Knicklicht selber machen

Today's video was shot at the university where I also study as one of several hundred chemistry students. The video was created in collaboration with the HHU Düsseldorf. Every child finds twinkling lights fascinating. After a pleasant crack, they radiate in colorful colors and shine subtly as a party armband. Or act as luminous throwing ammunition. The plan for today has nothing to do with dimly shining. The twinkling light should be oversized and as bright as possible. To do this, we combine the normal components of a twinkling light with a high-performance luminous material, which is usually used in OLED displays. More on that later. The most important component is a relatively complex molecule that generates energy, which is later converted into light. To do this, I use TCPO today. I say yes, relatively complex. TCPO emits the said energy during the reaction with hydrogen peroxide. Hydrogen peroxide is thus the next necessary chemical. Third, it needs a luminous material that absorbs the generated energy and converts it into light. The luminous material determines brightness and, above all, the color of the twinkling light. The fourth substance is sodium acetate, which is a weak base that catalyzes the reaction. Finally, you need a liquid in which all the mentioned components dissolve. This liquid will be ethyl acetate. Ethyl acetate, sodium acetate and hydrogen peroxide are standard chemicals that I can buy from any dealer. You can also get sodium acetate organized, but TCPO, the most important component of the twinkling light, is either sold nowhere or costs just over 600 euros per 25 grams. The thing is quite clear, in order to create a strong twinkling light without being proud of the open arms of the insolvency, I have to make the TCPO myself. I got in the car and a short time later I was on the campus of Heinrich-Heine-Universität. In line with the topic, I visit Professor Markus Sümter's lab today, where I was allowed to write my bachelor's thesis in the middle of last year. In the lab, inorganic light materials are then researched for various applications, such as luminescence, thermometry and LEDs. But now to the point. Today we want to synthesize TCPO worth 1,000 euros, and four chemicals are necessary for this. About 500 milliliters of toluene, 27 milliliters of triethylamine, 39.5 grams of 2,4,6-trichlorophenol and 9.5 milliliters of oxalyl chloride. The chemicals are either toxic, carcinogenic or both. Therefore, caution is required. By the way, this kind of danger is not unusual in research or in general practitioners during chemistry studies, but I found it worth mentioning. The synthesis itself is relatively easy, but I will also explain as many details as possible so that you get a deeper insight into the work in the lab. First, 39.5 grams of 2,4,6-trichlorophenol is added to a 1,000 milliliter round bulb. The chemicals have a strong odor, so that my gloves smelled of this substance even because of the touch of the bottle's outer wall. In addition, some residue remained in my cup glass, which we will have to take care of in the next step. Next, it gets a little more complicated right away. The toluene is particularly pure and dry, i.e. water-free. Since the reaction is water-sensitive, this fact plays into my cards. In order to keep the purity, the bottle is not opened, but the toluene is squeezed out of the bottle with the help of argon gas. The cup glass with the remaining 2,4,6-trichlorophenol, which did not quite work in the first step, is now rinsed with toluene, so that all of the substance can be transferred to reaction pistons. Next, 27 milliliters of triethylamine are added. A short swing up, here you can see a so-called Schlenk line, a glass apparatus from which various gases can flow out and with which vacuum can also be drawn. This step also pays attention to more or less earthwork, in which the unopened bottle is opened in argon current and the content is drawn out with a syringe through a thin cannula. Yes, quite a lot of information in one sentence. Incidentally, the cannula is the needle of the syringe. NerdRage and MyRed have already made very good videos on the synthesis of TCPO and did not dry the chemicals beforehand. The yield was around 60%. Therefore, I am curious whether our special way of working with argon gas and very pure chemicals leads to a higher yield. So far, only 2,4,6-trichlorophenol and triethylamine have been dissolved in toluene. For the actual reaction, salychlorine is also necessary. Since the reaction causes heat and the toluene is flammable, an ice bath must be cooled. In another research circle on the neighboring gang is an ice machine. That's perfect. It would be worth a thought to create something small for my own laboratory. Very important here, do not put the shovel into the ice bath afterwards, as it will disappear there almost hopelessly under newly produced ice. With the ice it went back to the laboratory to cool the piston. After a certain cooling time, 9.5 ml oxalyl chloride is drawn up in argon current with a syringe and then filled into a drip funnel that is placed on the piston. In the synthesis regulations that I have previously researched, most of the oxalyl chloride is warned, as it is of course also bent in front of it. The oxalyl chloride is slowly dripped into the piston through a drip funnel. And here we also have the first reaction of this synthesis. Oxalyl chloride reacts with 2,4,6-trichlorophenol to T-CPO, pronounced bis-2,4,6-trichlorophenyl oxalate. As a by-product, HCl is created. This is again a suitable place to point out that T-CPO is the most important component in bent light and the whole video is actually in addition to producing exactly that. The synthesis is worthwhile, as it would swallow a lot of money when buying. The triethylamine is used to convert the by-product HCl to triethylamine hydrochloride. Triethylamine hydrochloride is a white solid, which also forms in the gas phase above the liquid. It is recognizable due to the white smoke that is in the piston. The reaction mixture is stirred for 3 hours. A beige deposit has formed in the piston. Next, the T-CPO must be separated from the solution. Normal filtering would take forever, so we vacuum it. So far, the filter cake consists of two different white powders. In addition to the T-CPO, there is also triethylamine hydrochloride in it. You get that quickly in the truest sense of the word. Triethylamine hydrochloride is soluble in methanol and not in T-CPO. Small problem, methanol was not available in this laboratory. Convenient that there are other neighbors. Kindly asked, you may get it for free. As announced, the triethylamine hydrochloride dissolves in methanol and is drawn into the pistons. T-CPO remains alone in the filter cake. The filter cake becomes less voluminous and discolors. Vacuuming and washing was taken very seriously. As a tribute to a high degree of purity, several hundred milliliters of methanol were added. The last step in the synthesis is the drying of the T-CPO. To do this, we use a cooling trap, for whose cooling a cryo-liquid is necessary. As a coolant, liquid nitrogen serves with a temperature of minus 196 degrees Celsius. The actual drying takes place by means of a vacuum pump, which creates a vacuum in the product vessel via a hose line. Through this vacuum, all residual liquid is pulled out of the T-CPO, so that it becomes dust-dry as a result. Of course, you could have put the whole thing in an oven, but this variant is much faster. After a few minutes, the drying is complete and I could finally weigh it. We have produced 37.428 grams. This corresponds to a yield of 83.38%. Based on the assumption that the product is pure, 83.38% is a pretty good yield. This definitely speaks for our way of working. Since the T-CPO is now also available, we can mix a light bulb or light bulb. To do this, I use the following quantities. 500 mg T-CPO, 250 mg sodium acetate and 10 mg ruban. Ruban is an intensely colorful, more precisely, orange solid. As a solvent or light bulb liquid, I need a little less than 25 ml of ethyl acetate. What can I say, ethyl acetate is the next substance we don't have on hand. A second visit to the neighboring laboratory and the matter is resolved. This is the practical thing at a university. Yes, it's me again, ethyl acetate this time. Do you happen to have that in your closet too? Yes, tomorrow. Neat, tomorrow. Yes, thank you. You're welcome. So it can start. With 2.5 ml of 30% hydrogen peroxide, the light bulb can be started. Sorry, but if that doesn't light up ... I don't know. I don't think it will light up. Boy. Before we get to the 500 ml bulb, a little info. On Saturday, June 3, 2023, the University Information Day takes place at our university, where you can come by and learn everything about our courses and life at or at a university. A few years ago, I also stood there after my graduation and asked myself what I actually wanted from my studies and what my life will look like during my studies. This is an info day right on the campus of the HHU, a convenient way to get clarity about these important things. Get a friend, a girlfriend or your parents and just drop by on June 3 between 10 and 3 p.m. More information can be found at www.hochschulinformationstag.de, which is also linked in the video description. The same mixing ratio is found in the 500 ml bulb as before in the smaller version. Friendly, all graduation studies were together with me as props in the laboratory. That really looks like a dead ass that I have here. The reaction mechanism is not even that simple and also not 100% clarified. The previous theory states that in a reaction with hydrogen peroxide, 1,2-dioxetanedione or also called dimerous CO2 is carried out. Due to the high ring tension, it leads to a homolytic break, so that two CO2 molecules are created on different reactions. One of the two CO2 molecules is in a highly energetic stimulated state. The system therefore has chemical energy. This energy is then transferred to the actual luminous substance, the ruban, so that it is stimulated again. Stimulated is always bad for molecules. Therefore, the ruban changes into an energetic basic state by emitting excess energy in the form of light. In the technical jargon it is called light-emitting. The glow during the energetic decay is clearly visible. In addition, the color can be varied by the used luminous substance. I'll show you that in a later video. Many thanks to Markus Suter that I was allowed to film everything in their rooms and very freely with the camera, which I wanted to film. A big thank you goes to the PhD student Lukas Träger, who carried out the complete synthesis of the TCPO and really invested a lot of time for this video. In this way, many greetings go out to my channel members, without their support, long videos will hardly be possible. Videos of this kind are very time-intensive, so I am very happy about the monetary support. If you want to see more videos, such as chemicals and laboratory-required unboxings and behind-the-scenes, you are welcome to take a look around the member area.