Making black powder at home
- Thread starter Ian
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Ian
Notorious member
I saved about 1/4 bucket of Zamak wheel weights and several chunks of anode rod, but I know the filled and rolled over .45 brass does the trick and it's easy to make. I raided the scrap bucket again this afternoon and cast another 120 or so, crimped them and added to what was already going and that got it almost to a constant cascade. I had ground up and thrown in the pucks and leftovers from the first batch of Cottonelle so I'm working about 13 ounces of meal right now and the extra media really helped. I checked the meal after a couple of hours and am getting that oily slick feeling between the fingertips. Then I checked it after four more hours and it's clumping at the back of the drum. I dumped it out, broke up the packed in meal, dumped the media back in, meal on top, and started it up again. I'll check it again in the morning and see if it did it again overnight, no point in running it all day if half or more of the meal is clumped up and not getting milled. I think there's too much moisture in this batch.
I lit off a little line of the meal and it's starting to whoosh better, so that confirms it was undermilled before with my soft-sided jar and not nearly enough media.
I lit off a little line of the meal and it's starting to whoosh better, so that confirms it was undermilled before with my soft-sided jar and not nearly enough media.
Ian
Notorious member
It clumped again this morning so I left it for after work. When I got home I poured out the media, scratched out the cake at the solid end of the pipe, put it all back in and ran it until after supper. I think it's pretty well milled at this point but we'll find out.
I can't remember if I mentioned this or not so I'll write it down anyway: I added a process to my process which is sifting the dampened, spoon mixed meal through a flour sifter to more evenly distribute the moisture and break up the little dry BBs that compose about 30% of the mix. It makes a big difference as far as pressing goes, no little dry speckles on the surface of the pucks. This is especially important when pressing to a density less than 1.9 g/cc where the water doesn't begin to squeeze out. When it begins to squeeze out you know the moisture distribution is even, but the meal only requires wetting until it quits making dust to make good pucks and good, hard grains (any more water is risking re-crystalizing the oxidizer), but at the lower, commercial density that amount of water isn't forced out and mechanically ensuring even distribution is in my opinion a must.
So I got a fresh stack of pucks all pressed to 1.78 g/cc and made of Cottonelle Comfort Care charcoal at a ratio of 77/13/10. I'll give the pucks a few days to dry and then grind/classify them and see how it performs THIS time. If it is improved, but not as much as I'd like, I'll put all the ground powder on a cookie sheet in the sun all day to get it as dry as possible, then straight back in the ball mill and see if I can get it to incorporate any better without caking up in the drum. If it STILL cakes, I may try a fresh batch with oven-dried oxidizer and not add the sulfur until the last few hours.
I can't remember if I mentioned this or not so I'll write it down anyway: I added a process to my process which is sifting the dampened, spoon mixed meal through a flour sifter to more evenly distribute the moisture and break up the little dry BBs that compose about 30% of the mix. It makes a big difference as far as pressing goes, no little dry speckles on the surface of the pucks. This is especially important when pressing to a density less than 1.9 g/cc where the water doesn't begin to squeeze out. When it begins to squeeze out you know the moisture distribution is even, but the meal only requires wetting until it quits making dust to make good pucks and good, hard grains (any more water is risking re-crystalizing the oxidizer), but at the lower, commercial density that amount of water isn't forced out and mechanically ensuring even distribution is in my opinion a must.
So I got a fresh stack of pucks all pressed to 1.78 g/cc and made of Cottonelle Comfort Care charcoal at a ratio of 77/13/10. I'll give the pucks a few days to dry and then grind/classify them and see how it performs THIS time. If it is improved, but not as much as I'd like, I'll put all the ground powder on a cookie sheet in the sun all day to get it as dry as possible, then straight back in the ball mill and see if I can get it to incorporate any better without caking up in the drum. If it STILL cakes, I may try a fresh batch with oven-dried oxidizer and not add the sulfur until the last few hours.
Ian
Notorious member
It's level (has to be or it drags the roller flanges on one side or the other) but the PVC tube might wobble on one end more than the other, funneling stuff to the one end. There's a wooden plug in the end that cakes and a concave rubber cap on the one that doesn't. The rubber works like a de-ice boot on a wing as the media bumps along it, keeping stuff from sticking much.
I just threw a new, one pound batch together after drying out the oxidizer and then the charcoal at 285F in the convection oven and drying out the drum with the residue and media in it with a heat gun. I also ran with scissors on the way back from the shed. No mishaps.
I ground several pucks from the last batch and did some open-air tests, it's much improved and making white smoke instead of brown now, not as impressive as I'd hoped but seems ok. I'll try to shoot some this weekend and see how it improves.
The reason for making a fresh batch from scratch right away was both to see if the dried ingredients clump and to see if the brown residue on the burn plate goes away when using the broken in (cleaner) media. Much of the brass was dirty and tarnished and had to have the sharp edges worn off and of course that all ended up in the first run of powder, not to be discounted as a performance reducer. The media and drum are pretty well broken in and stabilized now so we'll see how the next batch mills out and make adjustments as necessary. I really like being able to mill a pound at a time and like that the mill is now 150 feet away from my house. I'd never mill that much at a time in my garage, it's just way to big of a bomb. You really have to plan out handling this stuff at all times like the amount you're working with is going to go off at any second because sooner or later it probably will.
I just threw a new, one pound batch together after drying out the oxidizer and then the charcoal at 285F in the convection oven and drying out the drum with the residue and media in it with a heat gun. I also ran with scissors on the way back from the shed. No mishaps.
I ground several pucks from the last batch and did some open-air tests, it's much improved and making white smoke instead of brown now, not as impressive as I'd hoped but seems ok. I'll try to shoot some this weekend and see how it improves.
The reason for making a fresh batch from scratch right away was both to see if the dried ingredients clump and to see if the brown residue on the burn plate goes away when using the broken in (cleaner) media. Much of the brass was dirty and tarnished and had to have the sharp edges worn off and of course that all ended up in the first run of powder, not to be discounted as a performance reducer. The media and drum are pretty well broken in and stabilized now so we'll see how the next batch mills out and make adjustments as necessary. I really like being able to mill a pound at a time and like that the mill is now 150 feet away from my house. I'd never mill that much at a time in my garage, it's just way to big of a bomb. You really have to plan out handling this stuff at all times like the amount you're working with is going to go off at any second because sooner or later it probably will.
Ian
Notorious member
You're welcome.
Powder meal turned out great this morning, no clumping or caking up in the ends of the drum, smooth as silk. Drying the oxidizer and fuel separately before throwing it all in the mill with the powdered sulfur did the trick. I don't know how to dry sulfur without melting it except for a few hours in the sun, but it didn't seem to matter much even if it did contain some traces of moisture.
I'll puck some tonight and get it drying for the weekend.
fiver
Well-Known Member
the blue root stuff dries right out with heat under it.
it'll change color when the water is out.
the yellow stuff i'm sure doesn't, but a simple pan in the PC machine should do it.
melting it would surely dry it, but leave you a thin hard cake to break apart.
it'll change color when the water is out.
the yellow stuff i'm sure doesn't, but a simple pan in the PC machine should do it.
melting it would surely dry it, but leave you a thin hard cake to break apart.
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Ian
Notorious member
All pucked away. Got 15, 1.04 ounce "boom cookies" drying on a paper plate and a spoonful of dampened meal left over, will let it dry and throw it in with the next mill batch.
One thing I noticed with this batch is it was getting hard to press the last 1/16" to the puck die limiting ring. I had to lean into it this time whereas last batch one finger on the handle easily pulled it to the limiting ring. I don't know what that means other than more bulk.
One thing I noticed with this batch is it was getting hard to press the last 1/16" to the puck die limiting ring. I had to lean into it this time whereas last batch one finger on the handle easily pulled it to the limiting ring. I don't know what that means other than more bulk.
Ian
Notorious member
I processed and tested this last batch a couple of weeks ago but forgot to update the thread.
77/13/10 Cottonelle tp, pucks air dried for 2-3 days, ground, classified, sun dried, glazed for three hours (no graphite), dusted (there wasn't much, it sort of impregnates all the pores of the kernels during a vigourous glazing), and tested. Poured in a volume measure and carded carefully with no compaction I was getting 51 weighed grains to a 50 grain measure and 1789 fps average with 20.8 SD using my 44" Kibler SMR, 50 grains volume, .445 PRB with .018" cotton patch and spit lube. Fastest powder yet. Only problem is it burns really dry and I don't think it will be the best on a hot, dry day, but I'm very pleased with the glazed density and performance. Only a slight carbon ring, no big deal.
So, since then I've learned that creosote is the ingredient needed for greasy, soft fouling and have been back to looking at wood again. I want to try sycamore, cottonwood, and revisit black willow now that I have a better mill and have been watching retort temperatures a lot more closely.
But........Jake did it again, this week he released a video on powder he made with bamboo charcoal and that got me thinking about something else I wanted to try: carizzo cane.
Carrizo cane is a nuisance and quite abundant on the banks of our creeks and rivers, not to mention the southern border. It turns out that a lot of research has been done on its physical properties by funded groups interested in its properties as a biofuel. First, ash content is surprisingly low (about 4%) making it borderline excellent in that regard. It can be ground and washed in hot water to reduce the inorganics and their catalyzing effects even more if needed. It seems to have a low creosote content but very high oil content that takes more than 600⁰F to burn completely off. Overall, seems good so I went and got some dead and dry but not rotted cane stalks and pyrolized them tonight.
Smoke started blue, then turned light grey in the flammable range and stayed there for a good while, then just as that petered out and it changed odor and to a slightly brown color, the internal retort temperature took off on its own. I don't know what happened but when it topped 600 I shut off the burner and pulled down the oven to try and stop the reaction. It topped out at nearly 700⁰F and and was pouring out acrid smoke from the vent until finally it started cooling off. When the temperature crossed over 647⁰ the smoke abruptly stopped so I have a baseline of what the minimum volatiles remaining are.
I like the results, nice and stinky, creosoty charcoalthat is very, very light and looks like it will reduce very easily to a super-fine powder. One problem with the harder charcoal is getting them to grind down to the single-digit micron size necessary for the best gunpowder. Hopefully tomorrow I'll get some oxidizer dried and a batch of this cane charcoal gunpowder going in the ball mill.
77/13/10 Cottonelle tp, pucks air dried for 2-3 days, ground, classified, sun dried, glazed for three hours (no graphite), dusted (there wasn't much, it sort of impregnates all the pores of the kernels during a vigourous glazing), and tested. Poured in a volume measure and carded carefully with no compaction I was getting 51 weighed grains to a 50 grain measure and 1789 fps average with 20.8 SD using my 44" Kibler SMR, 50 grains volume, .445 PRB with .018" cotton patch and spit lube. Fastest powder yet. Only problem is it burns really dry and I don't think it will be the best on a hot, dry day, but I'm very pleased with the glazed density and performance. Only a slight carbon ring, no big deal.
So, since then I've learned that creosote is the ingredient needed for greasy, soft fouling and have been back to looking at wood again. I want to try sycamore, cottonwood, and revisit black willow now that I have a better mill and have been watching retort temperatures a lot more closely.
But........Jake did it again, this week he released a video on powder he made with bamboo charcoal and that got me thinking about something else I wanted to try: carizzo cane.
Carrizo cane is a nuisance and quite abundant on the banks of our creeks and rivers, not to mention the southern border. It turns out that a lot of research has been done on its physical properties by funded groups interested in its properties as a biofuel. First, ash content is surprisingly low (about 4%) making it borderline excellent in that regard. It can be ground and washed in hot water to reduce the inorganics and their catalyzing effects even more if needed. It seems to have a low creosote content but very high oil content that takes more than 600⁰F to burn completely off. Overall, seems good so I went and got some dead and dry but not rotted cane stalks and pyrolized them tonight.
Smoke started blue, then turned light grey in the flammable range and stayed there for a good while, then just as that petered out and it changed odor and to a slightly brown color, the internal retort temperature took off on its own. I don't know what happened but when it topped 600 I shut off the burner and pulled down the oven to try and stop the reaction. It topped out at nearly 700⁰F and and was pouring out acrid smoke from the vent until finally it started cooling off. When the temperature crossed over 647⁰ the smoke abruptly stopped so I have a baseline of what the minimum volatiles remaining are.
I like the results, nice and stinky, creosoty charcoalthat is very, very light and looks like it will reduce very easily to a super-fine powder. One problem with the harder charcoal is getting them to grind down to the single-digit micron size necessary for the best gunpowder. Hopefully tomorrow I'll get some oxidizer dried and a batch of this cane charcoal gunpowder going in the ball mill.
JWinAZ
Active Member
Very interesting to follow this. Thank you.
I had a wonderful science class in the 7th grade: Introductory Physical Science. The instructor was outstanding. One of the things we did was destructive distillation of the wood sticks from cotton swabs. We broke off the cotton and put the sticks in a test tube. Stoppered the tube with a stopper that had a small glass tube going through. We speculated what would happen when heated by a Bunsen burner until the smoke stopped. Compared the product with the sticks and discussed what had happened. Compared the results to what we thought would happen. This was done at each of the lab tables, not just by the teacher. This was only one of several experiments done that could never, ever, be done in a 7th grade class now.
I had a wonderful science class in the 7th grade: Introductory Physical Science. The instructor was outstanding. One of the things we did was destructive distillation of the wood sticks from cotton swabs. We broke off the cotton and put the sticks in a test tube. Stoppered the tube with a stopper that had a small glass tube going through. We speculated what would happen when heated by a Bunsen burner until the smoke stopped. Compared the product with the sticks and discussed what had happened. Compared the results to what we thought would happen. This was done at each of the lab tables, not just by the teacher. This was only one of several experiments done that could never, ever, be done in a 7th grade class now.
Ian
Notorious member
It's rich for sure, but you should have seen the crystallized stalactites of crispy black goo that condensed out when I did that batch of chinaberry. Chinaberry made pretty good powder, on par with black willow but I think every insect in the entire southern end of the county keeled over the afternoon I cooked the charcoal. That was some toxic stuff and I probably won't mess with it again.
So here's some details of my process now. First I cook the charcoal and let it stand overnight at least before messing with it (there is a risk of spontaneous combustion from absorbing moisture and oxygen from the air even after the fresh char is completely cooled off). Then I crunch the stuff up, weigh out a dose for the amount of powder I'm making, and throw that in the ball mill for a couple of hours along with the residue from the previous batch of meal. Meanwhile I weigh out my granulated potassium nitrate and dry it on two paper plates in my convection oven and then let it cool. Then I stop the mill and add all the ingredients together and fire it up again for at least a 12 hour run. I'm still trying to figure out if that is long enough but the data I have so far indicates no significant speed difference between powder milled for 12 hours and same powder milled for twice that long. After milling I sift the meal out of the media using a brass sifter for polishing media, looks like a gold pan with lots of holes in the bottom. The green meal dust is then put in a plastic coffee can, dampened with water, and tossed/mixed until it is pretty evenly distributed, then I run that through a stainless steel crank type flour sifter to break up the pills and really get the water evenly distributed. Then I weigh doses for the pressing die and weigh/press/weigh/press until all the meal is pucked. Let those dry naturally for a couple of days to a week at less than 50% RH, break them up with a brass hammer, and run them through the hand-crank grain mill. I classify into a screen stack with the first being 20 mesh, then 50 mesh, then a blanked-off unit that collects the dust. If I want 2F I start with a 16 mesh and add a 30 between the 20 and 50. If I want 4F I drop a 40 mesh between the 20 or 30 and the 50, than add a 110 mesh and then the blank to catch dust under that. Anything that doesn't pass the first screen gets reground and passed again until it's all gone. All dust (about 15-25% of the total weight depending on the charcoal used, ratios, and moisture content of the pucks) is recycled into the green meal can for the next batch, or if the next batch is going to be a different composition then it gets dumped into the scrap powder jar to be re-milled and pressed for musket powder or whatever. After classifying the powder I usually let it dry a bit in the sun or in front of a heat lamp on a cookie sheet because it almost always contains enough moisture to want to clump a little. You don't want it TOO dry, but definitely don't want it clumping. After drying the grains I put it in my glazing jar which is a 1-gallon plastic jar with s couple of wood paddles screwed to the inside and tumble it for about 3 hours. I used to dust the powder after drying but found that the dust helps the glazing by packing into the surface pores of the fractured kernels and smoothing them over, after glazing the powder produces almost no dust. I also found that 1.78 g/cc pucks ground to 3F go from 41 grains weight/50 volume to 51 weight/50 volume with no settling when glazed in a 6", two paddle drum at 71 RPM for 3 hours, which is a major epiphany for me now that I'm not pressing to nearly maximum theoretical density anymore and limiting it to the commercial sporting powder density specifications. At this point I sift out the fines again using only the smallest screen for the grade I'm making and it's finished, ready to store in an airtight container.
I'm sure I'll refine my methods and equipment more eventually, but for now I'm pretty happy with the processes. Some important things I've learned about making superior powder are having clean and appropriate carbon sources, controlling the retort temperature closely to retain the last group of volatiles to boil off, getting the moisture of the press meal evenly distributed, weighing meal and pressing each puck to an exact and uniform density, and glazing the powder for accurate volume/mass measurements to equal commercial powder (if that matters to you).
So here's some details of my process now. First I cook the charcoal and let it stand overnight at least before messing with it (there is a risk of spontaneous combustion from absorbing moisture and oxygen from the air even after the fresh char is completely cooled off). Then I crunch the stuff up, weigh out a dose for the amount of powder I'm making, and throw that in the ball mill for a couple of hours along with the residue from the previous batch of meal. Meanwhile I weigh out my granulated potassium nitrate and dry it on two paper plates in my convection oven and then let it cool. Then I stop the mill and add all the ingredients together and fire it up again for at least a 12 hour run. I'm still trying to figure out if that is long enough but the data I have so far indicates no significant speed difference between powder milled for 12 hours and same powder milled for twice that long. After milling I sift the meal out of the media using a brass sifter for polishing media, looks like a gold pan with lots of holes in the bottom. The green meal dust is then put in a plastic coffee can, dampened with water, and tossed/mixed until it is pretty evenly distributed, then I run that through a stainless steel crank type flour sifter to break up the pills and really get the water evenly distributed. Then I weigh doses for the pressing die and weigh/press/weigh/press until all the meal is pucked. Let those dry naturally for a couple of days to a week at less than 50% RH, break them up with a brass hammer, and run them through the hand-crank grain mill. I classify into a screen stack with the first being 20 mesh, then 50 mesh, then a blanked-off unit that collects the dust. If I want 2F I start with a 16 mesh and add a 30 between the 20 and 50. If I want 4F I drop a 40 mesh between the 20 or 30 and the 50, than add a 110 mesh and then the blank to catch dust under that. Anything that doesn't pass the first screen gets reground and passed again until it's all gone. All dust (about 15-25% of the total weight depending on the charcoal used, ratios, and moisture content of the pucks) is recycled into the green meal can for the next batch, or if the next batch is going to be a different composition then it gets dumped into the scrap powder jar to be re-milled and pressed for musket powder or whatever. After classifying the powder I usually let it dry a bit in the sun or in front of a heat lamp on a cookie sheet because it almost always contains enough moisture to want to clump a little. You don't want it TOO dry, but definitely don't want it clumping. After drying the grains I put it in my glazing jar which is a 1-gallon plastic jar with s couple of wood paddles screwed to the inside and tumble it for about 3 hours. I used to dust the powder after drying but found that the dust helps the glazing by packing into the surface pores of the fractured kernels and smoothing them over, after glazing the powder produces almost no dust. I also found that 1.78 g/cc pucks ground to 3F go from 41 grains weight/50 volume to 51 weight/50 volume with no settling when glazed in a 6", two paddle drum at 71 RPM for 3 hours, which is a major epiphany for me now that I'm not pressing to nearly maximum theoretical density anymore and limiting it to the commercial sporting powder density specifications. At this point I sift out the fines again using only the smallest screen for the grade I'm making and it's finished, ready to store in an airtight container.
I'm sure I'll refine my methods and equipment more eventually, but for now I'm pretty happy with the processes. Some important things I've learned about making superior powder are having clean and appropriate carbon sources, controlling the retort temperature closely to retain the last group of volatiles to boil off, getting the moisture of the press meal evenly distributed, weighing meal and pressing each puck to an exact and uniform density, and glazing the powder for accurate volume/mass measurements to equal commercial powder (if that matters to you).
Ian
Notorious member
I snuck out and stole a teaspoon full of green meal from the tumbler after two and a half hours and checked on the clumping thing in the ends, no clumping whatsoever no that I do the extra drying step with the oxidizer. Did some burn tests and am liking it so far but it may be a bit rich with this charcoal. For some reason I reverted back to 75/15/10 and I'm getting only black residue, no white. The residue is actually oily and leaves a faint oily film when wiped off of the tile I do my burn tests on. I'm liking it, maybe if it performs well in the gunbarrels I'll have something that will will make softer fouling on 100-degree days. I can always adjust the oxidizer percentage for cleaner burn if necessary and also control the retort temperature to remove more or less of the creosote in the river cane. I sure hope this cane makes good power because it looks quite versatile so far and is very easy to break down for the retort, not to mention extremely simple to harvest (no bark peeling, splitting, seasoning, etc.).