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In this text I will describe synthesis of formaldehyde from methanol, reaction will be catalysed by metallic copper. However it is possible to use oxides of copper, since they will be reduced to metallic copper (spongy form). In this method, we will pass methanol/air fumes above heated copper wire, this will drive following reaction: CH3OH --O2/Cu--> CH2O + H2O Since reaction is exothermic, there will be created enough heat
to keep reaction going by its own, without external heating of
catalyst. As product we will obtain aqueous formaldehyde (<40%),
that can be easily converted to solid paraformaldehyde by drying in
excicator.
Assemble apparatus as showed on picture (note: original picture from referenced book can be found here):
Washer with H2SO4 seems to be optional.
Round bottomed 500 ml flask in water-bath have air inlet pipe that should go right to the bottom. Flask may have also an optional inlet with a dropping funnel with extra methanol (to make this a continuous process). Combustion pipe have a length of 30 cm and inner diameter of 1
cm, pipe must be made from heat-resistant glass. Here, I use a quartz
pipe with inner diameter of 0,8 cm, it was obtained from a microwave
oven :)
When apparatus is ready, place 200 ml of methanol into round bottomed flask in water-bath. Heat up copper coil with gas burner and attach a sucking pump to output of collecting flasks (see pic). When methanol/air fumes reaches hot copper coil, reaction will start. There will be evolved enough heat that will keep coil glowing, gas burner may then be removed. Adjust the air flow to keep about 2 cm of coil glowing. When reaction is complete (takes several hours), most of the product will be in first receiving flask. Contents of all receiving flasks may be mixed together.
Book author1 claim that usual yield in described procedure is 160 ml of 40% formaldehyde (that is with H2SO4 washer).
2. Some info was also taken from posts by Megalomania on roguesci forum, specifically info about prevention of autoignition of methanol fumes. |