigh that yeild to determine how I did.

Everything went according to plan, and I am optimistic.

Is there any way that one can utulize the non-freeflow form of DDNP?




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Rosco Bodine
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[*] posted on 14-5-2006 at 18:40


Could possibly densify it by dissolving in acetone
and then adding toluene ....or naphtha , or xylene,
maybe even white gasoline , maybe methanol
......I'm not sure ,
I'd have to check some references .
But I think there is a cosolvent precipitation method
for densifying the stuff .

Or you could make a methanolic extract of hydrazine
from hydrazine sulfate and experiment with the
hydrazine derivative , and their salts .
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[*] posted on 14-5-2006 at 19:07


Hydrazine sounds constructive, though, my reagents will need serious purifying before I will get any decent yeilds from it.

Too bad I messed up the DDNP batch, eh, live and learn. I am still midly amused the vitamin C actually worked nicely. Good idea ;)

Do you think it would be worth it to make a thread about DPNA? That stands for diazoperchlorate-3-nitroaniline, and apparently is quite fun. Or, perhaps 2,4-dinitrobenzenediazonium perchlorate> Basically, I am interested in aromatic diazo salt primaries. Does that make any sense? :P




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[*] posted on 14-5-2006 at 21:29


I can just see the checkout at the drugstore ,

A thousand aspirin tablets , and a kilo of vitamin C ....

yepper , got one hell of a headache , and feel a bad
case of scurvy coming on :D

That'll do it .:D

About the new thread , no I think there is already some extensive stuff posted on it , search and find .
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[*] posted on 15-5-2006 at 03:17


I still don't get it, according to the above ref also the amorphous stuff presses to 0.86 g/ccm, IIRC even under a low 240 bar. Since it cannot be dead pressed, I don't see why you cannot utilize it just the same. Notably in electric dets which are completely sealed, hence the reenforcing cap is not needed, neither is the "crumbling-out" of the pellet a problem.

I believe if pressed enough, you will get an equally good initiation pulse, and that the only advantage lies in the "free-flowing" property for easy filling my machines.

Swany might test this batch (so it is *not* wasted), and then the next batch (done Rosco's way) to see if it makes a difference in e.g. plate dent testing.
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[*] posted on 15-5-2006 at 06:37


I never tried something easily initiated like MHN as
a base charge for the low density DDNP , where it
would probably be fine . I most often use picric acid
as a base charge , which requires a pretty intense pulse
to initiate . And even for HMTD which has a really
good literature report of performance in unreenforced caps , it can be difficult and take a fair amount , which
is the way it looked for me concerning DDNP of the
fluffy variety ....nothing to campare with say lead azide
for example . So given the difficulty of making DDNP
and the light sensitivity , it just didn't impress me nearly
as good as say lead azide or the azo-clathrates . I
did not extensively test the DDNP , because its performance never seemed to come close to literature
references , and one good example of the exaggerated claims extended to the 50/50 eutectic with picric acid
which was reported in a patent to be fuse sensitive ,
which after my test I was forced to laugh and ask
in what quantities ...ten grams or twenty ? :D
So I just never really was much impressed with the
stuff . But I am sure it has potential usefulness if
the correct conditions are met , I just lost patience
with experiments with DDNP and moved on to other materials , thinking it was too fickle for my liking ,
not really a good general initiator . Azo-clathrates
are so slick I became enamored of them very quickly ,
and lost interest in alternatives which may still have value , particularly if made under more optimized conditions . I'll stay out on a limb here and say the
crystalline form still makes a difference no matter what
the literature may report to the contrary , and I would bet money that tests bear that out .
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[*] posted on 15-5-2006 at 15:02


Yes, I also ran into some trouble as my Na picramate was not totally dry, and was thus still basic and some of the first amounts of HCl were titrated against NaOH, not Na picrate :(

So, the yeilds are a bit off! I will venture to guess I recieved >5g.

Azo-clarthates do look quite interesting, and at one time, I was inspired to try them! I am caught between hydrazine and aromatic diazo perchlorate salts. :P




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