Use of amphiphilic compounds to produce novel classes of crystalline oxide materials

• US 5,250,282 A
• Filed: 10/27/1992
• Issued: 10/05/1993
• Est. Priority Date: 01/25/1990
• Status: Expired due to Term

• Current Assignee: Mobil Oil Corporation (Exxon Mobil Corporation)
• Original Assignee: Mobil Oil Corporation (Exxon Mobil Corporation)
• Inventors: Roth, Wieslaw J., Vartuli, James C., Kresge, Charles T., Leonowicz, Michael E.
• Primary Examiner(s): BRENEMAN, ROBERT B
• Application Number:
  US07/967,962
• Time in Patent Office: 343 Days
• Field of Search: 423/700, 423/701, 423/DIG. 30, 423/704, 423/705, 423/718
• US Class Current: 423/705
• CPC Class Codes: B01D 53/8628 Processes characterised by a specific catalyst
• CPC Class Codes: B01J 20/041 Oxides or hydroxides
• CPC Class Codes: B01J 20/06 comprising oxides or hydroxides of metals not provided for in group B01J20/04
• CPC Class Codes: B01J 20/08 comprising aluminium oxide or hydroxide; comprising bauxite
• CPC Class Codes: B01J 20/103 comprising silica
• CPC Class Codes: B01J 20/12 Naturally occurring clays or bleaching earth
• CPC Class Codes: B01J 20/18 Synthetic zeolitic molecular sieves
• CPC Class Codes: B01J 20/3078 Thermal treatment, e.g. calcining or pyrolizing
• CPC Class Codes: B01J 2229/26 to stabilize the total catalyst structure
• CPC Class Codes: B01J 2229/32 Reaction with silicon compounds, e.g. TEOS, siliconfluoride
• CPC Class Codes: B01J 2229/34 Reaction with organic or organometallic compounds
• CPC Class Codes: B01J 2229/36 Steaming
• CPC Class Codes: B01J 2229/40 Special temperature treatment, i.e. other than just for template removal
• CPC Class Codes: B01J 2229/42 Addition of matrix or binder particles
• CPC Class Codes: B01J 29/0308 Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
• CPC Class Codes: B01J 29/041 Mesoporous materials having base exchange properties, e.g. Si/Al-MCM-41
• CPC Class Codes: C01B 37/00 Compounds having molecular sieve properties but not having base-exchange properties
• CPC Class Codes: C01B 37/02 Crystalline silica-polymorphs, e.g. silicalites dealuminated aluminosilicate zeolites
• CPC Class Codes: C01B 37/08 Silicoaluminophosphates [SAPO compounds] , e.g. CoSAPO
• CPC Class Codes: C01B 39/00 Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination treatment to modify the sorption properties, e.g. shaping using a binder, B01J20/10; treatment to modify the catalytic properties, e.g. combination of treatments to make the zeolites appropriate to their use as a catalyst, B01J29/04; treatment to improve the ion-exchange properties B01J39/14
• CPC Class Codes: C10G 11/05 : Crystalline alumino-silicates, e.g. molecular sieves
• CPC Class Codes: C10G 47/16 : Crystalline alumino-silicate carriers

Abstract

There is provided a process for using amphiphilic compounds in preparing new classes of crystalline oxide materials. These oxide materials may have uniformly large pores, e.g., having a size of about 40 Angstoms in diameter. This process involves combining sources of oxides with micellar solutions of organic amphiphilic compounds, such as quaternary ammonium cationic surfactants. Aggregates of these micelles in the form of liquid crystals are believed to function as templates for the formation of the present highly porous, crystalline materials.

Claims

1. A process for using an amphiphilic compound to prepare a highly porous crystalline oxide material exhibiting an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100 and a benzene adsorption capacity of greater than about 15 grams benzene per 100 grams anhydrous crystal at 50 torr and 25°

C., said process comprising the steps of;

(a) preparing a reaction mixture capable of forming a precursor to said crystalline oxide material, said reaction mixture comprising one or more sources of at least one oxide, a solvent or solvent mixture and an amphiphilic compound;

(b) maintaining said mixture under sufficient conditions of pH, temperature and time for formation of a crystalline oxide containing residual amphiphilic compound;

(c) recovering said crystalline oxide containing residual amphiphilic compound from step (b); and

(d) calcining said recovered material from step (c) under conditions sufficient to remove residual amphiphilic compound,

wherein said amphiphilic compound is a cetyltrimethylammonium compound, and wherein said reaction mixture of step (a) has the mole ratio

space="preserve" listing-type="equation">Solvent/(R'"'"'.sub.2 O+M.sub.2 O)

of greater than 92, where R'"'"' is said amphiphilic compound and M is alkali metal or alkali earth metal, and wherein the calcined material from step (d) has a hexagonal electron diffraction pattern and a pore size of at least 13 Angstroms.