This paper uses centrifugal spray drying process to prepare powder polycarboxylate superplasticizer. The best spray drying process: speed of centrifugal atomizer is 16000r/min, feed liquid temperature is 30°C, import / export air temperature of drying chamber is 200°C/80°C. It achieves a high concentration of polycarboxylate superplasticizer to prepare powder product. It solves the problem of sticky and low-performance of powder polycarboxylate superplasticizer during traditional preparation. Analyzing the structure of polycarboxylate superplasticizer before and after spray-drying by infrared spectroscopy, and verifying the conclusion through macroeconomic performance experiments.