Thy Labs - 2022-03-19
This is video 2/5 on making TCPO (active ingredient in glow sticks) from scratch. Labcoatz channel: https://www.youtube.com/channel/UCcT_WBynr2K8nANsVrR8BYw?app=desktop Patreon: https://www.patreon.com/thyzoid Discord: https://discord.gg/UrjAt44HWH (Let me know if the discord link does not work) Instagram: https://www.instagram.com/thyzoyd/?hl=de 🐦 Twitter: https://twitter.com/thyzoid1?lang=de 📌Reddit: https://www.reddit.com/user/Feuerfrosch1
PCl5 is one of the most useful reagents in a lab. Plenty of things to do with it (and some can be done only using PCl5 as chlorinating agent - for instance if you want to make geminal dihalohydrocarbons from aldehydes or ketones)
It may be hard to obtain because it is listed in Schedule 3 of the Chemical Weapons Convention (wide peaceful uses, but has the potential to be used as a chemical weapon or its precursor), but I hasn't yet found any method of chemical weapon preparation that uses PCl5.
@Reinis Augustins can be used to make nerve agent precursors, although thionyl chloride is more often employed for that
@Costi What precursors specifically and for which nerve agents?
@Reinis Augustins methylphosphonyl dichloride (precursor to sarin gas)
@Reinis Augustins it is also involved in other steps in the synthesis of this dreadful gas
PCl5 is one of those compounds that are "Common" in lab's but a lot of ammateur like me almost never see.
It's so satisfying when you upload synthesis like these and we get to see a bunch of PCl5 and how it's made. Not that it's synthesis is hard but many amateurs dont try it, or can get Red P, so it's very nice when we can see an example as these makes the synthesis less of a rarity.
I can wait for the oxalyl Chloride !!
Like a Lil spooky haunted house kinda feeling
This is amazing. First video on youtube about synthesis of PCl5. Congratulations and can't wait to see more good stuff.
Great job man! I have some PCl5 that I need to purify. You made it look very easy, lol.
Very impressive work! I can hardly wait the continue.
This. Really impressive job.
Wish I saw this sooner...great job! I wish this stuff was easier to get because it's so darn useful.
Very interesting video! I didn't think it was so simple to do... Although it's always stuff to be careful with. 👍
Thank you for the PCl5 synthesis!
Great stuff - Haven't enjoyed chem videos this much since watching extractions and ire.
Pretty slick. Liked the issues with the glassware and the rx. Been there, done that. Once in a great while, and if fortune is smiling, something unexpected might happen and open the door to a newer finding. Happened to me... that newer finding... a couple of times now.
Good job. PCl5 is a very useful reagent.
Remember, when working with HCl vapors, always have a gas mask near the workspace. It recently saved my life.
Maybe these are two suggestions for an improvement of the Chlorine-Generator: 1. replace the TCCA by NaClO-solution, which is much cheaper and you afterwards don't need get rid-off "depleted" Cyanuric Acid waste, but only of NaCl solution. 2. In order to dry the SO2, you should bubble it through conc. H2SO4 instead the use of anhydrous CaCl2. I suppose H2SO4 is more effective, due to the more intense contact with the SO2 in a liquid phase and you can use it as a bubble counter, too. Thumbs up!
TCCA is cheaper for me in germany and cleaning is actually easier than most people think. Regarding conc. H2SO4: I agree it would be MUCH better but >15% is banned in germany so I must use other drying agents
Is it true that you can reduce phosphorous pentachloride with silver powder to phosphorus trichloride? I read that in a source on advanced phosphorus chemistry, I can give you the name of that reference if you want.
What do you think about granulating the RedP a bit before adding it to the column to increase the available surface area?
I’d honestly just wrap the reaction tube in 400*C heating material and increase the flow of chlorine. Increasing the surface area by granulating should not help much because the fast forming layer of PCl5 quickly destroys that benefit.
Would be super great to have a video on P making from Ca3(PO4)2, SiO2 and C pyrolysis and distillation into water...then PCl5 would be more OTCish than from red P.
Calcium phosphate is one of the main ingredients of calcinated bones...SiO2 is basically sand...
problem is that makes WP not RP. does make me wonder if you use a glass container and keep the WP submerged in sunlight if that would substitute for the inert atmopshere ampoule ?
@Anthony Zouras
Just keep the WP in a cold vaccuum or under N2 / CO2 atmosphere and allow futher heating at a given T° in a closed/hermetical recipient...
WP (white P) will turn into RP (red P)... then if even further / longer (hotter?) heating ... polymerisation/multimerisation increases and PP (purple/violet) and BP (brown or black P)...
The higher the molecular weight and the larger the 3D bond structure... the higher the mp, boiling points and the lower the reactivity....
WP <==> RP
But probably the reversibility of the reaction is less easy with RP - PP/VP - BP
Done this one. It requires very high temperatures. Basically put the reaction mixture into some large ceramic flower pots as a simple electric arc furnace and retort. The lower one had a cable attached to a graphite block in the bottom, the middle was a mixture of fine sand, bone ash, a lye to make the melt more conductive and start glass formation, and a 60/40 mix of charcoal and graphite powder with steel wool bridging the top electrodes and the bottom graphite electrode for starting. Make sure the sand is the component in excess because the goal is to make a calcium silicate glass and reduce the phospate to CO gas and phosphorus. Too much bone ash and the phosphorus wont reduce, too much carbon and you will get calcium and silicon carbide and the reaction will stop once these bridge the electrodes. The whole works was buried in a sand pit and powered by an arc welder. The phosphorus vapor and CO gas was conveyed by a steel tube in the upper hole with pottery clay and partly air cooled and the moten phosphorus dropped under warm water in a enamal glazed steel pot. WP is no joke though, ebery now and then a bubble of CO would have enough phosphorus vapor to burn. Definitely an outside project to be sure. The reaction is done when the bubbling stops indicating that all the carbon is used up and the phosphorus is completely reduced. When the phosphorus is cool and solid it can be cut up with a pizza cutter under the water and transferred to a small jar like a pint or half quart mason jar under water. 🤓
Hi man, I really love your chanel. I'm a amateur chemist from Spain, and have been looking for a way to make some 2,4,6 triclorophenol for about a year. Could you explain me any process? Or give me any places to look for more info. I would love to see a video with the full synthesis. Thank u very much, adios <3
It is really easy. Literally just pass chlorine gas trough a SLIGHTLY warm phenol solution. overchlorination is hard to achieve but not impossible. Look up a few papers before doing this. you certainly don´t want to make the super poison dioxin. I will eventually make a video on this.
@Thy Labs ok, thank u very much for the awnser but, wich solvent should I use for the phenol? Also, using a TCCA/HCl Cl2 generator, how long aproximately will take the chlorination process? Any recomended beakers or material for the setup? Sorry for asking that much questions but papers related to this are pretty hard to find :/
@Moortin really. look into the papers. by no means is this a safe procedure. TCDD is one of the deadliest man made poisons. As a solvent CCl4 would be ideal although chloroform should also work. Reccomended beakers? You need a fully sealed apparatus with gas scrubbers on the outlet. Don´t even think about using beakers. You need a ground glass apparatus. READ THE PAPERS. If your reaction gets too hot you get TCDD. Maybe not too much but even a few milligrams are a great problem.
What do you think about the alternative method of bubbling the CL2 into a well stirred suspension of P in chloroform? It avoids the passivation issue.
It’s only for small scales though.
This is the question to the drafters of the Chemical Weapons Convention which I have seen in many chemistry publics: If pinacolyl alcohol is listed in the Schedule 2 (some peaceful uses) as a precursor of the nerve agent Soman, then why isopropyl alcohol is not included in Schedule 2 or Schedule 3 (wide peaceful uses) as a precursor of the nerve agent Sarin and why pinacolyl alcohol is in Schedule 2, not Schedule 3?
The scedule also depends on how useful the chemical is for the public sector. you cannot make isopropanol more restricted than absolutely neccessary while pinacolyl alcohol isn´t.
Someone on such public had writted that pinacolyl alcohol may be included in Schedule 2, because its relatively useless, but Wikipedia says that it is used as a solvent for paints and dyes.
Can you make a video about making and some experiments with PCl3? It may be also hard to get, because it is also listed in Schedule 3 of the Chemical Weapons Convention, because as Wikipedia says it is because it may be used to produce mustard gas and used as a viable chemical warfare pulmonary agent and because legislation in some countries, like Ukraine considers PCl3 as a drug precursor, with all the restrictions and possible prison terms for drug possession and being very hard to obtain.
I will eventually show how to make it as i need some for another project. It´s legal so idgaf
Is it considered as a drug precursor/dangerous poison in any EU country?
@Reinis Augustins it is considered a precursor but making/owning it is not illegal. only selling it to anyone would be
@Thy Labs So its fine that you have an ampoule with PCl3 in your apartment and is PCl5 considered as a drug precursor/dangerous poison in any EU country?
And why PCl3 is considered as a drug precursor? Maybe it can used to make other precursors?
Thy, I would like to react this pcl5 with oxalic acid, producing both oxalyl chloride (a milder and more selective acid chloride than thionyl chloride) and phosphoryl chloride.
The oxalyl chloride can then be reacted with pyridine to make the glow stick chemical. All in theory until I find out how the mechanism works. I expect temperature control will be important and of course acyl halides are corrosive
that´s the plan once i made even more PCl5 (watch my drying oxalic acid video for more info). it is reacted with trichlorophenol and not with pyridine though
@Thy Labs another possibly viable route to oxalyl chloride. React ethylene glycol with urea at 150c with a zinc oxide catalyst, hopefully no elevated is pressure needed for it to form ethylene carbonate. Then pass chlorine through that under a uv light for however many hours...
Mixing solid pcl5 and dry oxalic acid and waiting a day for it to become a liquid sounds a lot simpler but it's a challenge to get any useful amount of the PCl5. I've cheated and ordered 100g PCl5 since I spotted some on ebay but even that isn't really a lot to work with or for the price I paid
That is easier to say than to do it in the UK, because there oxalic acid is considered to be a dangerous poison,maybe because it causes kidney stones and you will need a licence which is hard-to-get to just buy it. However soluble oxalates, which are as toxic as oxalic acid, are not considered poisons and are freely available.
@Reinis Augustins I'm in uk, it wasn't a problem to get it
Wow, thanks. I loved this one. You going to use this to form acetyl chloride later on?
Made my setup look really amateurish. I used white phosphorus though and it reacted immediately with chlorine gas, but my setup was bad and I lost lots of product. I had just enough phosphorus tri/pentachloride needed for a few drops acetyl chloride.
Thank you for uploads and good work which I really appreciate...
Na I won’t use this for acetyl chloride but I might make some by bubbling Cl2 trough glacial acetic acid with red phosphorus in it.
Getting red P is very tough around here, sadly.
How did you get the chlorine to react without the oxygen reacting?
i flushed the apparatus with argon
I’m sorry for the mic crack at some point in this video. Need to get a good microphone soon but just spent a ton of money on a new stirrer hotplate.
I thought it was heat to get that hydroxyl off the phenol, but I guess not hahahaha. Like the summery at the end!!!
Hello sir please explain of polinium, iodine and lithium if these 3 had combined what will be the reaction of these liquids
None of these are liquids but probably polonium iodide and lithium iodide would be formed
@Thy Labs
Thank for you reply sir I need one more information polinium powder low radiation can you explain usage of pollinium
can anyone tell me the name of the glassware in which he places the phosphorus? I know it is not a regular condenser since it does not have an outer cooling jacket.
It’s called a reaction tube or also a burning tube
@Thy Labs Thanks. before I got your reply I ordered an air condenser. Would that work?
@Thy Labs before I got your reply I bought. myself an air condenser. Would that work?
@ian rinehart Probably yes but in general I recommend not to use equipment for unintended purposes because an air condenser (if poor quality) might crack releasing nasty fumes if you use it as a burning tube.
@Thy Labs Yes I forgot in school they called it a combustion tube.
The accent really sells it! I enjoy watching your videos over enyone elses just for it!
Wish I could find one of these burning tubes
How about some videos on how to make Phosphorus from Phosphates!
Maybe. I’ve still got about some phosphorus left though.
@Thy Labs yeah but I can't buy Phosphorus here, think of us lol
@Matt Hunter I’ve planned to build a tube furnace soon anyways as I’ve already got most of the parts then i might make a video on white P from phosphates
@Thy Labs have you figured out the process already or will that be an afterthought? Usually you do carbothermal reduction of phosphate but then you have P in gaseous form and need to condense, which leads to problems with clogging.
I couldn't really overcome that hurdle with small diameter pipes.
Already tried it on a microscale successfully
you sound very happy ^^ thats great to hear!
Well it didn’t kill me so theres a reason to be happy 😂
Nein, achtung!
I don’t agree with this experiment from my chemical chair.
1:08 the wing nut is rusty.
As a German you must have some standards.
No good no good.
I thumb you up no matter being your favourite commentator and fan 😁😍
Good luck making TCPO.
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Der discord link funktioniert nicht
@Reaction Lab danke! Jetzt hoffentlich schon
Ja hat funktioniert
What was your total yield?
Didn’t I calculate it at the end of the video?
@Thy Labsu didnt
where do you get your red phos?
bought it on amazon 2 years ago
@Thy Labs in the form of match box strikers?
@Serbian Femboy in the form of a bag full of an entire kg of this element. Back two years ago it was available up to 1000kg on amazon to order without any problem. It’s not available anymore as sales here are now restricted to 100g of red phosphorus per year.
@Thy Labs fml
@Thy Labs I think that it may be fine if you buy only 100 g per year and use it very rationally, e.g. few milligrams per experiment. I also think that obtaining PCl5 is much easier than red P, despite it being listed in the Schedule 3 of the Chemical Weapons Convention, which may create some legal issues over legality of buying it.
Nices Video
When you say TCCA are you referring to trichloroisocyanuric acid ?
yes
The question is were to get red phosphorus?
pocket reduction method
can be use phosforus pentaoxide?
no
cool
Ur German, right..hehe,gr8..!!
Thy Labs - 2022-05-21
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