Apparently there's interest here, so I'll start a thread.
PLEASE USE EXTREME CAUTION. IF YOU DOUBT YOUR ABILITY TO DO THIS SAFELY, JUST DONT.
Also, if our hosts deem this inappropriate, please, nuke the thread.
PPE. PPE. PPE. PPE.
Understand that I am not a professional, I'm going off instructions from several sources including the manufacturer of the chemicals I'll be using. If you've done this before and see me doing something wrong or unsafe, CALL ME OUT.
Also, do not take what I say as gospel. This is a learning experience for me. I am no chemist.
Now that's said, here we go.
Black powder. The organic stuff. This is messy, smelly, corrosive, and a whole lot of fun.
You may ask why I'm bothering, since pyrodex and triple 7 are synthetic substitutes and both are readily available. The reason is because I want to learn how, and because my flintlock can't use the synthetic substitutes due to higher ignition temps and slower burn rates. The last US manufacturer of BP shut its doors in September and best I can figure is the import stuff won't be available for several months. Coupled with the going rates of $30/lb, I've decided to roll my own.
The ingredients are simple enough: charcoal, sulfer, and potassium nitrate (saltpeter). I'll not give the mixture here, but it is easily available with a quick google. I ordered my chemicals from https://www.skylighter.com/ $52 plus shipping gets you 10lbs worth. Included in the kit is a bag of dextrin but this should not be used for powder used in firearms, as it will cause excessive fouling and result in ignition issues.
There are several methods of mixing, but the one I'm using and recommending is tumbling. The media will fully powderize and mix the ingredients. Most folks recommend using hardened lead shot for media in the tumbler, but I can't find anyone with stock, so I used marbles. DO NOT USE STEEL OR ROCKS! RISK OF SPARKS COULD CAUSE EXPLOSION! Regular lead shot will result in lead dust in your mixture, this is not ideal.
Rotary tumbler. FIL granted me the use of his HF rotary tumbler. Skylighters recommends the same unit (which they sell at a higher price) and they include instructions to alter the operating rpm. I've not done this, and most folks I talk to or read/watch make no mention of it. Since we use this tumbler for cleaning brass and other things on the regular, I elected not to muck with it.
PPE! PPE! PPE! PERSONAL PROTECTIVE EQUIPMENT!
Everything I've found and the one local old timer I've talked to say that more time tumbling is better. 10-12 hours is ideal. This is where I am currently. I set the machine up outside and away from the house and anything flammable and let it run all night. Local temps were in the low 40s which shouldn't matter but the cold made me a little more comfortable.
The resulting mix is is a HIGHLY COMBUSTIBLE fine powder, about the same consistency/texture as talcum powder. PLEASE WEAR GLOVES AND BREATHING PROTECTION.
I measured out my raw ingredients inside but the rest of the process will be completed outdoors. Still, breathing protection and gloves and eye protection.
Let's make putty. Traditionally water is used for this step, but most will recommend isopropyl alcohol. In a disposable container mix the powder by adding small amounts of fluid until the mixture is about the consistency of modeling clay or play dough.
Commercial powder is then put through a process called corning which will result in a denser mixture. This process requires about 12 tons of pressure and I do not have the stones to attempt compressing this stuff at home.
Most of the math says uncompressed powder requires about 12% higher charge to achieve the same muzzle velocity. I can live with that, and come on, folks were making powder hundreds of years ago and it worked just fine. I'm willing to bet that if revolutionary farmers could turn out a usable product then so can I.
Once you have putty, it needs granulated. Anyone familiar with gunpowder of any flavor should be aware of the different shapes and sizes of powder granules. I'll be aiming for something between ff and fff. An eyeball guess and zero experience saw the purchase of a kitchen strainer that I think will do nicely. The powder putty is then grated through the strainer and onto a cookie sheet lined with aluminum foil and set in the sun to dry thoroughly.
Once dry it should be ready for a test against some commercial stuff. A small amount in a safe area, and BE CAREFUL. It should burn almost instantly.
That's what I've got and hopefully this weekend I can granulate my powder and test the burn rate. If it looks good, I'll move on to testing it in my rifle.
I'll post progress and pictures as I'm able.