Danger. Home made…

Alright. Finally was able to get over and granulate my mixture. 
 

12 hours tumbling

the apparatus:

i mixed it by hand with some 91% isopropyl. Water works too, but takes way longer to dry. 
 

a light breeze and some sunlight for about 45 minutes:

I learned a couple things. 1-The alcohol dries fast, so a wetter putty isn't a dealbreaker. 2-Pressure used while grating is important; a light touch seems to be better. 3- I'll use a soft brush next time to kind of spread out the granules and help separate them. 
 

And the results

im satisfied with the results. Up next is testing in the rifle. 
 

Please be safe out there. Don't do what I do unless you remember two things:

1- IM AN IDIOT. 
2- Im extremely lucky. If the world were fair, I'd have died years ago, but somehow I keep surviving. Do not let my survival lull you into any sense of security. 

Remember when I said this was an experiment? Well, it's a successful one because I'm learning. That said, my current product is not what I want to end up with. The granules are unstable. Like a sandcastle, shape it wet and let it dry and it will hold shape until you touch it. 

Supplied in my 10lb kit was a bag of dextrin, which is a binder. It'll keep the granules together very well, but it will foul the gun in a hurry. there are other binders, redgum, rice starch, others. These are still not ideal. 
 

So I'm back to pressing the powder. I know this is what is done commercially. From what I understand (again, not a chemist) this causes the sulfer to plasticize and act as a binder. 
Some reading suggests most folks use a 12ton press, but apparently the HF 6 ton press will work with slight modifications.

Then I'll need tooling. You can buy dies from the reloading suppliers or the chemical suppliers($$$), but apparently it's the drug folks who make the most cost effective solution. 

So. That's where I am at. I need to order some tools. 
 

Now, this process is a little different and slower. Instead of putty, we just need enough water (not alcohol with this method) to keep the dust down. Load an oz or two in the die and slowly press until it won't anymore. Let sit for 10 minutes and remove the product and let dry thoroughly. This will give a solid and hard puck.
 

Once dry, use a rolling pin to crush it into granules. The results will not be uniform. Using the same screen I granulated with before, I'll filter out the usable powder (aiming for FFFg) and recycle the rest. Anything too large can be broken down, and anything too small can be wetted, dried, briefly milled again and reloaded into the press. 
 

This method yields a 15-20% denser product. Denser explosions are more powerful and therefor require less volume per load. We're saving powder here, folks. 
 

Quick math says the first 10lbs or powder costs around $250, but the tooling should last a very long time. 10lb of commercial product is currently about $300 if you can find any. Obviously the cost drops drastically after the first batch. Hopefully I can pick up the tooling soon, because I'm eager to keep learning. That said, I e got some personal stuff coming up soon and I'll be on a pretty strict limit for what I can lift and do physically for a couple months, so I'm really not in a rush. 

Fascinating!

What precautions are you using to mitigate static electricity?

Scott

I've made several 100 pounds of black powder and fireworks. There are a bunch of recipes and ways to do it. If you spend some time on the fireworks forums the horror stories of the mistakes people have made are endless. Houses burned down. Death. Maiming. There is a lot of power in these little black grains. Treat it with respect.

A couple of suggestions. Pay close attention to the humidity when mixing and working with these chemicals. The tiniest spark can set it off. My rule was if the humidity was below 55%, I would not work with anything explosive. The chance of static sparks was too high. Anything below 70% I wore an antistatic wrist strap. I made most of my black powder during the summer months and stocked up for the winter. Stars as a general rule aren't explosive so I could make them year-round but I still usually didn't work with the chemicals when it was dry. 

PPE. Wear a full face shield, not goggles. And make it a good one. You aren't just trying to stop dust or debris, you want to stop the fire or explosion from taking away your eyes. The flimsy HF junk won't do the job. 

Wear insulated leather gloves with latex gloves over them. Again, think fire and explosion. Black powder burns very quickly but it also burns very hot. Protect those hands. 

I would also wear long sleeve cotton shirts and a thick jacket. I had a Carhart canvas jacket that I wore that I had sprayed with a flame retardant. Even when it was hot I would keep the jacket zipped up and deal with the sweat.

Work with small quantities. It's tempting to mix up a 10-20 pound batch. More is always better. Until you have an accident. My maximum in any stage of production was around 2 pounds. So I would have 2 pounds in the ball mill, 2 pounds drying and being caked, 2 pounds being screened. These quantities were never on the bench at the same time nor stored in the same area of the shop. Physical separation is the best way to contain a fire. I stored just about everything in paint cans. The metal cans ground themselves, and with the lids on loosely will direct any explosion up. You can buy the cans from Lowes. My drying trays were aluminum baking pans. Again because they self grounding. I didn't mix anything in plastic containers. 

Any time you are creating dust, I consider that to be a bad thing. I ball-milled charcoal wet, I ball-milled the powder wet. I used water. Yes, it slows down the process, but it also substantially reduces the chance of an explosion. I would recommend using lead balls as well. They will not generate a spark when striking each other. 

Get out the fire extinguishers. I still have 6 fire extinguishers around my shop leftover from my fireworks days. I wanted one within arms reach at all times. 

I made fireworks and black powder for 6-8 years. Everything from smoke bombs to 4" mortars. Luckily, I never made a mistake that resulted in a fire or injury. 

This stuff is the real deal. It can be a lot of fun, and it can and will ruin your life. Treat it accordingly.

In reply to Toyman! :

Thanks for the input! Any information on technique, recipes, safety, or anything else is highly appreciated. 
Re. Quantities: I can only do about 8oz in the mill, and I don't plan to have more than 1lb in a given place. 
Humidity? I'm in Utah, we don't have any. 
Static is something I hadn't considered, and I'll definitely take steps to mitigate that risk. I plan to do everything outside, so grounding should be pretty easy. 

I like the paint cans for storage, but they may be a bit overkill for the volumes I plan to work with. This isn't for fireworks, but for muzzleloaders and a couple lbs should last me a year. 
 

I'll likely wait to mix any more until I have a method finalized for granulating. Maybe another 8oz if I need to experiment. Definitely not more. 
That said, 1 lb final product should get me 100+ shots, and with the limits of flintlocks, that's at least 5 outings, which for me means 2-3 months worth. Maybe more. A little goes a long way, and I'm not a prepper. 

In reply to Toyman! :

Question regarding wet milling. I like the idea. Is there a certain volume of water that seems to work best? Drying time is no issue for me. 

Wet milling I used enough water or alcohol to keep the mix from caking. Basically it needs to be wet enough to keep it from sticking to the balls and mill. I would then filter and press it in cloth to remove the excess water and granulated the cakes while still damp. 

For granulating, I pushed the mix through a piece of fiberglass screen. IIRC fireworks uses a coarser grain than guns. 

As for static, metal pans, a well grounded metal work surface, and a grounding wrist strap should take care of a lot of it.

I will have to see if I can find my notes from back then. Most of my mixtures came from the fireworks forum and a book.

In reply to Toyman! :

Thanks! 
 

I'll be revising my granulating method as noted in my post above. Screens are out, as I'm not using a binding agent (cause fouling in firearms)

I'll have to experiment with water. Shouldn't be too difficult. 

In my time in paint supply we could get paint cans down to 4oz. 
I don't have any interest in guns but this is super neat. 
 

I worked in a munitions and black powder fuse plant for seven years, way back when, so I'll reinforce a few things.

Static can kill you. Ground everything, including yourself. Be very aware of any synthetic clothing you own and don't wear it.

No steel tools, use brass or copper if possible because they're non-sparking.

When storing finished powder in any type of container (we had cardboard barrels) put a paper tube down the  center of the container. Toilet paper rolls or waxed paper tubes work great. They'll behave like a pressure safety relief in the event of it catching fire. They only work when the container is open. Once you put a lid on it ceases to be effective.

Always work in a space where you can turn and sprint straight out of the building in the event anything goes wrong. Our 2nd floor powder hoppers had a crash door leading to an escape slide every 10 feet so operators only had to turn around and dive headfirst through the doors.

If this sounds excessive, it may be. We used 35 lb containers of powder and there were many in each location. The operating and safety principles still apply. We had enough stuff around to knock down the building or kill an operator , while you're only talking enough to really hurt yourself, but that could be blinding or serious burns. Take care.

In reply to DeadSkunk (Warren) :

Thanks for the input. Yes, small volumes, but safety is still key. 
my strainer is stainless, and my cookie sheet is aluminum. The pressing die I ordered is aluminum and the press will be outside and grounded. Still nervous about the press, if I'm honest. Hopefully a damp mixture and lack of a heat source... maybe I set up a shielding wall out back. 

In reply to barefootskater5000 :

The idea of static electricity came to me when I saw the powder residue sticking to the sides of your plastic container.

In reply to Noddaz :

I had the thought, though it didn't really register. My thinking was that the commercial stuff comes in plastic bottles... And I had planned to store mine in a reused pyrodex jar. So I didn't give it any more thought. 

Updates finally. I've decided to use glass jars for storage. Specifically Adams peanut butter jars because otherwise I'll just throw them away...

I haven't mixed any more. I have some ingredients measured and ready, but I wanted to do some testing before I mixed more. 
 

Now, I've been told that you can use the powder in this super fine form, but because science you need to run 10-15% higher charge and it won't have the same consistency in ballistics as granulated stuff. So, we granulate. In that vein, I made this:

Which is just a small press. Or will be when combined with my little 6T bottle jack. My reason for building this is because of size and cost. The C channel was in the scrap pile and should be more than strong enough. And under 10lbs means I can easily carry it out and away from house and shop. Gonna paint it red and call it done. 
 

I took out my previously mixed powder yesterday and did another test burn. If anything, the time it has had to fully dry has been good. Seemed to burn even faster. Hopefully next weekend I can make time to press some of it into pucks. That involves a little water and will require a week or two to dry before I can crush and screen it to size. 

Keep in mind that glass is not only an insulator for any static electricity buildup, it also turns into thousands of pieces of really sharp shrapnel when it explodes. 

I would also consider using an air-over hydraulic cylinder so you can do your pressing from a distance. Flammables, closed places, and pressure = spectacular explosions. 

Yes, I am a little paranoid. 

Have fun!

Be Safe!

In reply to Toyman! :

Hadn't considered air/hydraulic. I'll look into that. The amount of powder I'll be pressing at a time is only about 100 grains, and will be slightly wet. It will be in a stainless sleeve, and I honestly don't know what the failure point would be if something went bad. 

M2Pilot said:

Floating Doc (Forum Supporter) said:

I was going to add this to the meme thread, but it sort of fits here. 

We used to do that to some extent. My uncle blew up a lot of stumps in a pasture on our farm that we were changing to row crops.

I had a 2nd cousin who was missing a thumb because of a blasting cap mishap while he was farming with dynamite.

When my dad was still knee high to a grasshopper, (born in 1929) his father dug a canal out with powder sticks, in from the York river into an old farmers land; that land is now the spook base in VA; anybody that knows where that is, may have seen that canal 

It is still there, but I have not seen it. 
After my dads father was gone, he has story's from his teens of buying a few sticks (14 to 15 years old!) at he hardware store to clear stumps. He was much more responsible as a teen than me!

Put your tumbler outside on a nice long extension cord. Put it in the closest thing you can make to a roofless vault so stuff goes up not out. 

The longer you tumble it the better the results but the more likely you are to have something go pearshaped whilst tumbling.

You can get a really good facsimile to corned powder by wetting the finished product to thick paste texture and pushing it through an appropriately sized seive and sizing the results and then dry it out real good...

i wetted and pressed two pucks. I "measured" about 10ml in a medicine cup and mixed in some water with a toothpick until it wouldn't stick to the cup. Cleaned the die and away we go. Away from everything, that is. It's amazing how much the stuff compresses. I cranked the jack until it really started to fight and let sit for 5 minutes. We get a nice smooth puck:

I know paper towels are not ideal. I could not find my cookie sheet. I made two as proof of concept. I've been told to let this sit and dry for a week or two. So that's where we are. 

Once I'm ready to break these down into granules, I'll be experimenting a bit. My basic plan is my aluminum rolling pin and some stainless strainers. I've seen folks use meat grinders, but A- I don't have one, and 2- something about that doesn't seem like a great idea. Not sure why. 

In reply to barefootcyborg5000 :

I really like all the safety tips that have been mentioned! And really love your disclaimers!!!!

I was not the most safety oriented guy growing up... hey I remember napping in the package shelf under the back window of a 63 galaxy, on road trips. Different times. Living through my life does make me a safety mentor now! And the best teaching is setting a good example!

I am not sure of the best answer, but I would worry about the contact pressure that a stainless rolling pin could generate on a small grain. Something softer might be good. Not saying grinder, but since it was mentioned, a grinder can be set so that the metal grinding bits never touch each other.

I guess you can test with little tiny dots of powder you made and see how hard you have to treat them to get ignition. Try hammers and whatnot, just so you know. Just pretend you are trying to make cap gun caps.

In regards to the press, does the mold have a vent hole? Should it? A lot of rifles have a hole in the receiver in the event of a pressure "excursion" or just a blown case. A vent cuts down the pressure spike and can help the gizmo from becoming a grenade. Yes, some powder would leak out, but you may still get a good enough puck.

Just thoughts while waiting for the real BP experts to chime in.

In reply to matthewmcl :

The stainless die isn't vented. It isn't exactly sealed either. The water in the powder does drain out when squeezed. 
As for the rolling pin, mine is aluminum. And I'll be rolling on an aluminum cookie sheet. Outside. With sleeves and a shield on my face. Maybe it's overkill, idk. I'm at least a couple weeks before I attempt anything. Maybe more; it's hot out. 
 

Eyeballing it, these pucks are about the size I was aiming for, and I suspect if I get 100% yield from each puck I might have enough for 4 shots. This method is cheap, but hardly efficient. Still, I could likely make 10 in an hour. I suspect it'll take longer to crush and screen. As for screening, I'm starting with a guess. I have two stainless strainers of different mesh. My goal is something approximating fffg. My screens may not be the right sizes but I won't know until I try. 

Starting to wonder how difficult it might be to fabricate a grinder or modify one with copper bits. I have a rather good source of (legal!) scrap copper and the ability to solder/braze... to eBay I go.

I made some more pucks tonight. A storm rolled through making the ground just wet enough to cut the dust, and raising the humidity to florida levels. But most importantly, it cooled us way down. 
I learned some things

1- I can mix way wetter. The extra simply squeezes out the mold. This is good because in my mind wetter powder is less dangerous. 

2- I can squeeze harder. This may be good or it may be overkill. I don't have a way to measure the pressure so I'm hoping it doesn't effect consistency. 

3- I can granulate right after compressing. My testing shows that the compressed powder is still very stable once crushed even when still slightly wet. These little granules are tough. Which means the process works. Great news.

4- I need to find a quicker way to grind the pucks. They can be broken into smaller chunks by hand (a benefit to making thin pucks) but my method of essentially pestle-mortar grinding using a big brass punch in a 6" stainless kitchen strainer is super slow.

5- I got lucky in guessing the right size of screens. Having no experience to draw on, I eyeballed two the I thought would be a minimum and maximum size. Even better is the fact that they are the same size and can be stacked in use:

I did not plan this. But what I've found is I can keep two jars, one for unprocessed stuff, and the other for a finished product ready to be dried. Stacking the course mesh inside the fine and placing both over the unprocessed jar (outside, don't worry) I grind the pucks. Anything that makes it through the course mesh is small enough to use, and the stuff that is too fine falls through and back into the 1st jar to be reprocessed. What is left in the fine strainer gets put into the finished jar. 
What I end up with seems to be about 80% of the puck being good and the rest can be reprocessed later. 

slow though. 
I'm thinking maybe some brass-toothed pliers might make quick work of the bulk of crushing. The pucks are small. 40mm diameter. Idk. I'll think of something. Maybe there's such a thing as a brass rasp. Off to the internet. 

Might find something in barillium bronze. MUCH harder than brass, and non sparking!! I know it when I see it, have used everything fro a 12" adjustable to a chisel... just can't spell it!