4.7 Article

Crystallization of potassium-zeolites in organic-free media

Journal

MICROPOROUS AND MESOPOROUS MATERIALS
Volume 341, Issue -, Pages -

Publisher

ELSEVIER
DOI: 10.1016/j.micromeso.2022.112026

Keywords

Polymorphs; Integrowths; Nanoparticles; Interzeolite transformations

Funding

  1. Welch Foundation [E-1794]
  2. U.S. Department of Energy (DOE), Basic Energy Sciences (BES), Materials Sciences and Engineering (MSE) Division, Synthesis and Processing Sciences [DE-SC0021384]
  3. U.S. Department of Energy (DOE), Nuclear Energy University Program (DOE-NEUP) [18-15496]
  4. U.S. Department of Energy (DOE) [DE-SC0021384] Funding Source: U.S. Department of Energy (DOE)

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Research on zeolite synthesis without organic structure-directing agents has focused on controlling the polymorphism of K-zeolites. By studying the synthesis conditions of five K-zeolites, new synthesis strategies and methods have been developed to achieve nanosized crystals and reduce crystallization times.
A ubiquitous phenomenon in zeolite synthesis is the generation of polymorphs leading to either single or multiphase products. The use of organic structure-directing agents (OSDAs) often ensures a high degree of phase purity for a desired zeolite; however, OSDAs can be economically and environmentally prohibitive. The use of alkali metals as inorganic structure-directing agents (ISDAs) is a common alternative, although reductions in polymorph specificity and/or purity in organic-free media are significant limitations. Developing more controlled, facile synthesis strategies without the aid of OSDAs relies on understanding how zeolite growth conditions impact polymorph selection and alter the physicochemical properties of crystalline products. Relatively few studies of organic-free syntheses have systematically explored potassium growth media. In this study, we examine synthesis conditions that promote the formation of five K-zeolites: CHA, LTL, MER, EDI, and BPH frameworks. Time-resolved analyses reveal distinct trends in crystallization kinetics and interzeolite transformations for potassium compared to prior studies that have largely focused on Na-zeolites. We also highlight methods to achieve nanosized crystals and markedly reduce crystallization times for zeolites, such as chabazite, which are notoriously difficult to synthesize in organic-free media at reasonable timescales. Collectively, these findings identify routes to control K-zeolite polymorphism and provide general design strategies to tailor their crystallization.

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