FanofYellow
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PGDN synthesis
Greetings everyone! Here because of the attention of our favorite upside-down and copper-based tetrazole explosive friends from the youtubes. Anyway:
here's my first contribution and a PSA:
PROPYLENE GLYCOL NITRATES DIFFERENTLY THAN GLYCERINE.
used my typical blend for NG synthesis (2/3 95%+ HNO3/95%+ H2SO4) @ <5 degrees c (thanks jacketed beaker), with my typical addition rates and had
runaways 3 times. Evolved a TON of BROWN NO2. Mixture turned brown too before I drowned it with 3x volume of distilled water. Runaways suck, but
they're okay in small batches it turns out. I saw a bunch of NO2 come off right away as temperature spiked to 60o and I said my prayers (honest), but
it really wasn't that bad. Thanks improvised fume hood.
Currently running my 4th batch except doing additions of PG VERY VERY VERY slowly. If there's any interest I'll report back with my final synthesis.
Couldn't find a good one here so made one up on my own.
Addendum: If you're gonna nitrate PG yourself, DON'T BE FOOLED BY THAT TEMPERATURE DROP A FEW SECONDS AFTER ADDITION. THE PG IS LYING TO YOU.
[Edited on 3-2-2022 by FanofYellow]
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B(a)P
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Welcome to the forum!
PGDN
I assume you have seen this thread? From memory the patent in that thread has a method similar to the conditions you describe.
Please do share your synthesis once you are happy with it.
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FanofYellow
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====Until I figure out how to condense these to follow-able instructions, I'm sorry but you guys have to process the raw chemistry to the best of my
ability====
PROPYLENE GLYCOL DI-NITRATE SYNTHESIS. A BY-THE-MINUTE SYNTHESIS FROM A GUY THAT ONLY KNOWS HOW TO TAKE NOTES
Compared to Glycerin synthesis, Propylene Glycol synthesis LOVES to run away from you when you think it's safe. Take whatever time you think NG
synthesis requires and multiply it by 5 to make PGDN. This is a a 'live' synthesis recording.
STARTING:
20mL 90-100% HNO3 (who the fuck knows, it's yellow, lol)
40mL 90-98% H2SO4 (Also, Random drain cleaner. Was clear.)
Cool nitration solution as far as you're capable (4.8 degrees in my case with 2 degree coolant from my chiller)
Once solution is cooled to as low as it goes, add a few drops of Propylene Glycol (99.9% anyhydrous according to my ebay source)
Measured amount of addition was .5mL, or about 15 drops from my addition pipette)
22:48:00
Temperature will immediately spike from 4.8 to 6.0 upon additions
22:48:15
-WARNING- THIS STABILIZATION IS NOT A SIGN TO ADD MORE -WARNING-
Wait about 5 minutes 22:53:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette)
22:58:00
Temperature will immediately spike. (5.0 to 6.3 in my case)
-WARNING- THIS STABILIZATION IS NOT A SIGN TO ADD MORE -WARNING-
22:58:15
You'll see that the temperature stabilizes at this point after expecting it to go down.
I think this is a weird quirk of nitrating Propylene Glycol, and it's much safer to wait
for temperatures to stabilize at your starting before proceeding with additions.
I had 3 runaway reactions (lots of NOx evolution plus my mix turning sewage-water
brown) and was deceived a few times by the delayed nitration of PG
BE CAREFUL and have your drowning solution on hand whilst attempting this.
Blowing on my mix evolved fumes, which indicates some kind of life to the nitrating
mixture still. Can you tell I'm not a real chemist and just taking notes for what I see?
Mixture is back at starting (4.8 degrees) 23:01:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
23:02:00
Immediate temperature increase to 5.8 degrees
-WARNING- THIS STABILIZATION IS NOT A SIGN TO ADD MORE -WARNING-
Still holding at 5.4 degrees after 4 minutes compared to previous
additions. I think this is where the PG nitration differs from
regular glycerin synthesis. 23:06:00
Allow to settle back to baseline temperature (4.8 degrees)
Temperature stabilized at 5.2 degrees (2.5 coolant) 23:13:30
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 6.2 degrees 23:14:00
Temperature stabilized at 5.5 degrees (3.1 coolant) 23:14:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 6.5 degrees 23:26:00
Temperature stabilized at 5.2 degrees (3.4 coolant) 23:31:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 6.4 degrees 23:32:00
Temperature stabilized at 5.6 degrees (3.9 coolant) 23:38:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 6.5 degrees 23:39:00
4.0 degree Setpoint. Chiller kicks on 23:40:00
Temperature stabilized at 5.5 degrees (3.8 coolant) 23:46:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 6.2 degrees 23:48:00
Temperature stabilized at 5.1 degrees (3.1 coolant) 23:58:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 5.9 degrees 0:00:00
Temperature stabilized at 4.9 degrees (2.6 coolant) 0:04:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 6.0 degrees 0:05:00
Note: Mix temperature is starting to fall more quickly
Hypothesis: Nitration mixture is being 'used up', reactions happen
slower
Temperature stabilized at 4.9 degrees (2.4 coolant) 0:08:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 5.4 degrees 0:09:00
Temperature stabilized at 4.7 degrees (2.3 coolant) 0:13:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 5.5 degrees 0:14:00
Temperature stabilized at 4.5 degrees (2.1 coolant) 0:19:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 5.3 degrees 0:19:00
Temperature stabilized at 4.1 degrees (2.0 coolant) 0:25:00
Add .5mL Propylene Glycol (about 15 drops from transfer pipette) 0.5
Immediate temperature increase to 5.2 degrees 0:26:00
Temperature stabilized at 4.3 degrees (2.0 coolant) 0:31:00
Add .5mL Propylene Glycol (squirting in at this point) 0.5
Immediate temperature increase to 5.0 degrees 0:32:00
turned off stirring.
Solution is milky, no coalescence like with NG synthesis.
Blowing on the nitration solution still produced visible fumes.
Turned stirring back on.
Temperature stabilized at 4.3 degrees (2.0 coolant) 0:36:00
Add .5mL Propylene Glycol (squirting in at this point) 0.5
Immediate temperature increase to 4.9 degrees 0:36:00
Wife got home, Son woke up, had to be a dad. Excuse the
discrepancy in times/measurements lol
Temperature stabilized at 4.1 degrees (2.0 coolant) 0:49:00
Add .5mL Propylene Glycol (squirting in at this point) 0.5
Immediate temperature increase to 4.8 degrees 0:51:00
Temperature stabilized at 4.1 degrees (2.0 coolant) 0:54:00
Add .5mL Propylene Glycol (squirting in at this point) 0.5
Immediate temperature increase to 4.9 degrees 0:55:00
Temperature stabilized at 4.1 degrees (2.0 coolant) 0:58:00
Add 1mL Propylene Glycol (squirting in at this point) 1
Immediate temperature increase to 5.3 degrees 0:59:00
Temperature stabilized at 4.1 degrees (2.1 coolant) 1:02:00
Add 1mL Propylene Glycol (squirting in at this point) 1
Immediate temperature increase to 5.3 degrees 1:03:00
Temperature stabilized at 4.6 degrees (2.2 coolant) 1:08:00
Add 1mL Propylene Glycol (squirting in at this point) 1
Immediate temperature increase to 6.0 degrees 1:09:00
Temperature paused at 4.8 degrees (2.3 coolant) 1:12:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 6.4 degrees 1:14:00
pH check: 3/4
Temperature paused at 4.7 degrees (2.5 coolant) 1:18:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 6.2 degrees 1:20:00
Temperature paused at 5.0 degrees (2.8 coolant) 1:26:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 6.6 degrees 1:28:00
Temperature paused at 5.1 degrees (3.0 coolant) 1:33:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 6.6 degrees 1:35:00
Temperature paused at 5.1 degrees (3.5 coolant) 1:42:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 6.1 degrees 1:43:00
Temperature paused at 5.9 degrees (3.8 coolant) 1:47:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 6.7 degrees 1:48:00
Temperature paused at 6.2 degrees (4.0 coolant) 1:51:00
Add 1.5mL Propylene Glycol (squirting in at this point) 1.5
Immediate temperature increase to 7.0 degrees 1:52:00
Decided to terminate nitration at this point. Crashing out to 200mL
chilled Distilled water @ 0 degrees
Crashed out into 200mL of 0 degree water Can see droplets of 1:59:00
SOMETHING collecting on surface. Gave 'hearty' stir with clean
glass stir rod and allowed to coalesce while taking these notes.
Gave up trying to separate. Moved product 'soup' to 'cold room'
while allowing to separate and colalesce. Currently being burned
by acid mixture while I type this. (WHERE THE **** IS MY NEUTRAL
IZING POWDER ****************
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FanofYellow
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I forget how to edit posts for old-style forums like these (been a while lol)
Please edit my previous post to this:
Hey again guys. Sorry for the wait.
Happy with my synthesis, so here's the condensed version for addition into the PGDN thread:
Compared to Glycerin synthesis, Propylene Glycol synthesis LOVES to run away from you when you think it's safe. Take whatever time you think NG
synthesis requires and multiply it by 5 to make PGDN.
STARTING:
20mL 90-100% HNO3
40mL 90-98% H2SO4
40mL Propylene Glycol anhydrous (way excessive)
Cool nitration solution as far as you're capable (4.8 degrees in my case with 2 degree coolant from my chiller, picture of Reaction vessel with
Antifreeze mix running through it).
http://swalltronics.com/chemistry/PGDN/chilled_acid.jpg
Once solution is cooled to as low as it goes, add a few drops of Propylene Glycol (99.9% anhydrous according to my eBay source). I added 0.5mL but you
could go to 1mL without any problems as long as your nitration solution is 'hot'. In my case it turned out to be about 10 drops/mL with my addition
pipettes.
You'll see that the temperature stabilizes at this point after expecting it to go down immediately like with NG.
I think this is a weird quirk of nitrating Propylene Glycol, and it's much safer to wait
for temperatures to stabilize at your starting before proceeding with additions.
I had 3 runaway reactions (lots of NOx evolution plus my mix turning sewage-water
brown) and was deceived a few times by the delayed nitration of PG
BE CAREFUL and have your drowning solution on hand whilst attempting this.
I didn't calculate any stoichiometry (shame on me), but after every addition I waited for temperature to stabilize before adding again. As soon I
added the next round of Propylene Glycol and didn't observe any temperature change I drowned the whole thing in ice-cold distilled water and then
transferred this to a beaker to allow coalescence to happen.
http://swalltronics.com/chemistry/PGDN/End_synthesis.jpg
http://swalltronics.com/chemistry/PGDN/Before_coalescence.jp...
http://swalltronics.com/chemistry/PGDN/After_coalescence.jpg
I moved this final beaker to my 'mud room' where the temperature is at refrigerator levels but without worry of poisoning my family. After coalescence
happened, I pipetted my end product off and washed it twice in a saturated sodium bicarbonate solution.
http://swalltronics.com/chemistry/PGDN/Second_wash.jpg
No gas was evolved during the second washing so I switched over to washing with cold tap water and transferred the final product to my Polypropylene
test tubes for storage outside.
http://swalltronics.com/chemistry/PGDN/Final_wash.jpg
http://swalltronics.com/chemistry/PGDN/Finished_product.jpg
End product looks the same as my nitroglycerin to me and gives me an equally bad headache the next day when I was dumb enough not to have gloves on
for one of the stages. Not really sure how to test it or clear up the cloudiness but would appreciate suggestions.
[Edited on 9-2-2022 by FanofYellow]
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Laboratory of Liptakov
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Just out of curiosity, I ask, will your PGDN have any end purpose? Or is the whole effort just a skill test? ...
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite (2024)
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katyushaslab
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You will probably want to remove the excess water by washing with saturated salt soln or similar? Looks awful "wet" as-is, and from experience, you
don't want to store liquid nitric esters "wet" with water. It seems to promote decomposition.
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FanofYellow
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I honestly have no idea. I know I'm not going to set everything off at once, but I might do a shock test with a few drops. I've compared the freezing
point to regular NG (20oF here), and the PGDN is staying viscous but not freezing like the NG, which is a solid pellet right now. Kind of worried
about when it starts getting warm, I might dig a small hole and bury the whole thing back in the corner of the yard
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FanofYellow
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Quote: Originally posted by katyushaslab  | | You will probably want to remove the excess water by washing with saturated salt soln or similar? Looks awful "wet" as-is, and from experience, you
don't want to store liquid nitric esters "wet" with water. It seems to promote decomposition. |
I'm not sure how to do this, Do I just dissolve a ton of NaCl in water and mix the two? Throw granulated salt into the mix and let it dry?
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katyushaslab
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Make a saturated solution of salt, mix well with the PGDN, and wait for it to phase separate. Take off the organic (PGDN) layer, discard the saltwater
layer.
If your product is still cloudy, its still wet. Further drying over reasonably anhydrous magnesium sulfate (just bung some epsom salts in the oven on
high for a few hours to get this), or dry calcium chloride should help a shitload.
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MineMan
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Maybe you could make some naan with it??
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ManyInterests
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This sounds really interesting, since I was thinking of making NG or even methyl nitrate (is methyl nitrate more sensitive than NG or less sensitive?)
once I get back in the energetics hobby. But if you can do everything with PGDN that you can do with NG and it's safer (albeit more challenging to
make) than I might try to make a few batches of that.
Would mixing it with normal sawdust or shredded paper make for a proper absorbent? Also would it be useful for making double base gunpowder? I'm
interesting in making my own smokeless gunpowder in the future. I know that double base powder is often a combination of nitrocellulose (which I am
fairly experienced in making) and NG. But NG is obviously no joke, and if PGDN can be substituted for it, I'll definitely go that route.
| Quote: | | If your product is still cloudy, its still wet. Further drying over reasonably anhydrous magnesium sulfate (just bung some epsom salts in the oven on
high for a few hours to get this), or dry calcium chloride should help a shitload. |
When you say dry over, you mean put the container of PGDN in another container full of epsom salts or calcium chloride? Would epsom salts work in lieu
of calcium chloride, because epsom salts are available everywhere where I live. Also by 'high' in your oven, you mean in the range of 200-220C/425-450
F?
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FanofYellow
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edit 3: I give up with quotes.
Edit 2: STILL screwed them up haha
Edit: I screwed up the Quote tags
[/rquote=670986&tid=158342&author=ManyInterests]
When you say dry over, you mean put the container of PGDN in another container full of epsom salts or calcium chloride? Would epsom salts work in lieu
of calcium chloride, because epsom salts are available everywhere where I live. Also by 'high' in your oven, you mean in the range of 200-220C/425-450
F?
[/rquote]
I believe katyushaslab is talking about NaCl (didn't specify), that's what I'm going to try.
PLEASE keep in the front of your mind that nitration happens with a DELAY for this reaction. I had three runaways because it tricked me before I
realized, make sure your temperature is rock solid for at least.... 5? Minutes before doing your next small addition. My runaways were realized by a
huge spike in temperature (I think 5c to >60c in less than the sample rate of my thermometer=1 second), the mix turning shit brown and more NO2
than I thought my janky fume extractor could handle (it did, no edema lol-I'm a terrible chemist).
[Edited on 12-2-2022 by FanofYellow]
[Edited on 12-2-2022 by FanofYellow]
[Edited on 12-2-2022 by FanofYellow]
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katyushaslab
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So for drying liquids like this that are full of water from washing steps, I usually go in two stages.
Firstly, drying with a saturated salt (NaCl) solution in a separatory funnel, this gets rid of a good amount of the water it picks up from washing
steps.
Secondly, drying by putting it in a beaker with a bunch of anhydrous magnesium sulfate or anhydrous calcium chloride - you mix the PGDN (or other
liquid) with the drying agent. This should pick up the rest of the water. You can simply filter or decant to get your product.
To get anhydrous magnesium sulfate, I simply put a layer of epsom salts in a lasagne dish in the oven, as high as it can go, and leave it for a few
hours until all the water fucks off.
For storage over "longer than a couple of days", in the past I would dilute NG with ~20% or so of acetone - so 80 grams NG to 20 grams of acetone.
This rendered it fairly safe to store, though still detonable with a small booster or particularly strong cap. When you need the NG on its own, just
let the acetone evaporate. I think this will work with PGDN as well.
I have no idea if PGDN will form a collidon or whatever with nitrocellulose.
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ManyInterests
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Just a tip on using the quotes. You can type them down like this
quote]
Insert text you want to quote here.
/quote]
Just add an additional [ at the start of the word quote, of course.
| Quote: |
PLEASE keep in the front of your mind that nitration happens with a DELAY for this reaction. I had three runaways because it tricked me before I
realized, make sure your temperature is rock solid for at least.... 5? Minutes before doing your next small addition. My runaways were realized by a
huge spike in temperature (I think 5c to >60c in less than the sample rate of my thermometer=1 second), the mix turning shit brown and more NO2
than I thought my janky fume extractor could handle (it did, no edema lol-I'm a terrible chemist).
|
Yes. I am aware of just how dangerous some nitrations can be. I wanted to do a Keto-RDX synthesis (my last synthesis before I put chemistry on the
backburner for now) and due to a variety of factors I did have a fairly dramatic runaway. In part because I underestimated just how exothermic
hexamine in a fuming nitric acid/sulfuric acid nitration mixture was. Also because my thermometer had its measure marks burned off from a previous
runaway, and the fact that I didn't realize how much expansion it would make while nitrating it, and my 250 ml beaker was not enough to hold
everything, and my next bigger thing was a 1000ml beaker (I now have a 500ml beaker that I will use for future nitrations of that scale). That bobbed
up and down in my ice bath since the volume of the mixture was now too small to anchor it in place (I don't have a jacketed beaker. I won't get one
since those are too expensive. But they look AWESOME).
It was then that I had no idea how hot it was and just put in the remaining hexamine (there was a spoonful left) and it caused a runaway. Thankfully I
got away unharmed.
But yes. I will look at your notes (they are VERY detailed) and make sure that with every addition I wait 5 or more minutes before putting in the
next. I will need to get an eye dropper to make sure I don't put in more than 0.5ml.
| Quote: |
Firstly, drying with a saturated salt (NaCl) solution in a separatory funnel, this gets rid of a good amount of the water it picks up from washing
steps.
|
I don't have a separatory funnel. But I have seen videos were people used it in the manner you describe to dry out methyl nitrate. Is there another
way of doing it? Like drawing off the cleaner product from a beaker using a pipette? Those funnels can be pricey and I am not sure I want to buy one.
| Quote: | | Secondly, drying by putting it in a beaker with a bunch of anhydrous magnesium sulfate or anhydrous calcium chloride - you mix the PGDN (or other
liquid) with the drying agent. This should pick up the rest of the water. You can simply filter or decant to get your product.
|
Ok so pour the PGDN/NG directly into the magnesium sulfate? It won't affect the PGDN or NG? I guess that can work and decanting/filtering with coffee
filters sounds easy enough.
| Quote: | | To get anhydrous magnesium sulfate, I simply put a layer of epsom salts in a lasagne dish in the oven, as high as it can go, and leave it for a few
hours until all the water fucks off. |
I like the way you put it! 'until all the water fucks off'! My trusty lasagna baking dish has seen more chemicals go through it (potassium nitrate,
potassium chlorate, hydrazine byproducts, nitric acid to neturalized, etc etc) than it has actual lasagna. It's purely for chemsitry since no matter
how inert the pyrex glass dish is, I won't be cooking anything I will put in my mouth with it.
For the temp, the max it can go is 250C, so I guess that's what I will set it to for a couple of hours. Any earlier preparation of the epsom salts are
needed? Like crushing them or something or the other?
| Quote: | | For storage over "longer than a couple of days", in the past I would dilute NG with ~20% or so of acetone - so 80 grams NG to 20 grams of acetone.
This rendered it fairly safe to store, though still detonable with a small booster or particularly strong cap. When you need the NG on its own, just
let the acetone evaporate. I think this will work with PGDN as well. |
That sounds good. I made blasting caps with 1 gram of ETN and 0.4 grams of NHN. Those are more powerful than conventional military blasting caps
(which I believe use around 0.5 grams of RDX or PETN with a small amount of ASA (lead azide, lead styphnate, aluminum) as the primary mixture. I think
that might be sufficient to detonate the dilute amount.
But if I wanted to do that, I would want to try to see if I can turn the PGDN into dynamite first by using a sorbant. I might not have access to
diatomeceous earth, but I did hear that simple sawdust is good enough. I can get a block of wood and just drill at it to make ultra fine sawdust as an
sorbant.
| Quote: | | I have no idea if PGDN will form a collidon or whatever with nitrocellulose. |
Well then! I think this experiment (when the time comes that I get back into chemistry) will be a focus of mine. Try to see if PGDN is a good
substitute for NG when making smokeless gunpowder.
I will document what I did and report it here. I don't have a background in chemistry beyond what I did in making some energetics, but this is
something I maybe can contribute to. I find that exciting.
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Herr Haber
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Definitive answer will be in Urbanski along with a ton of other data but I'm sure it does.
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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ManyInterests
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That sounds good. It'll be an interesting challenge to make some home made gunpowder and priming mixture.
While this might be unrelated to this thread... do you know where I can get some antimony sulfide? It appears to be a key ingredient in priming
compounds. Some older priming compounds use it in conjuction with potassium chlorate (the corrosive kind) or mercury fulminate (the non-corrosive
kind). I know that white phosphorous (from strike anywhere matches) and armstrongs mixture (which can be made from safety matches and the red
phosphorous of the striker pad), but those are also corrosive and aren't challenging to make.
But maybe I should make a bit of armstrongs mixture.
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Herr Haber
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Sb2S3 is a "common" ingredient in pyrotechnics to make white fires so it shouldnt be too hard to find.
Or replace. I'm sure you could find half a dozen primer composition that are sensitive to impact / mechanical stimuli in one of Conklin's book. Very
good read.
You definitely dont want armstrong mixture at the beginning of a pyrotechnic train that ends with a bullet !
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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ManyInterests
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I'll have to look up Conklin's book. It rings a bell, but I am not sure if it is the book I think it is. I also would like to see what needs to be
done to make double base smokeless powder. Like stuff for both pistol and rifle and powders if possible.
I also did see in the thread on PGDN (posted above) that PGDN is safer than NG or EGDN, but I am never really sure what that means. I did see a video
of MEKP where bits of the MEKP were smacked with a hammer several times before popping, but I've said in many previous videos that I refuse to deal
with any peroxide based explosives.
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