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- Nachgewiesen in: USPTO Patent Grants
- Sprachen: English
- Patent Number: 11155,467
- Publication Date: October 26, 2021
- Appl. No: 16/330592
- Application Filed: September 05, 2017
- Claim: 1. A process for producing a zeolitic material having an MWW framework structure comprising YO 2 and B 2 O 3 , wherein Y is Si, the process comprising: (i) mixing one or more sources for YO 2 , one or more sources for B 2 O 3 , one or more organotemplates, and seed crystals, to obtain a mixture; (ii) crystallizing the mixture to obtain a layered precursor of the MWW framework structure; and (iii) calcining the layered precursor to obtain the zeolitic material having the MWW framework structure, wherein: the one or more organotemplates have the formula (I): R 1 R 2 R 3 N (I) R 1 is cyclohexyl; R 2 and R 3 are independently from each other H; and the mixture and the layered precursor comprise 35 wt. % or less of H 2 O based on 100 wt. % of YO 2 contained in the mixture and the layered precursor, wherein the mixture prepared in (i) and crystallized in (ii) contains 5 wt. % or less of fluoride calculated as the element and based on 100 wt. % of YO 2 .
- Claim: 2. The process of claim 1 , wherein the mixture and the layered precursor comprise 3 wt. % or less of fluoride calculated as the element and based on 100 wt. % of YO 2 .
- Claim: 3. The process of claim 1 , wherein the mixture and the layered precursor comprise 5 wt. % or less of P and/or Al calculated as the respective element and based on 100 wt. % of YO 2 .
- Claim: 4. The process of claim 1 , wherein the layered is selected from the group consisting of B-MCM-22(P), B-ERB-1(P), B-ITQ-1(P), B-PSH-3(P), B-SSZ-25(P), and mixtures of two or more thereof.
- Claim: 5. The process of claim 1 , wherein the zeolitic material having the MWW framework structure is selected from the group consisting of B-MCM-22, B-ERB-1, B-ITQ-1, B-PSH-3, B-SSZ-25, and mixtures of two or more thereof.
- Claim: 6. The process of claim 1 , wherein apart from organotemplate optionally contained in the seed crystals, the mixture does not contain piperidine or hexamethyleneimine.
- Claim: 7. The process of claim 1 , wherein the crystallization is conducted under autogenous pressure.
- Claim: 8. The process of claim 1 , wherein, after the crystallizing and prior to the calcining, the process further comprises: (a) isolating the layered precursor, to obtain an isolated layered precursor; (b) optionally washing the isolated layered precursor, to obtain a washed layered precursor; (c) optionally drying the isolated layered precursor or the washed layered precursor, to obtain a dried layered precursor; (d) optionally subjecting the layered precursor, the isolated layered precursor, or the washed layered precursor, or the dried layered precursor to ion exchange, to obtain an ion exchanged layered precursor; and (e) optionally subjecting the isolated layered precursor, the washed layered precursor, the dried layered precursor, or the ion exchanged layered precursor, to isomorphous substitution.
- Claim: 9. The process of claim 8 , wherein the isomorphous substitution is performed such that boron in the framework structure of the isolated layered precursor, the washed layered precursor, the dried layered precursor, or the ion exchanged layered precursor, is isomorphously substituted against one or more trivalent and/or tetravalent elements.
- Claim: 10. The process of claim 1 , wherein the calcination is carried out at a temperature of from 300 to 900° C.
- Claim: 11. The process of claim 1 , further comprising, after the calcining: (iv) deboronating the zeolitic material having an MWW framework structure with a liquid solvent system, thereby obtaining a deboronated zeolitic material having an MWW framework structure.
- Claim: 12. The process of claim 11 , wherein the deboronation is carried out at a temperature of from 50 to 125° C.
- Claim: 13. A synthetic zeolitic material having an MWW framework structure obtained by the process of claim 1 .
- Claim: 14. A composition, comprising the synthetic zeolitic material of claim 13 , wherein the composition is selected from the group consisting of a molecular sieve, an adsorbent, a catalyst, a catalyst component, and a combination thereof.
- Patent References Cited: 4954325 September 1990 Rubin et al. ; 4992615 February 1991 Huss, Jr. et al. ; 5107047 April 1992 Del Rossi ; 5173281 December 1992 Chang et al. ; 5284643 February 1994 Morrison et al. ; 5382742 January 1995 Morrison et al. ; 2015/0298983 October 2015 Maurer et al. ; 2015/0368115 December 2015 Parvulescu et al. ; 2017/0225959 August 2017 Maurer et al. ; 104591203 May 2015 ; WO 2014/086300 June 2014 ; WO 2015/185633 December 2015 ; WO 2016/058541 April 2016 ; WO-2018046481 March 2018
- Other References: Xu etal,“A Novel Method of Preparation of Zeolite ZSM-5”, J. Chem. Soc., Chem. Comm. (1990) pp. 755-756 (Year: 1990). cited by examiner ; Deforth et al, “Dry Synthesis of B-MFI, MTN- and MTW- type materials” Microporous Materials 9 (1997) 287-290 (Year: 1997). cited by examiner ; International Search Report dated Nov. 30, 2017 in PCT/EP2017/072200 filed Sep. 5, 2017, 5 pages. cited by applicant ; International Preliminary Report on Patentability and Written Opinion of the International Searching Authority dated Mar. 21, 2019 in PCT/EP2017/072200 filed Sep. 5, 2017, 10 pages. cited by applicant ; Michael E. Leonowicz, et al., “MCM-22: A Molecular Sieve with Two Independent Multidimensional Channel Systems” Science, vol. 264, 1994, pp. 1910-1913 and cover page. cited by applicant ; Limin Ren, et al., “Solvent-Free Synthesis of Zeolites from Solid Raw Materials” Journal of the American Chemical Society, vol. 134, 2012, pp. 15173-15176. cited by applicant ; Yinying Jin, et al. “Solvent-Free Synthesis of Silicoaluminophosphate Zeolites” Angewandte Chemie International Edition, vol. 52, 2013, pp. 9172-9175. cited by applicant ; Russell E. Morris, et al. “Solventless Synthesis of Zeolites” Angewandte Chemie International Edition, vol. 52, 2013, pp. 2163-2165. cited by applicant ; Qinming Wu, et al. “Sustainable Synthesis of Zeolites without Addition of Both Organotemplates and Solvents” Journal of the American Chemical Society, vol. 136, 2014, pp. 4019-4025. cited by applicant ; P. Frontera, et al., “Transformation of MCM-22(P) into ITQ-2: The Role of Framework Aluminium” Microporous and Mesoporous Materials, vol. 106, 2007, pp. 107-114. cited by applicant
- Primary Examiner: Brunsman, David M
- Attorney, Agent or Firm: Faegre Drinker Biddle & Reath LLP
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