Synthetic gel and glass of illitic composition, natural kaolinite, and
mixed-layer illite-smectite were used as starling materials for hydro
thermal synthesis of ammonium illite. Ammonium illite was prepared fro
m synthetic gel by hydrothermal treatment at 300 degrees C. The onset
of crystallization began within 3 h, and well-crystallized ammonium il
lite appeared at 24 h. Increasing reaction time (up to four weeks) led
to many illite layers per crystal. In the presence of equivalent prop
ortions of potassium and ammonium, the gel was transformed to illite w
ith equimolar contents of K and NH4. In contrast, synthesis using glas
s under the same conditions resulted in a mixture of mixed-layer ammon
ium illite-smectite with large expandability and discrete illite. Hydr
othermal treatments of the fine fractions of natural kaolinite and ill
ite-smectite produced ammonium illite from kaolinite but the illite-sm
ectite remained unchanged.