The invention discloses a preparation method of 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane, and aims to solve the problems that in the prior art, used reactants are not environmentally friendly, theyield is low and the like. 4-methoxyphenol and triethylene glycol are used as raw materials, and the preparation method comprises the following steps: (1), stirring at 20 DEG C, adding 4-methoxyphenoland triethylene glycol into acetonitrile, adding dicyclohexylcarbodiimide, reacting for 24h at 85 DEG C, and evaporating out acetonitrile to obtain a turbid liquid 1; (2), adding dichloromethane intothe turbid liquid 1, filtering, washing for 3 times with 1M sodium hydroxide, washing twice with saturated sodium chloride, drying by anhydrous magnesium sulfate, and evaporating out dichloromethaneto obtain a yellow powdery solid 2; (3), adding ethyl ether into the yellow powdery solid 2, raising the temperature to 35 DEG C, filtering out insolubles, cooling to -15 DEG C, lowering the temperature for 4 hours, and filtering to obtain a white powdery solid, namely 1, 2-bis (2-(4-methoxyphenoxy)ethoxy)ethane. The method is mainly applied to preparation of 1, 2-bis(2-(4-methoxyphenoxy)ethoxy)ethane.