Production of a zeolite-containing solid

Abstract

In a process for concentrating an at least partially crystalline solid containing at least one zeolite in a mixture comprising at least one auxiliary, for example a template compound, and said solid, the mixture is ultrafiltrated in a step (II) to divide the mixture into a retentate and a permeate, the solids content in the retentate being higher than that in the mixture and the solids content in the permeate being lower than that in the mixture. This procedure allows auxiliaries, in particular template compounds, present in the permeate to be recycled into a crystallizing step (I) upstream of step (II).

1 - 23 . (canceled)  
   
   
       24 . A solid containing at least one zeolite that is prepared by an integrated process, comprising: 
 (I) at least partly crystallizing solid particles containing at least one zeolite from a synthesis mixture to produce a mixture (I) comprising a mother liquor, said solid particles and at least one template compound;    (II) concentrating the solid present in mixture (I) by ultrafiltration to produce a retentate and a permeate, said permeate comprising the at least one template compound; and    (III) agglomerating or granulating or agglomerating and granulating the solid particles in the retentate from step (II), wherein the permeate obtained in step (II) or the at least one template compound present therein is at least partly recycled into step (I).    
   
   
       25 . The solid as claimed in  claim 24 , wherein, in step (II), the solid is concentrated by ultrafiltration through at least one membrane that contains separating layers having pore diameters ranging from 10 nm to 500 nm.  
   
   
       26 . The solid as claimed in  claim 25 , wherein the geometry of the at least one membrane is selected from the group consisting of flat, tubular, multichannel-element, capillary and wound geometries.  
   
   
       27 . The solid as claimed in  claim 24 , wherein the ultrafiltration of step (II) is conducted under a transmembrane pressure ranging from 0.5 to 20 bar.  
   
   
       28 . The solid as claimed in  claim 24 , wherein the solids content in the permeate does not exceed 1% by weight, based on the total weight of the permeate.  
   
   
       29 . The solid as claimed in  claim 24 , wherein the mother liquor does not contain more than 5% by weight of particles of more than 2 nm in size.  
   
   
       30 . The solid as claimed in  claim 24 , wherein at least one of the steps of agglomerating or granulating or at least two of these steps is/are selected from the group consisting of: 
 (i) spray drying,    (ii) fluidized-bed drying,    (iii) spray drying with integrated fluidized bed,    (iv) batchwise vacuum contact drying,    (v) belt drying,    (vi) fluidized-bed spray granulation drying,    (vii) continuous contact drying,    (viii) continuous paste mill drying,    (ix) microgranulation in a spray tower,    (x) agglomeration by addition of a binder, and    (xi) agglomeration by changing the pH.    
   
   
       31 . The solid as claimed in  claim 30 , wherein, in steps (i) to (xi), at least one additive is added prior to, during or after the respective drying/granulating/agglomerating steps.  
   
   
       32 . The solid as claimed in  claim 30 , wherein, in steps (i) to (xi), at least one additive is added prior to and after the respective drying/granulating/agglomerating steps.  
   
   
       33 . The solid as claimed in  claim 30 , wherein, in steps (i) to (xi), at least one additive is added prior to and during the respective drying/granulating/agglomerating steps.  
   
   
       34 . The solid as claimed in  claim 30 , wherein, in steps (i) to (xi), at least one additive is added during and after the respective drying/granulating/agglomerating steps.  
   
   
       35 . The solid as claimed in  claim 30 , wherein, in steps (i) to (xi), at least one additive is added prior to, during and after the respective drying/granulating/agglomerating steps.  
   
   
       36 . The solid as claimed in  claim 24 , wherein step (III) is followed by a shaping step (S), the at least one shaping step being selected from the group consisting of briquetting, pelletizing and sintering.  
   
   
       37 . The solid as claimed in  claim 24 , wherein at least one of steps (II) and (III) is followed by a calcining step (C) at temperatures in excess of 400° C.  
   
   
       38 . A method of epoxidation, comprising: 
 epoxidizing a compound having at least one C—C multiple bond in the presence of a catalyst of the zeolite containing solid as claimed in  claim 24 .    
   
   
       39 . A method of ammoximation, comprising: 
 reacting a compound having a C═O group with hydroxylamine in the presence of a catalyst of the zeolite containing solid as claimed in  claim 24 .    
   
   
       40 . A method of hydroxylation, comprising: 
 hydroxylating an organic compound having at least one aromatic functionality in the presence of a catalyst of the zeolite containing solid as obtained by the process as claimed in  claim 24 .    
   
   
       41 . A method of preparing hydroxylamine, comprising: 
 preparing hydroxylamine in the presence of a catalyst of the zeolite containing solid as claimed in  claim 24 .    
   
   
       42 . A method of epoxidation, comprising: 
 epoxidizing a compound having at least one C—C double bond in the presence of a catalyst of the shaped zeolite containing solid as claimed in  claim 36 .    
   
   
       43 . A method of ammoximation, comprising: 
 reacting a compound having a C═O group with hydroxylamine in the presence of a catalyst of the shaped zeolite containing solid as claimed in  claim 36 .    
   
   
       44 . A method of hydroxylation, comprising: 
 hydroxylating an organic compound having at least one aromatic functionality in the presence of a catalyst of the shaped zeolite containing solid as claimed in  claim 36 .    
   
   
       45 . A method of preparing hydroxylamine, comprising: 
 preparing hydroxylamine in the presence of a catalyst of the shaped zeolite containing solid as claimed in  claim 36.