Verified Syntheses of Zeolitic Materials

First Edition


Preface

 

There are over 100 known zeolite structure types without - including the "octahedral molecular sieves" and related Mesoporous materials. These materials occur naturally in some cases, but most are prepared synthetically. Many of these zeolite- like phases can be prepared with significantly different Si/AI ratios or with elements other than Si and Al. Porous aluminum phosphates show an even greater range of T-atom substitutions. Few are available commercially; researchers wanting to test a zeolite in a new application have very little selection unless they are willing to attempt the synthesis of the base zeolite in the laboratory. This book is intended to assist in this endeavor.The recipes in this book read on conventional zeolites and aluminum phosphates with tetrahedrally bound oxygen ions. Pillared clays and mesoporous structures are not included, nor are the tetrahedral/octahedral structures such as ETS-10. The products of these recipes are micron- sized particles, usually polycrystalline. Synthesis of large, single zeolite crystals has been accomplished in some cases, but it is beyond the scope of this book. Likewise the synthesis of nano crystals, also demonstrated in a few cases, is not treated here.The products described here are the direct result of crystallization or the result of crystallization plus washing and calcination. Post-crystallization modifications such as calcination of the hydrogen form of type Y (FAU) which produces ultra-stable Y are not considered, nor are post-treatments such as dealumination or insertion of Al3+ or other cations in tetrahedral positions.Even with these restrictions the synthesis literature of the past 50 years is voluminous. This can be intimidating to the researcher who is less than expert in the synthesis art. Replicating a synthesis from the literature is often unsuccessful even when done by experienced investigators using well-documented examples. To improve the probability of success by "one reasonably skilled in the art," the recipes in this book are presented in uniform format and in considerably more detail than is commonly found in the literature. Most are prepared by experts in their field and have been reviewed by the IZA Synthesis Commission. Further, the recipe has been laboratory tested and verified by two independent investigators in addition to the author's laboratory. Experience has shown that in many cases this verification process reveals ambiguities and criticalities which were not obvious before.Even with these precautions, success is not guaranteed. The editor wants to hear of the readers' successes and is willing to advise in case of failure.To assist the average researcher in getting started in the practice of zeolite synthesis, the Synthesis Commission has included a series of short articles on techniques of zeolite synthesis and characterization. These articles have been prepared by experts in their fields but are written on a technical level of the average graduate student. They are intended to show the possibilities and requirements of the method rather than detailed steps for its implementation. References to more basic articles are included for those willing to dig deeper.The recipes presented here are invited contributions in most cases; a few were volunteered by experts who were aware of the project. Invitations were based on recent publications which indicated a reasonable level of definition of the synthesis variables and a well-formed crystalline product.Improved synthesis methods or products with significantly different composition are to be expected in the future. It is anticipated that the recipe collection will be expanded in subsequent editions until all the zeolitic materials in general interest are covered. Readers who believe they can expand or improve on the collection are invited to submit their recipes to the editor of this volume.

October 1997
Harry Robson
Louisiana State University
Chemical Engineering Department
Baton Rouge, LA 70803, USA