Synthetic crystalline zeolite produced from dehydrated aluminum silicate

• US 3,065,054 A
• Filed: 06/02/1959
• Issued: 11/20/1962
• Est. Priority Date: 06/02/1959
• Status: Expired due to Term

• Current Assignee: Frank J. Dzierzanowski, Walter L. Haden Jr
• Original Assignee: Frank J. Dzierzanowski, Walter L. Haden Jr
• Inventors: Haden, Walter L. Jr., Dzierzanowski, Frank J.
• Application Number:
  US03/817,472
• Time in Patent Office: 1,267 Days
• US Class Current: 423/701
• CPC Class Codes: C01B 33/2815 of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L)
• CPC Class Codes: C01B 33/2876 from a reacting mixture containing an amine or an organic cation, e.g. a quaternary onium cation-ammonium, phosphonium, stibonium
• CPC Class Codes: C01B 33/2892 containing an element or a compound occluded in the pores of the network, e.g. an oxide already present in the starting reaction mixture
• CPC Class Codes: C01B 39/30 Erionite or offretite type, e.g. zeolite T
• CPC Class Codes: Y10S 423/24 LTA, e.g. A, alpha, ZK-4, ZK-21, ZK-22

Claims

1. A METHOD FOR MAKING A SYNTHETIC CRYSTALLINE ZEOLITE IN THE FORM OF COHERENT MICROSPHERES OF SUBSTANTIALLY HOMOGENEOUS POLYCRYSTALLINE COMPOSITION WHICH COMPRISES FORMING AN APPARENTLY HOMOGENEOUS MIXTURE CONSISTING ESSENTIALLY OF FINELY DIVIDED DEHYDRATED KAOLIN CLAY AND AN AQUEOUS SOLUTION OF NAOH IN AN AMOUNT TO PROVIDE ABOUT 0.5 MOL OF NA2O PER MOL OF SIO2 IN SAID MIXTURE, SPRAY DRYING THE MIXTURE UNDER CONDITIONS SUCH THAT THE H2O/NA2O MOL RATIO IN THE RESULTANT MICROSPHERES IS WITHIN THE RANGE OF FROM ABOUT 4.5 TO ABOUT 11.5, REACTING THE CLAY WITH SAID NAOH WHILE MAINTAINING SAID MICROSPHERES OUT OF CONTACT WITH AN EXTERNAL AQUEOUS LIQUID PHASE AND CONTROLLING THE TEMPERATURE OF THE MICROSPHERES WITHIN THE RANGE OF ABOUT 70*F. TO ABOUT 200*F. UNTIL AN AMORPHOUS HOMOGENEUOS REACTION PRODUCT IS FORMED, AND AGING SAID AMORPHOUS REACTION PRODUCT AT A TEMPERATURE FROM ABOUT 70*F. TO ABOUT 325*F. UNDER AT LEAST AUTOGENOUS PRESSURE TO CONVERT SAID AMORPHOUS REACTION PRODUCT INTO COHERENT MICROSPHERES OF SUBSTANTIALLY HOMOGENEOUS CRYSTALLINE ZEOLITIC COMPOSITION.