Verified Syntheses of Zeolitic Materials
First Edition
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