Thoroughly enjoyed the video, ESPECIALLY the setup and cleanup tips. The reaction wouldn't be tough to find online, but making it safe and repeatable is golden. I was *just* about to start typing questions about cleanup at the end, when you started talking about cleanup! Great video.
hi doug, in the last two weeks or so i watched your uploads and have really enjoyed them! since i am not so much into chemistry i definitely don`t understand all the reactions going on but i have the feeling, of quite-getting-your-explainations-right, though this might be dunning-kruger-effect ;) anyway, keep on your great work! greetings from germany!
Such a well done video!! Can't wait for the next one. I teach high school chem so it's been years since I've been in a real lab. I live vicariously through your videos now hahah. Keep 'em coming!
Excellent demonstration and performance. This is indeed a dangerous chemical to work with and your whole setup can handle it, especially the fume hood.
Great! I love this kind of reaction (and I love reactions with sulfur in general). I would have added another distillation just for good measure (maybe fractional, although allowing it to reach the top of the coloumn would have required a ton of heat), but you know the boiling point of the stuff that came over and I guess that it was reasonably pure.
it would be great to see more videos from you, Unfortunately you haven't uploaded any videos for a long time, for example I would be very interested in the synthesis of thionyl chloride or phosphorus trichloride
May I submit a proposal for the preparation of Thionylchloride? I found a hint, that it should be possible to prepare SOCl2 in lab- scale out of Sulfurdichloride and Sulfurtrioxyde according SO3 + SCl2 -> SOCl2 + SO2. Thionylchloride is known to be a useful chlorinating agent and may replace the phosphorous-clorine compounds in many cases (PCl3, PCl5 and POCl3), which are very hard to obtain, due to their "dual-use" characteristics.
It's probably not necessary, but I also added in a bubbler in between the drying tube and the sulfur flask, I filled it with sulfuric acid just to dry the chlorine gas even more.
Brave one, working with such a great quantity of chlorine gas! Could you somehow make thionyl chloride to be used to introduce Cl in place of OH in syntheses? ;)
Very nice work! After the chlorination was finished you're still left with a chlorine generator setup filled with chlorine gas. How did you clean that one up without exposing yourself to chlorine gas? I used a two-neck RBF as the generator flask, and when things were finished, through the free neck I'd connect an aquarium air pump and blow the excess chlorine out into a beaker of aq. NaOH..
apart from alkalies, a lot of reducing agents come to mind for dealing with chlorine (FeCl2, sodium sulfite and thiosulfate, even carbonate and bicarbonate)
Ever thought about going a step further with this and making sulfur tetrachloride? It only exists at low temps (like dry ice acetone bath theps), but it does exist and seems like interesting stuff! It hydrolyses to thionyl chloride and I'd be really interested in seeing what it does to an anhydrous carboxylic acid. Maybe make an acid anhydride and thionyl chloride, which then reacts with another acid to make an acid chloride? Nothing like making two usefull things at the same time lol!
Hi Doug, I have been watching your videos with great interest. I watched nurdrage's making of potassium metal using the catalyzed magnesium reduction method. And he/she said that this method replacing the potassium hydroxide with sodium hydroxide it should be possible to make sodium metal if you got a longer chain of alcohol's. Would be fun to watch if you tried to make sodium metal using this method. Nurdrage never got it to work do.
Not a bit necessary to melt the sulfur beforehand. Cl2 reacts with the solid easily and the S2Cl2 can be distilled off easily. If you want the monochloride, you wILL HAve to distill from excess sulfor anyway.
convert S2Cl2 o SCl2, react the dichloride with SO2 and Cl2 and you get SOCl2, which is a very useful reagent (acyl chlorides, alkyl halides, alkyl sulfites and other interesting things can be obtained from it; unlike phosphorus chlorides, it is a much cheaper chlorinating agent, albeit more volatile and toxic)
Hey Doug, is there any chance that the “carbon” that you said was left over in the reaction flask was actually amorphous sulfur? I made a video exploring the physical properties on my channel and I think the “carbon” is just some plastic sulfur converting back to crystalline sulfur. Love your vids and can’t wait for the upload later today.
it must be carbon. all types of sulfur react with chlorine, so considering the excess of chlorine and high temperature in the flask, the remnant was definitely not sulfur
My research is based around phosphines and phosphorus compounds so I'm used to stenches, but I've heard the smell of this described as a mix of extreme BO and a decomposing corpse. Bleugh.
@@elnombre91 The smell is not easily described, but it is by far the worst I have encountered. I wouldn't say it necessarily smells like rotting flesh, although it is reminiscent of that. It smells more like what you would expect a chlorine compound and hydrogen sulfide to smell like. For the most part, however, you do not come into contact with it during this synthesis since it must not contact the air.
Another interesting video, thank you. Your glassware is super clean, I wonder how you do that. But never mind that. What was the powder, the something hypochlorite? I didn't think sodium hypochlorite could exist safely as a solid. My hearing is good, and you do speak a little fast :-) but I heard you say it was some percent something-or-other-hypochlorite. Is there an OTC source for that? Like TCCA or other pool chlorinator? Very nicely done though - the end product had a nice color.
no mercury chemistry! Yes, its interesting, but if there is soluble or even organic mercury anywhere around me id escape asap its not a fucking joke to play with these kinds of things
What's some of the uses of sulfur monochloride? And how do you avoid breathing in chlorine gas when you disassemble the apparatus after it has had the generator running?
+WeekendScience There are quite a few uses. I will hopefully be demonstrating some in upcoming videos! When I disassemble the chlorine generator I use a spray bottle with aqueous ammonia to neutralize the remaining gas. The fan sucks out the NH4Cl smoke.
Hey guys, I have a question, since the reaction that this guy is doing involves Cl2 generation, how does he prevent his system from blowing up from pressure build up? He cant really use a breathing hole, or the Cl2 would leak out, which is a no no, and as far as I know, CaCl2 wouldnt absorb Cl2 or anything.
The Cl2 is getting used up so if the rate of Cl2 production is low enough it should all get taken up by the S without any excess getting past the reaction flask Also at 8:52 of the video you can see a line attached to the vacuum adaptor which likely leads to the back of the fund hood for any excess Cl2 to vent.
What you said about there being only 3 types of sulfur chloride is not true. Other sulfur chlorides can be made with a common chlorosulfane and a sulfane. For ex S7Cl2 is made from S2Cl2 and H2S3
Liquids like these, especially the ones that react readily with moisture and water, scare me because of the fumes getting in the eyes and nasal cavities. Wouldn't want sulfur condensing inside me...
Doug. For shame you are not wearing a lab coat !!! There is no excuse. Dude i would not have a said anything but you are important to your family and friends and followers. 'Nuff said. Your friend from central TX bill
Why bother with such palaver..? It's far more simple to just burn sulphur and bubble the SO2 through ice cold hydrogen peroxide solution (as strong as you can get) chemplayer has a good tutorial on b!tchute detailing the proceedure.
@@antejl7925 The yield is vastly different. The SO2/peroxide method gives a linear yield. Sulfur chlorides are a self creating catalyst the rate of production is exponential and the reaction proceeds at room temperature.
@@DougsLab You could dehydrate sodium bisulfate to sodium pyrosulfate, and then on heating it would yield sodium sulfate and sulfur trioxide gas. According to wikipedia you should then be able to get thionyl chloride by bubbling that through sulfur dichloride. What complications are you running into? Here's a preparation from a cookbook I have: Flask A of the apparatus in Fig. 166 is charged with pure 65% oleum, flask B with 100 g. of SC12 (see p. 370). Flasks is slowly heated in an H2SO4 bath, while B is cooled with an ice-water bath. The stoichiometric quantity of SO3 is thus gradually distilled onto the SCl2. The reaction proceeds with SO2 evolution (use a hood!). Partial solidification of the flask contents frequently occurs at the beginning. However, the contents should again be completely liquid when the addition is completed. If necessary, the flask is heated at the end for a short time on a water bath. Flask A is then disconnected, the ground joint at Q is stoppered, and the mixture is slowly distilled through a column (use a hood!). The mixture must be protected from contact with atmospheric moisture. The middle fraction is further purified by repeated careful fractionation, with S added to the distillation charge in order to convert all sulfur chlorides present to S2Cl2. The contents are distilled through an efficient column until a completely colorless product, coming over at 76-77°C, is obtained. The yield is about 80% of theoretical.
Doug! Speak a little more slowly, please. Yes, we know what you're doing, but it isn't necessary to speak as though you're an auctioneer! And stop mumbling a bit, too. Thank you, a fan.
