Tungsten hexacarbonyl is a coordination compound formed by transition metal tungsten and carbon monoxide ligands, which is widely used in organic synthesis. However, the existing technology has the disadvantages of harsh reaction conditions, complex operation, low synthesis efficiency and high production cost. Therefore, in order to solve the above shortcomings, some researchers proposed a new preparation method. The specific steps are as follows:
(1) Put tungsten oxide, carbon tetrachloride, non-polar organic solvent and independently packaged reducing agent in a sealed reaction kettle with agitator;
(2) Remove the air in the reaction system by repeatedly charging and discharging carbon monoxide into the reactor, and then heat the reactor to 200-250°C and keep it warm for 4-8 hours;
(3) After the reaction system cools down to 30-50°C, inject carbon monoxide to 5-20MPa and keep the pressure, then turn on the reactor stirring device, break the packaged reducing agent container, and the stirrer speed is 100-200 rpm , continuous reaction for 1-12 hours;
(4) After the reaction is completed, the reaction solution is taken out after the solution is cooled to room temperature, and the colorless crystal of tungsten hexacarbonyl is obtained by distillation and heating sublimation.
Notes on this preparation method:
1) The reducing agent described in step (1) is a mixture of active metal powder and carbonyl metal complex that can provide CO ligands at a ratio of 1:2; the active metal powder is aluminum powder, zinc powder or iron powder, Metal carbonyl complexes providing CO ligands are nickel tetracarbonyl or iron pentacarbonyl.
2) The mass percentages of tungsten oxide, carbon tetrachloride, reducing agent and non-polar organic solvent in step (1) are: 2-5%, 8-12%, 9-15%, 70-80%. The non-polar organic solvent is anhydrous ether or anhydrous acetone.
3) The purity of carbon monoxide used in the reaction system is greater than 92%.
The advantages of this production technology include simple process, safe production, low cost and high synthesis efficiency.
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