Suspensions containing 15% of binapacryl with a particle size range of 1-8μm in 0.2% aqueous Ca-ligunosulfonate were prepared by repeated wet-sedimentation. The concentration of 4, 6-dinitro-2-sec-butylphenol (DNBP, an impurity in technical grade binapacryl) in the dispersion medium was kept below 130ppm because the particle growth of binapacryl was found not to be enhanced by DNBP at concentrations below 130ppm.
The change in the particle size distribution of binapacryl was monitored by Coulter counter TA-II during the preservation of the suspensions at constant temperatures. Binapacryl particle growth occurred above 45°C and temperature accelerated the particle growth. A positive correlation was found between the growth rate of binapacryl particles and the vapor pressure of binapacryl above 50°C. From the microscopic observation of binapacryl particles during the particle growth and the high level of agreement with the experimental particle size distribution and the calculated one based on the hypothesis that binapacryl particles bond at random two by two and grow, it is apparent that the particle growth of binapacryl is attributed to the bonding of particles. No polymorphic change during particle growth was detected by X-ray diffractometry.
From these results, it is concluded that the particle growth of binapacryl in aqueous suspensions is caused by the bonding of binapacryl particles owing to a sintering phenomenon occuring above 45°C.
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