Method for producing crystalline, zeolitic solid matter

• US 6,805,851 B1
• Filed: 02/20/2002
• Issued: 10/19/2004
• Est. Priority Date: 08/20/1999
• Status: Expired due to Term

• Current Assignee: BASF AG (BASF SE)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Müller, Ulrich, Hill, Friedrich, Rieber, Norbert
• Primary Examiner(s): SAMPLE, DAVID R
• Application Number:
  US10/049,907
• Time in Patent Office: 972 Days
• Field of Search: 423/705, 423/716, 423/717, 502/60, 502/242
• US Class Current: 423/705
• CPC Class Codes: B01J 20/18 Synthetic zeolitic molecular sieves
• CPC Class Codes: B01J 29/7049 containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
• CPC Class Codes: B01J 29/89 Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium B01J29/005 takes precedence
• CPC Class Codes: C01B 37/00 Compounds having molecular sieve properties but not having base-exchange properties
• CPC Class Codes: C01B 37/005 Silicates, i.e. so-called metallosilicalites or metallozeosilites
• CPC Class Codes: C01B 39/026 After-treatment
• CPC Class Codes: C01B 39/04 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
• CPC Class Codes: C01B 39/36 Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
• CPC Class Codes: C01G 23/04 Oxides; Hydroxides
• CPC Class Codes: Y02P 20/10 Process efficiency
• CPC Class Codes: Y10S 423/22 MFI, e.g. ZSM-5. silicalite, LZ-241

Abstract

Process for the preparation of a crystalline solid comprising at least one zeolitic material, in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed directly to a drying stage.

Claims

1. A process for the preparation of a crystalline solid comprising at least one zeolitic material, in which the solid is crystallized from at least one precursor compound and the reaction discharge of the crystallization is fed directly to a drying stage, drying being carried out in an atmosphere comprising less than 10% by volume of oxygen and at least one inert gas,

characterized in that said crystallization is carried out in the presence of at least one template compound, and

characterized in that, after contact with the atmosphere in the form of a carrier gas stream with the reaction discharge to be dried, condensable template compounds present in the stream are condensed out.

2. The process as claimed in claim 1, characterized in that said drying is spray-drying.

3. A process as claimed in claim 1, characterized in that template compounds which are included in the dried crystalline solid are separated from the solid by means of at least one wash process.

5. The process as claimed in claim 2, characterized in that template compounds which are included in the dried crystalline solid are separated from the solid by means of at least one wash process.

4. An integrated process for the preparation of a crystalline solid comprising at least one zeolitic material, in which

(i) the solid is continuously crystallized from at least one precursor compound in the presence of at least one template compound,

(ii) the reaction discharge from the crystallization is continuously spray-dried, no component of the reaction discharge of the crystallization being separated off before the drying,

(iii) the drying is carried out in an atmosphere comprising oxygen, preferably less than 10% by volume of oxygen, and at least one inert gas, this atmosphere being circulated as a carrier gas stream,

(iv) template compounds condensable from the carrier gas stream after contact of the stream with the reaction discharge to be dried are condensed out and are recycled to (i),

(v) the spray-dried crystalline solid from (ii) is subjected to a continuous wash process in which template compounds which are included in the crystalline solid are separated off and recycled to (i), and

(vi) the crystalline solid obtained from (v) is calcined, the energy released as a result of burning of the remaining amount of template compounds being fed back to (i).