ABSTRACT
A new applicator system for microwave heating of aqueous solutions for the hydrothermal synthesis of zeolite crystals has been developed and experimentally characterized. It is based on a short-ended coaxial waveguide with the solution being inserted as a lossy dielectric. The electrical and thermal design of the autoclave has been optimized by numerical simulations of the E-field and of the temperature distribution respectively. Different reference temperature profiles--a homogeneous and a gradient one--could be established within the zeolite solution and were held constant over time. From temperature measurements at various positions in the solution the two reference profiles could be verified. Temperature differences of less than 15 degrees C have been measured within the homogeneous autoclave whereas differences up to 55 degrees C have been found in the gradient autoclave. In the first synthesis experiments using this applicator zeolite crystals of the zeolite A and VPI-5-type could be successfully crystallized.
Subject(s)
Microwaves , Zeolites , Chemical Phenomena , Chemistry, Physical , Crystallization , Electrochemistry , Temperature , Zeolites/chemistryABSTRACT
Variations of the phase and amplitude of a transmitted ultrasonic wave package were monitored in real time during the synthesis of zeolite A and zeolite X. For both materials, characteristic changes of the measured attenuation and the sound velocity of ultrasonic waves traveling in the reaction fluid were observed, correlating with the processes of gel formation and zeolite crystallization, respectively. Aging effects of the reaction fluids are demonstrated. The observation of the onset of the zeolite crystallization was verified with ex-situ X-ray diffraction (XRD) measurements.
