The invention discloses a preparation method of 2,2'-bis(trifluoromethyl)-4,4'-biphenyl dicarboxylic acid chloride, which comprises the following steps: a. taking 2,2'-bis(trifluoromethyl) base)-4,4'-diaminobiphenyl as the starting material, firstly through the diazotization reaction, and then through the bromination reaction to obtain 2,2'-bis(trifluoromethyl)-4,4'-dibromide Biphenyl; b, 2,2'-bis(trifluoromethyl)-4,4'-dibromobiphenyl undergoes a Grignard reaction / substitution reaction followed by reaction with carbon dioxide to give 2,2'-bis(trifluoromethyl) base)-4,4'-biphenyldicarboxylic acid; c, 2,2'-bis(trifluoromethyl)-4,4'-biphenyldicarboxylic acid was chlorinated to obtain 2,2'-bis(trifluoromethyl) Fluoromethyl)-4,4'-biphenyl dicarboxylic acid chloride. The method of the invention has short synthesis route, low production cost, especially high reaction yield, no need of highly toxic substances, high safety, and is suitable for large-scale industrial production.