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Desktop demonstration of the Fischer-Tropsch synthesisAdded:
In this video, I will show you how to build a desktop version of the Fischer-Tropsch synthesis and carry out the experiment.
The Fischer-Tropsch synthesis is a collection of chemical reactions that converts a mixture of carbon monoxide and hydrogen, known as syngas, into liquid hydrocarbons.
It was discovered in 1925 by the German chemist Franz Fischer and the German-Austrian chemist Hans Tropsch.
The whole project began with a custom design and construction of a temperature controller for the mini quartz tube furnace.
Here you can see most of the components of the quartz tube furnace.
The compression fittings for the quartz tube are made of PTFE.
The heating element is made of nichrome wire with a diameter of 1 mm.
The ceramic tube is used for insulation.
The screw terminal housings are also made of ceramic as they must be heat resistant.
The quartz tube has an outer diameter of 12 mm and an inner diameter of 8 mm.
The thermocouple is secured to the ceramic tube with stainless steel cable ties. This allows it to measure approximately the temperature on the inner surface of the quartz tube.
Finally, the furnace was insulated several layers of ceramic wool to make it easier to read the temperature on the OLED display and operate the rotary encoder. I 3D printed a bracket for the PCB.
The program I wrote for the temperature controller includes a PID algorithm.
This is used slowly to set the temperature at the start of the experiment since the reaction itself is strongly exothermic.
I used these laboratory gas generators to synthesize hydrogen and carbon monoxide. The chemical equations are as follows.
Next, a stand for the two gas generators was built using 2020 V-slot aluminum profiles and pipe clamps.
For the mounting blade, I repurposed another polypropylene kitchen cutting board. This time a yellow one measuring 600 by 400 by 20 mm.
Since I'm German, I over-engineered the stand [clears throat] for the cold trap a bit.
On the right-hand side, you can see the borosilicate glass tube which has been drawn out into a nozzle and fitted with copper wool to serve as a flashback arrestor. It is used to burn off excess gases since carbon monoxide is highly toxic and like hydrogen forms explosive mixtures with oxygen. I also printed a mounting ring for the vacuum flask which later will be used for the ice salt bath.
In the next building step, everything was mounted onto the base plate.
>> The three-way stopcock is needed to flush the apparatus with argon in order to remove all oxygen.
The dropping funnels are equipped with Bunsen valves. The Bunsen valve is essentially a one-way valve used to stop suck-back problems. It is simple and cheap to make and works very efficiently.
Next, I connected everything accordingly using silicone tubing.
>> And this is what the finished Fischer-Tropsch apparatus looks like.
In preparation for the experiment, the two drying tubes were filled with silica gel.
Now it was time to make the catalyst. It must always be freshly prepared. Its effectiveness starts to decrease after just a few hours.
First, 1 g of cobalt nitrate is dissolved in 25 ml of distilled water.
In the next step, about two teaspoons of silica gel with a mesh size of 140 to 70 are placed in a petri dish. The silica gel particles have a very large surface area and is typically used for column or flash chromatography.
Using a pipette, the cobalt nitrate solution is dripped onto the silica gel until it cannot longer absorb any more liquid.
The saturated silica gel is then transferred to a fireproof ceramic dish.
The material is then calcined using a burner. The following reaction takes place during this process.
Since nitrogen oxides are produced and cobalt 2-3 oxide is carcinogenic, it is essential to work under a fume hood or outdoors.
After a few minutes, we are left with silica gel whose best surface area is now covered with cobalt 2-3 oxide.
To secure the catalyst, ceramic wool was inserted into the quartz tube.
The catalyst was transferred into the quartz tube using a piece of silicone tube and a funnel.
>> A cooling bath was then prepared using crushed ice and calcium chloride. The mixture can reach a stable temperature as low as minus 50° C.
Now it was time to set up the gas generators. Don't worry if you have lost track. I will show you a diagram of the experiment in a minute. It should explain the entire setup.
Immediately before the experiment, the apparatus was eventually purged with argon.
>> A few minutes after the experiment had started, the temperature in the quartz tube furnace rose sharply and eventually reached nearly 1,000° C.
Notice how the pale blue flame slowly turns into a yellow flame.
That was also the moment when I knew it was working.
One of the most difficult challenges I faced was keeping the two gas generators running in sync so that they delivered roughly the same amount of gas. I therefore highly recommend using gas cylinders equipped with pressure regulators, needle valves, and flow meters instead.
In total, I conducted the experiment three times following all the steps described and cleaning the apparatus beforehand.
When I opened the cold trap the first time, a gasoline-like smell immediately hit my nose.
This entire yield was then transferred to a test tube, and it turned out that two clearly separated phases had formed.
The bottom layer consists mostly of water, one of the most reliable indicators of the reaction, even after volatile components have been evaporated.
And now, what we've all been waiting for, is the top layer, which had a total volume of 2 ml flammable.
Oh boy, sure it is. What a reward for the more than 200 hours I've spent working on this project.
Also, sure I don't know what it is.
Aside from determining the boiling point, I can perform a qualitative chemical detection of aromatic compounds using a Friedel-Crafts alkylation reaction.
Typically, aromatics react with anhydrous aluminum chloride as a catalyst and chloroform as a solvent to form colored triarylmethane dyes.
Another option would be the bromine water test for detecting multiple carbon bonds. I might make a follow-up video on this, since I need to order some chemicals for it.
Thanks for watching. Stay stay true.
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