IP Library › Granted Patent US 12,559,377
Granted Patent B2
US 12,559,377 · App. 18/004,161 · Granted Feb 24, 2026

Method of synthesizing a molecular sieve of MWW framework type

Inventors: Sina Sartipi (Brussels, BE); Marc H. Anthonis (Vlaams Brabant, BE); Aaron W. Peters (New Hope, PA); Mariame Akouche (Montgomery, FR); Scott J. Weigel (Allentown, PA)
Assignee: ExxonMobil Chemical Patents Inc.
C01B39/48B01J29/7038C01P2002/72C01P2002/86C01P2004/03C01P2006/11
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Quick Facts
Patent No.
US 12,559,377
App. No.
18/004,161
Granted
Feb 24, 2026
Kind
B2
Abstract

Disclosed is a method of synthesizing a molecular sieve of MWW framework type, and molecular sieves so synthesized. The method comprises preparing a synthesis mixture for forming a molecular sieve of MWW framework type, said synthesis mixture comprising water, a silicon source, a source of a trivalent element X, a potassium cation source, a structure directing agent R, and a source of another alkali metal cation M.

Claims (32)

1 . A method of synthesizing a molecular sieve of MWW framework type, the method comprising the steps of:

a) preparing a synthesis mixture capable of forming a molecular sieve of MWW framework type, said synthesis mixture comprising water, a silicon source, a source of a trivalent element X, a potassium cation source, a structure directing agent R, a source of another alkali metal cation M, optionally a source of a pentavalent element Z, optionally a source of hydroxide ions, and optionally seed crystals, the synthesis mixture having the following molar ratio composition:

Si:X 2 =8 to 18

H 2 O:Si=5 to 100

(M+K + ):Si=0.1 to 0.5

M:K + =1 to 10

R:Si=0.1 to 1;

b) heating said synthesis mixture under crystallization conditions for a time sufficient to form crystals of said molecular sieve of MWW framework type, said crystallization conditions including a temperature of from 100° C. to 220° C.; and

c) recovering said crystals of the molecular sieve of MWW framework type from the synthesis mixture.

2 . The method according to claim 1 , wherein the potassium source comprises potassium hydroxide, potassium aluminate, potassium silicate, a potassium salt such as KCl or KBr or potassium nitrate, or a combination thereof.

3 . The method according to claim 1 , wherein the synthesis mixture has a molar ratio (M+K + ):Si=0.15 to 0.25.

4 . The method according to claim 1 , wherein the synthesis mixture has a molar ratio K + :Si=0.01 to 0.1.

5 . The method according to claim 1 , wherein the structure directing agent R is selected from the group consisting of cyclopentylamine, cyclohexylamine, cycloheptylamine, hexamethyleneimine (HMI), heptamethyleneimine, homopiperazine, pentamethonium bromide or hydroxide, hexamethonium bromide or hydroxide, heptamethonium bromide or hydroxide, and combinations thereof.

6 . The method according to claim 1 , wherein X is selected from the group consisting of aluminum, boron, gallium, and mixtures thereof.

7 . The method according to claim 1 , wherein the source of a trivalent element X comprises Al 2 O 3 .

8 . The method according to claim 1 , wherein the silicon source comprises SiO 2 .

9 . The method according to claim 1 , wherein the synthesis mixture has a molar ratio M:K + =2 to 8, wherein M is sodium, lithium and/or rubidium.

10 . The method according to claim 1 , wherein the synthesis mixture comprises the alkali metal cation M source in a molar ratio of M:Si of from 0.1 to 0.25.

11 . The method according to claim 1 , wherein the synthesis mixture comprises a source of hydroxide ions, wherein the OH source is an alkali metal hydroxide.

12 . The method according to claim 1 , wherein the synthesis mixture comprises seed crystals in an amount of from 0.05 to 2 g seed /g (silicon source+source of trivalent element X).

13 . The method according to claim 1 , wherein the crystallization conditions in step (b) include a temperature of from 100° C. to 200° C.

14 . The method according to claim 1 , wherein the crystallization conditions in step (b) include heating for a period of from 1 to 800 hours.

15 . The method according to claim 1 , wherein the recovered crystals of molecular sieve of MWW framework type has a Si/X 2 molar ratio of from 8 to 16.

16 . A molecular sieve of MWW framework type obtainable by the method of claim 1 .

17 . The molecular sieve of claim 16 , having, in its as-synthesized and dried form, a density, as measured by a pycnometer, higher than 2.0 g/cm 3 .

18 . The method according to claim 1 , further comprising forming the molecular sieve and using the molecular sieve in a hydrocarbon chemical conversion process.

19 . The method according to claim 1 , wherein X is aluminum.

20 . The method according to claim 1 , wherein the synthesis mixture does not contain any pentavalent element Z.

21 . The method according to claim 1 , wherein the synthesis mixture comprises a source of hydroxide ions in a OH/Si molar ratio of from 0.1 to 0.5.

22 . The method according to claim 12 , wherein the seed crystals comprise a molecular sieve of framework type MWW.

23 . The molecular sieve of claim 16 , wherein the molecular sieve has, in its calcined and anhydrous form, a composition with a Si/X 2 molar ratio of from 8 to 18.

24 . The method of claim 18 , wherein the hydrocarbon chemical conversion process is aromatic alkylation.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 31, 2025
From: SARTIPI, SINA; ANTHONIS, MARC H.; PETERS, AARON W.; AKOUCHE, MARIAME; WEIGEL, SCOTT J.
To: EXXONMOBIL CHEMICAL PATENTS INC.
Reel/Frame 071896/0214 →
Priority Claims (1)
EP 20204269 · Oct 28, 2020 · regional
Continuity (2)
Provisional Application 63052526 · Jul 16, 2020
Related Publication 20230264965A1 · Aug 24, 2023
References Cited (32)
US 4439409A · Puppe et al. · 1984 [cited by applicant]
US 4826667A · Zones et al. · 1989 [cited by applicant]
US 4954325A · Rubin et al. · 1990 [cited by applicant]
US 5236575A · Bennett et al. · 1993 [cited by applicant]
US 5250277A · Kresge et al. · 1993 [cited by applicant]
US 5362697A · Fung · 1994 [cited by examiner]
US 5453554A · Cheng et al. · 1995 [cited by applicant]
US 5827491A · Emerson et al. · 1998 [cited by applicant]
US 6077498A · Diaz Cabanas et al. · 2000 [cited by applicant]
US 6756030B1 · Rohde et al. · 2004 [cited by applicant]
US 7713513B2 · Jan et al. · 2010 [cited by applicant]
US 7842277B2 · Roth et al. · 2010 [cited by applicant]
US 7959599B2 · Matusch · 2011 [cited by applicant]
US 8110176B2 · Roth et al. · 2012 [cited by applicant]
US 8115001B2 · Corma Canos et al. · 2012 [cited by applicant]
US 20110021856A1 · Lai et al. · 2011 [cited by applicant]
CN 102452665A · 2012 [cited by examiner]
EP 0293032 · 1993 [cited by applicant]
WO WO1997017290 · 1997 [cited by applicant]
WO WO2000006493 · 2000 [cited by applicant]
WO WO2000006494 · 2000 [cited by applicant]
WO WO2007094937 · 2007 [cited by applicant]
WO WO2010014406 · 2010 [cited by applicant]
WO WO2010021795 · 2010 [cited by applicant]
WO WO2013048636 · 2013 [cited by applicant]
WO WO2015043114 · 2015 [cited by applicant]
WO WO2015112293 · 2015 [cited by applicant]
Delitala, C. et al. (2009) “Synthesis of MCM-22 Zeolites of Different Si/Al Ratio and Their Structural, Morphological and Textural Characterisation,” [cited by applicant]
Gao, S. et al. (2013) “Green Synthesis of SUZ-4 Zeolite Controllable in Morphology and SiO [cited by applicant]
Lawton, S. L. et al. (1996) “Zeolite MCM-49: A Three-Dimensional MCM-22 Analogue Synthesized by in Situ Crystallization,” [cited by applicant]
Schwanke, et al. (2018) “Lamellar MWW-Type Zeolites: Toward Elegant Nanoporous Materials,” [cited by applicant]
Vuono, D. et al. (2004) “Synthesis and Characterization of MCM-22 and MCM-49 Zeolites,” [cited by applicant]