January Chem
Added 2025-01-05 12:25:11 +0000 UTCHi all! Back to work tomorrow… I’m sure many of you are feeling this… apologies for reminding you…
But lots of shed chem going on! Here’s the overview of the current projects:
Extractions&Ire:
- Er/Yb doped Y2O3 for demonstrating upconversion fluorescence. Starting from Y, Er and Yb metal, we’ll make the nitrate slats and then do a ‘solution combustion synthesis’ followed by a calcination. I’ve ordered a 980nm laser to demonstrated the IR to visible fluorescence, so hopefully that arrives before the end of the month to help this video.
- Making Yellow. I’ve decided to tackle my grudge head-on… we’ll be making a new yellow pigment from a recent paper, that is a ‘tantalum doped yttrium molybdate’. This is a very intriguing collection of obscure elements, and we are starting from samples of the metals. Also, it needs to be heated to 1400 C, which is hot. And for 6 hours. Which is long. So that’s a fun challenge!
- Perovskite nanocrystals video 2… this was meant to be the main focus of Jan, but getting the oleylamine was tricky. I’ve got someone who is sending me some but it’ll take some time, so we’ll get to that video sometime soon. I’ve got a new ceramic mill and media for the grinding, and I’m excited to (hopefully!) see some things glow!
- Large scale cubane- next video is the bromination. Need to make lots of bromine. Also dioxane.
Explosions&Fire
- In some excellent news, I’ve finally opened the XeF2 I bought years ago! I was thinking it might have decomposed after sitting around for 4 years or so… but it is completely fine! (pictured in the little Teflon vial in this post). So today I attempted a synthesis of Perbromate (BrO4-) which will be the focus of the next video. If you’ve never heard of perbromate before, you’re not alone…. It is very rare. Is it anything special?? No not really, but sometimes it is about the treacherous and toxic journey rather than the mildly oxidising destination.
That’s all, thanks for your support, quite a bit of equipment is getting bought to support these videos thanks to you… but not in a way that makes the videos easy or professional…. Just more stuff for me to use and abuse etc…
Tom
Comments
Next level amateur rocket science lol
Uhrig Antoine
2025-03-10 21:28:14 +0000 UTC1400 for several hours, sounds like you need an arc furnace Pretty easy to make one, if you have a power supply that can do it, or you could sacrifice the microwave (for its transformer) and rewind it for the high current supply you need. Ceramic fibre would not cut it for that temperature, you would have to use high alumina (aluminium oxide) refractory bricks, or refractory cement on the hot side. Assuming small scale, you could build it in a 2gal metal bucket with 100mm diameter chamber for your crucible. You will need a viewport to adjust the carbon electrodes, to strike, then maintain an arc, the rods burning away slowly. A simple light dimming switch can be used to vary the heat input if using a home brew transformer, or the current control on a welding machine (if you have one). Carbons are available from any welding shop, you want them on the chunky side 8mm or 10mm (they will know them as gouging carbons) the copper plated ones are easier to connect wires to, so get them if possible. If you need any help I’m an electrical and electronic engineer, with experience in incineration and waste to energy (advanced pyrolysis and gasification) so pretty decent if you’re wanting to heat shit up.
Richard Pruen
2025-02-12 22:07:32 +0000 UTCPerbromate? I wonder if you can make solid rocket fuel from it. Toxic as all hell, i imagine.
Paul Ste. Marie
2025-01-07 00:18:43 +0000 UTCActually, here is a US patent (https://patents.google.com/patent/EP1050527) describing the exact process of making oleylamine (or any other fatty amine) in high volume and purity from a fatty nitrile. They use a Raney catalyst of 90-96% Nickel, 3-9% Aluminum, and 0.5-3% Molybdenum (by weight) to obtain the optimal reaction rate and purity. The molybdenum can be added as ammonium molybdenate to the above Raney catalyst in slurry form. The amount of catalyst used is 0.05-1% by weight for a fatty nitrile, and it should be carried out at a hydrogen pressure of 0.05-50Mpa at a temperature of 60-160C. The synthesis pathway is to take your fatty acid (oleic acid), and react with liquid ammonia to make a fatty amide, which can be converted to a fatty nitrile by dehydrating it. You then react the amide with the Raney nickel and hydrogen to make the final fatty amine. Alternatively, you can go straight from the triglyceride (you'd make trioleoin) to the oleylnitrile in one step by using a vapor phase reaction with gaseous ammonia at 400C using a metal catalyst such as iron oxide. (https://pubmed.ncbi.nlm.nih.gov/31457425/)
Morthra
2025-01-06 12:25:45 +0000 UTCHappy new year bud. Good luck out there
Tim Johnson
2025-01-05 17:19:22 +0000 UTCRe: the oleylamine you could conceivably make it yourself from olive oil (which is about 55% oleic acid) if you hydrolyze the triglycerides into free fatty acids and separate it from the glycerol. My lab actually has a protocol for base hydrolysis of fatty acids if you need it. This paper (https://www.researchgate.net/publication/325716138_Isolation_and_Ultra-Purification_of_Oleic_Acid_Extracted_from_Olive_Oil_Using_Urea_Crystallization) used urea crystallization to isolate the oleic acid specifically from olive oil. You could then make the oleylamine by hydrogenation in excess of ammonia using Raney nickel or copper chromite (not sure if you have any of these on hand). Raney nickel is prepared by dissolving nickel in molten aluminum (1:1 by weight) and then ground up and activated with concentrated (~5M sodium hydroxide) at 70-100C could even be content for the E&F channel as it's pyrophoric if dried. This paper (https://pubs.acs.org/doi/pdf/10.1021/ja01212a023) discusses its preparation. I dunno feels like the synthesis of oleylamine would be more in line with shed chemistry (as you could do it with almost everything purchased from the hardware store) but safety is a potential risk if you end up making Raney nickel (although if stored under degassed water it's very stable) and you'd have a hydrogen cylinder to worry about as well.
Morthra
2025-01-05 12:42:21 +0000 UTC
