In this work sodium bisulfate was used as a blocking agent to block polymethylene polyphenylisocyanate (PAPI). The particle size distribution rate and the factors influencing the stability of the blocked isocyanate emulsion were studied by varying the stirring speed. Furthermore the blocked isocyanate was characterized using a variety of methods. In order to determine the best stirring speed for preparing blocked isocyanate, a laser particle size analyzer and thermo gravimetric analysis were used to the measure particle size distribution rate and the stability of the blocked isocyanate emulsion, respectively. Experimental results show that blocked rate was 96.77%, and that the blocked isocyanate emulsion dispersion was best, and had the greatest stability, at the stirring speed of 400 r/min. Different solvents were used to wash the blocked isocyanate emulsion and the freeze-dried product. Analysis by XPS, FTIR, DSC and TGA were used to characterize the blocked products, and the blocked isocyanate was also quantitative analyzed. Results from XPS, FTIR, DSC and TGA analytical methods were able to qualitatively analyze the various components of products. Combining these results with the quantitative analysis the blocked rate of instrument analysis was found to be 86.18%. This was lower than the value of 96.77% for the blocked rate measured by chemical analysis. This work could provide a reference for researchers to distinguish the components of blocked isocyanates and provide an instrument analysis method for measuring the blocked rate. (C) Koninklijke Brill NV, Leiden, 2012