Patent RU-2757001-C2 (RU)
Title: Method for producing titanium-containing zeolite
Inventor: PARVULESKU Andrej-Nikolae
IPC: B01J29/70
Filed: 2017-12-12
Granted: 2021-10-08
Abstract: FIELD: chemistry. 
     SUBSTANCE: invention relates to a method for producing titanium-containing zeolite material with MWW type of a frame structure, titanium-containing zeolite material obtained by this method, and to the use of the specified material as a catalyst, catalyst substrate or a catalyst precursor. The method for producing titanium-containing zeolite material includes: (i) obtaining boron-containing zeolite material with MWW type of a frame structure, where at least 99 wt.% of the zeolite frame structure consists of B, Si, O and H, and where an MWW template compound is used to obtain boron-containing zeolite material with MWW type of a frame structure; (ii) deboronation of boron-containing zeolite material obtained at stage (i), obtaining deboronized zeolite material, where at least 99 wt.% of the zeolite frame structure of deboronized zeolite material consists of B, Si, O and H, and where the zeolite frame structure of the deboronized zeolite material has empty sites of the frame structure; (iii) inclusion of titanium in deboronized zeolite material obtained at stage (ii), including (iii.1) preparation of an aqueous synthesis mixture containing deboronized zeolite material obtained at stage (ii), a titanium source, and the MWW template compound, where in the aqueous synthesis mixture obtained at stage (iii.1), the molar ratio of the MWW template compound and Si, calculated as SiO 2  and contained in deboronized zeolite material obtained at stage (ii), is at least 0.5:1; (iii.2) hydrothermal synthesis of titanium-containing zeolite material from the aqueous synthesis mixture obtained at stage (iii.1), obtaining a mother liquor containing water, the first part of the MWW template compound used at stage (iii.1), and titanium-containing zeolite material containing the second part of the MWW template compound used at stage (iii.1); (iv) separation of titanium-containing zeolite material containing the second part of the MWW template compound from the mother liquor, using a solid-liquid separation method, obtaining an aqueous mixture containing the first part of the MWW template compound, and additionally obtaining separated titanium-containing zeolite material containing the second part of the MWW template compound; (v) recycling the first part of the MWW template compound contained in the aqueous mixture obtained at stage (iv) to at least one of stages (i) and (iii.2). At the same time, at stage (iii.1), the titanium source is tetra-n-butylortotitanate, and the MWW template compound is piperidine. The mother liquor obtained at stage (iii.2) contains water, the first part of piperidine, titanium-containing zeolite material containing the second part of piperidine, and n-butanol, and the aqueous mixture obtained at stage (iv) contains the first part of piperidine and n-butanol. After stage (iv) and before stage (v), (x) separation of n-butanol from the aqueous mixture obtained at stage (iv) is carried out by the method specified in the claim.  
     EFFECT: technical result is providing a method for producing titanium-containing zeolite material with reduced losses of the template compound; producing titanium-containing zeolite material with higher crystallinity and specific surface area. 
     16 cl, 2 ex