Abstract: The present invention relates to a process for production of chlorine dioxide by reacting in a reaction vessel an alkali metal chlorate, sulfuric acid and methanol as a reducing agent. A reaction medium is maintained at a temperature from about 50.degree. C. to about 100.degree. C. and is subjected to a subatmospheric pressure sufficient to effect evaporation of water whereby a mixture of chlorine dioxide and water vapor is withdrawn from an evaporation region in the reaction vessel and alkali metal sulfate is precipitated in a crystallization region in the reaction vessel. Raw methanol purified by separation and adsorption is used as reducing agent. The raw methanol is purified by dilution with water whereby an unpolar phase is separated and and the remaining methanol-water phase is contacted by an adsorbing agent. The adsorbing agents used can be zeolites, active carbon or polymer adsorbing agents.