An method of quick analysis of azo dyes synthesis process relates to the quick analysis of a dye, comprising Step 1, the analysis and detection of the diazotization process in the synthesis of azo dyes and Step 2, the analysis and detection of the coupling process in the synthesis of azo dyes; S1, first establishing the analysis model for the para-ester diazonium salt, preparing in real time series of para-ester diazonium salt solution samples to be measured, immediately gathering spectroscopic data with a spectrograph, and measuring the content of para-ester diazonium salt under different time for para ester diazotization reaction; S2, first establishing the analysis model for the reaction product from coupling, preparing in real time series of solution samples to be measured for coupling reaction, immediately gathering spectroscopic data with a spectrograph, and measuring the content of azo dyes under different time for coupling reaction thus to achieve process control. The present invention is used for the real-time control of the synthetic process of dyes and it has the merits of easy operation, short examination cycle, high accuracy, low examination cost and is thus significant in the monitoring and control of dye products quality.