A co-production process for 4-cumylphenol and 2

4-dicumylphenol was developed.The effect of raw material ratios，amount of catalysts，reaction temperature and dosage of re-crystallization solvents on alkylation of phenol and α-methyl-styrene were studied.Approximate 100% phenol conversion，and above 90% yield of 4-cumylphenol and 2

4-dicumylphenol were obtained.The purity of 2

4-dicumylphenol was better than 99% when a two-step re-crystallization with different solvents was employed.The emission of wastewater phenol-containing and other organic pollutants can be completely avoided when a new in-situ neutralization method was utilized for removal of catalysts.The problems of the present production technologies of 4-cumylphenol and 2

4-dicumylphenol，including difficulties in separation and purification，low yields and environmental pollution，could be solved.