Separation of neon isotopes by rectification over a packed column is examined. The separation coefficient of the isotope pair 20Ne–22Ne is close to unity due to their similar properties. Rectification columns with contact space ~ 20 m in height are required to obtain isotopic products of high purity. The separation was carried out in a compact column using several stages because of vertical limitations. The obtained fractions were collected in gas tanks, compressed, purified, and directed for further enrichment in the same column. The degree of 22Ne extraction was shown to increase if the concentration of it in the distillate was held to the minimum. Ne isotopes could be obtained in 99.99% purity in 5–8 consecutive separation stages depending on the operating regime. An industrial pilot plant was built. A method for estimating the column operating time to produce a given volume of isotopic product was proposed.