Tracking Sub-Nano-Scale Structural Evolution in Zeolite Synthesis by High-Energy X-ray Total Scattering Measurement with Pair Distribution Function Analysis.

The crystallization mechanism of zeolites remains unclarified to date because of lack of effective techniques in characterizing the local structures of amorphous precursors under synthetic conditions. Herein, high-energy X-ray total scattering measurement with pair distribution function analysis is performed throughout the hydrothermal synthesis of SSZ-13 zeolite to investigate the amorphous-to-crystalline transformation at the sub-nano level in real time. Ordered four-membered rings (4Rs) are dominantly formed during the induction period, prior to the significant increase in the number of symmetric six- and eight-membered rings (6Rs and 8Rs) in the crystal growth stage.

Exploring Hydrothermal Synthesis of SAPO-18 under High Hydrostatic Pressure.

The effect of external hydrostatic pressure on the hydrothermal synthesis of the microporous silicoaluminophosphate SAPO-18 has been explored. The crystallization of the SAPO-18 phase is inhibited at 150 °C under high pressures (200 MPa) when using relatively diluted synthesis mixtures. On the contrary, the use of concentrated synthesis mixtures allowed SAPO-18 to be obtained in all the studied conditions.

Unique crystallization behavior in zeolite synthesis under external high pressures.

The function of pressure has long been overlooked in the hydrothermal synthesis of zeolites, which is typically carried out under an autogenous pressure (below 2 MPa). We herein report, the first of its kind, a detailed investigation on the hydrothermal synthesis of zeolites under external high pressures, where crystallization behaviors contradicting the common observations were generated.

Extremely Stable Zeolites Developed via Designed Liquid-Mediated Treatment.

Improving the stability of porous materials for practical applications is highly challenging. Aluminosilicate zeolites are utilized for adsorptive and catalytic applications, wherein they are sometimes exposed to high-temperature steaming conditions (∼1000 °C). As the degradation of high-silica zeolites originates from the defect sites in their frameworks, feasible defect-healing methods are highly demanded.

Continuous flow synthesis of ZSM-5 zeolite on the order of seconds.

The hydrothermal synthesis of zeolites carried out in batch reactors takes a time so long (typically, on the order of days) that the crystallization of zeolites has long been believed to be very slow in nature. We herein present a synthetic process for ZSM-5, an industrially important zeolite, on the order of seconds in a continuous flow reactor using pressurized hot water as a heating medium. Direct mixing of a well-tuned precursor (90 °C) with the pressurized water preheated to extremely high temperature (370 °C) in the millimeter-sized continuous flow reactor resulted in immediate heating to high temperatures (240-300 °C); consequently, the crystallization of ZSM-5 in a seed-free system proceeded to completion within tens of or even several seconds.

Effects of ATP, Mg2+ and a mixture of the two on the formation of large DNA aggregates induced by spermidine.

To investigate the effects of ATP, Mg2+, and a mixture of the two on the formation of large DNA aggregates induced by spermidine, we constructed novel phase diagrams of the spermidine/DNA/Tris-buffer system in the presence of these compounds. These diagrams reveal not only the difference in the inhibition of the aggregate formation between ATP and Mg2+ but also a type of buffering effect whereby the complex formation of ATP and Mg2+ diminishes their individual inhibitory actions. Furthermore, the equilibrium composition of ATP, spermidine, Mg2+, and their complexes in the liquid phase was estimated using the equilibrium constants for the complex formations and their mass balances.