The invention belongs to the technical field of coalification and synthesis and separation of organic products, and particularly relates to a method for separating a 2, 4-
xylenol / 2, 5-
xylenol mixture and producing 2, 4-
xylenol as a byproduct. A 2, 4-xylenol / 2, 5-xylenol
raw material with high 2-ethyl-6-
cresol and o-
isopropyl phenol content and
methanol are subjected to a catalytic
methylation reaction, then rectification is performed to obtain a mixture of 2, 4, 6-xylenol, 2, 3, 6-tricresol, 2-ethyl-4, 6-xylenol and 2-
isopropyl-4, 6-xylenol, and then a catalytic ethyl and
isopropyl removal reaction is performed to obtain 2, 4-xylenol, 2, 4, 6-tricresol, 2, 3, 6-tricresol and 2-isopropyl-4, 6-xylenol. According to the method, a mixture of 2, 4-xylenol, 2, 4, 6-tricresol and 2, 3, 6-tricresol is obtained through rectification, and 2, 4-xylenol, 2, 4, 6-tricresol and 2, 3, 6-tricresol are obtained through rectification again, so that separation of 2, 4-xylenol / 2, 5-xylenol with high 2-ethyl-6-
cresol content and high o-isopropyl
phenol content in
tar phenol extraction is realized.