US 12,478,959 B2
Continuous synthesis of a titanosilicate zeolitic material, said zeolitic material, molding prepared thereof, and their use
Hannah Schreyer, Ludwigshafen am Rhein (DE); Andrei-Nicolae Parvulescu, Ludwigshafen am Rhein (DE); Ulrich Mueller, Neustadt (DE); Dominic Riedel, Ludwigshafen am Rhein (DE); Jaroslaw Michael Mormul, Ludwigshafen am Rhein (DE); and Ralf Boehling, Ludwigshafen am Rhein (DE)
Assigned to BASF SE, Ludwigshafen am Rhein (DE)
Appl. No. 17/785,856
Filed by BASF SE, Ludwigshafen am Rhein (DE)
PCT Filed Dec. 18, 2020, PCT No. PCT/EP2020/087104
§ 371(c)(1), (2) Date Jun. 15, 2022,
PCT Pub. No. WO2021/123227, PCT Pub. Date Jun. 24, 2021.
Claims priority of application No. 19218167 (EP), filed on Dec. 19, 2019.
Prior Publication US 2023/0028936 A1, Jan. 26, 2023
Int. Cl. B01J 29/89 (2006.01); B01J 20/16 (2006.01); B01J 20/30 (2006.01); B01J 29/00 (2006.01); B01J 37/00 (2006.01); B01J 37/02 (2006.01); B01J 37/03 (2006.01); B01J 37/04 (2006.01); B01J 37/06 (2006.01); B01J 37/10 (2006.01)
CPC B01J 29/89 (2013.01) [B01J 20/16 (2013.01); B01J 20/3007 (2013.01); B01J 20/3014 (2013.01); B01J 20/3042 (2013.01); B01J 20/3057 (2013.01); B01J 20/3071 (2013.01); B01J 20/3078 (2013.01); B01J 20/3085 (2013.01); B01J 29/005 (2013.01); B01J 37/0018 (2013.01); B01J 37/0236 (2013.01); B01J 37/031 (2013.01); B01J 37/04 (2013.01); B01J 37/06 (2013.01); B01J 37/10 (2013.01); B01J 2235/00 (2024.01); B01J 2235/05 (2024.01); B01J 2235/15 (2024.01)] 12 Claims
 
1. A continuous process for preparing a zeolitic material having an MFI framework structure type comprising TS-1, comprising Si, Ti, and O, said process comprising
(i) preparing a mixture comprising one or more sources of Si, one or more sources of Ti, one or more tetraalkylammonium cation R1R2R3R4N+-containing compounds as structure directing agent, and water;
(ii) continuously feeding the mixture prepared in (i) into a continuous flow reactor; and
(iii) crystallizing the zeolitic material having an MFI framework structure type, wherein the mixture is heated to a temperature in the range of from 130 to 220° C., wherein R1, R2, R3, and R4 independently from one another stand for alkyl, and wherein the H2O:Si molar ratio of water to the one or more sources of Si calculated as SiO2 in the mixture prepared in (i) is in the range of from 3 to 11;
wherein the mixture constituting the feed crystallized in (iii) consists of a first liquid phase and a second liquid phase, wherein the first liquid phase is an aqueous phase comprising water, and the second liquid phase comprises a lubricating agent;
wherein the lubricating agent comprises one or more fluorinated compounds or a liquid paraffin.