Making Phosphorus Pentachloride: A Powerful Chlorinating Agent (TCPO 2/5) 

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.

@@reinisaugustins8555 can be used to make nerve agent precursors, although thionyl chloride is more often employed for that

@@SuperAngelofglory What precursors specifically and for which nerve agents?

@@reinisaugustins8555 methylphosphonyl dichloride (precursor to sarin gas)

@@reinisaugustins8555 it is also involved in other steps in the synthesis of this dreadful gas

Oxalyl chloride is a spooky boy, I'll tell you what

Like a Lil spooky haunted house kinda feeling

Der discord link funktioniert nicht

@@reaction_lab danke! Jetzt hoffentlich schon

Ja hat funktioniert

This. Really impressive job.

Well it didn’t kill me so theres a reason to be happy 😂

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

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.

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 ?

@@anthonyzouras8017 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. 🤓

i flushed the apparatus with argon

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.

@@THYZOID 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 :/

@@moortin3783 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.

yes

You can actually get ONLY 100 GRAMS PER YEAR without special reporting and registrations!

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.

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

@@THYZOID 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.

@@reinisaugustins8555 I'm in uk, it wasn't a problem to get it

water is not nearly hot enough. you could use a tube furnace though.

@@THYZOID ooh ok that makes sense

I was thinking ,some way has to be a little easier than flaming it with a torch

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.

It’s only for small scales though.

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?

@@reinisaugustins8555 it is considered a precursor but making/owning it is not illegal. only selling it to anyone would be

@@THYZOID 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?

pocket reduction method

None of these are liquids but probably polonium iodide and lithium iodide would be formed

@@THYZOID Thank for you reply sir I need one more information polinium powder low radiation can you explain usage of pollinium

no

It’s called a reaction tube or also a burning tube

@@THYZOID Thanks. before I got your reply I ordered an air condenser. Would that work?

@@THYZOID before I got your reply I bought. myself an air condenser. Would that work?

@@ianrinehart3762 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.

@@THYZOID Yes I forgot in school they called it a combustion tube.

bought it on amazon 2 years ago

@@THYZOID in the form of match box strikers?

@@serbianfemboy 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.

@@THYZOID fml

​@@THYZOID 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.

Didn’t I calculate it at the end of the video?

​@@THYZOIDu didnt

already did that in my thionyl chloride vid

Maybe. I’ve still got about some phosphorus left though.

@@THYZOID yeah but I can't buy Phosphorus here, think of us lol

@@TheHuntermj 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

​@@THYZOID 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