The invention discloses a preparation method of 2, 2, 6, 6-tetramethyl-4-methoxypiperidine nitroxide free radicals, which comprises the following steps: in a reaction container equipped with a
nitrogen protection system, dissolving tetramethyl-4-hydroxypiperidine nitroxide free radicals in 2-methyltetrahydrofuran, and maintaining the
reaction system in an
inert environment by the
nitrogen protection system; adding a supported
sodium hydride catalyst into the
reaction system, wherein the
molar ratio of the supported
sodium hydride catalyst to the tetramethyl-4-hydroxypiperidine nitroxide free radical is (1.0-1.5): 1; the preparation method comprises the following steps: adding 2, 2, 6, 6-tetramethyl-4-methoxypiperidine into a reaction kettle, dropwise adding
methyl iodide, stirring for 4-6 hours, separating an organic phase, and crystallizing to obtain the 2, 2, 6, 6-tetramethyl-4-methoxypiperidine nitroxide free radical. According to the preparation method provided by the invention, the supported
sodium hydride catalyst is introduced, and the 2-methyltetrahydrofuran
solvent system is combined, so that the reaction efficiency and safety are remarkably improved. According to the preparation method provided by the invention, through
nitrogen protection and staged purging, low-temperature
crystallization and explosion-proof equipment control, the generation amount of
hydrogen is reduced, and the concentration of
solvent vapor is reduced.