Synthesis of crystalline porous solids in ammonia

• US 5,589,153 A
• Filed: 06/02/1995
• Issued: 12/31/1996
• Est. Priority Date: 11/03/1994
• Status: Expired due to Fees

• Current Assignee: The Dow Chemical Company (Dow, Inc.)
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Howard, Kevin E., Millar, Dean M., Garces, Juan M.
• Primary Examiner(s): Bell, Mark L.
• Assistant Examiner(s): NOT, DEFINED
• Application Number:
  US08/460,166
• Time in Patent Office: 578 Days
• Field of Search: 423/700, 423/701, 423/702, 423/703, 423/704, 423/705, 423/718, 423/713, 423/714, 423/715, 423/335, 502/60, 502/62, 502/77
• US Class Current: 423/705
• CPC Class Codes: C01B 37/02 Crystalline silica-polymorphs, e.g. silicalites dealuminated aluminosilicate zeolites
• CPC Class Codes: C01B 39/48 using at least one organic template directing agent
• CPC Class Codes: Y10S 423/27 Beta, e.g. NU-2

Abstract

A process of preparing a crystalline porous solid selected from silicas and metallosilicates, such as, aluminosilicate zeolites or clathrasils. The process involves preparing a reaction mixture containing ammonia; water in a controlled concentration; a (hydrocarbyl)ammonium polysilicate hydrate salt; a mineralizer, such as ammonium fluoride; optionally, a source of a metal oxide, such as aluminum nitride; and optionally, a source of a charge-balancing cation or a structure directing agent; and maintaining the mixture at a temperature and for a time so as to produce the crystalline porous solid. A novel silica which is isostructural with zeolite P1 is prepared. Also prepared are a novel silica which is isostructural with zeolite beta and a novel TMA sodalite having a silica/alumina molar ratio between 12 and about 20.

Claims

1. A crystalline microporous silica having an composition represented by

View Dependent Claims (2)

2. The composition of claim 1 prepared by a process comprising preparing a first nutrient mixture containing:

(a) tetramethylammonium polysilicate hydrate having the composition C₃₂ H₉₆ N₈ Si₈ O₂₀.nH₂ O and zeolite HY in amounts sufficient to prepare the composition,

and preparing a second nutrient mixture containing;

(b) aluminum nitride and ammonium fluoride in amounts sufficient to prepare the composition,

and thereafter adding the second nutrient mixture to the first nutrient mixture to form a reaction mixture, and thereafter combining the reaction mixture with anhydrous ammonia such that the molar ratio of ammonia to water is greater than about 5 and less than about 26, the water optionally being derived from the water of hydration of the polysilicate hydrate, and then maintaining the resulting mixture at a temperature ranging between about 100°

C. and about 180°

C. for a time sufficient to produce the composition.