Small crystal EMM-17, its method of making and use

Patent metadata

Field	Value
Publication number	US-10696560-B2
Application number	US-201816021176-A
Country	US
Kind code	B2
Filing date	Jun 28, 2018
Priority date	Jul 27, 2017
Publication date	Jun 30, 2020
Grant date	Jun 30, 2020

Abstract

A molecular sieve material, EMM-17, has in its as-calcined form, a total surface area of greater than 550 m2/g and/or an external surface area of greater than about 100 m2/g as measured by the BET Method, and a specific X-ray diffraction pattern.

First claim

The invention claimed is:

1. A crystalline molecular sieve material having, in its as-synthesized form, a particle size of less than 1.0 micron as measured by SEM, and an X-ray diffraction pattern including the following peaks in Table 2:

TABLE 2

d-spacing
Relative Intensity

(Å)
[100 × I/I(o)] %

17.3-16.4
1-10

11.8-11.3
60-100

11.1-10.7
60-100

10.7-10.3
30-100

8.58-8.34
30-80 

4.21-4.15
10-40 

4.17-4.11
5-30

4.07-4.01
10-40 

3.951-3.899
60-100

3.922-3.871
10-40 

3.832-3.784
50-90 

3.737-3.691
10-40 

3.704-3.659
10-40 

3.677-3.632
5-30

3.537-3.496
10-40 

2.077-2.063
 5-30.

2. The crystalline molecular sieve material of claim 1 having a composition comprising the molar relationship:
k F: m Q:( n )YO 2 :X 2 O 3 ,

wherein 0≤k≤1.0, 0<m≤1.0, n is at least 30, F is a source of fluoride, Q is an organic structure directing agent, X is a trivalent element and Y is a tetravalent element.

3. The crystalline molecular sieve material of claim 2 , wherein X includes one or more of B, Al, Fe, and Ga and Y includes one or more of Si, Ge, Sn, Ti, and Zr.

4. The crystalline molecular sieve material of claim 2 , wherein X is aluminum and Y is silicon.

5. The crystalline molecular sieve material of claim 2 , wherein Q is selected from the group consisting of 1-methyl-4-(pyrrolidin-1-yl)pyridinium cations, 1-ethyl-4-(pyrrolidin-1-yl)pyridinium cations, 1-propyl-4-(pyrrolidin-1-yl)pyridinium cations, 1-butyl-4-(pyrrolidin-1-yl)pyridinium cations and mixtures thereof.

6. A crystalline molecular sieve material having, in its as-calcined form, a total surface area of greater than 550 m 2 /g and/or an external surface area of greater than 100 m 2 /g as measured by the BET Method, and an X-ray diffraction pattern including the following peaks in Table 1:

TABLE 1

d-spacing
Relative Intensity

(Å)
[100 × I/I(o)] %

17.4-16.4
1-10

12.6-12.1
1-20

11.8-11.4
60-100

11.2-10.8
5-30

10.7-10.3
30-80 

8.62-8.38
10-40 

6.09-5.96
1-20

5.71-5.61
1-20

4.23-4.17
1-20

4.09-4.03
1-10

3.952-3.901
10-40 

3.857-3.809
5-30

3.751-3.705
1-20

3.727-3.682
1-20

3.689-3.644
1-10

3.547-3.506
 1-20.

7. The crystalline molecular sieve material of claim 6 and having a composition comprising the molar relationship:
( n )YO 2 :X 2 O 3 ,

wherein n is at least 30, X is a trivalent element, and Y is a tetravalent element.

8. The crystalline molecular sieve material of claim 7 , wherein X includes one or more of B, Al, Fe, and Ga and Y includes one or more of Si, Ge, Sn, Ti, and Zr.

9. The crystalline molecular sieve material of claim 7 , wherein X is aluminum and Y is silicon.

10. The crystalline molecular sieve material of claim 6 , wherein the ratio of the external surface area to the total surface area of said as-calcined crystalline molecular sieve is greater than or equal to 0.35 as measured by the BET Method.

11. A method of making said crystalline molecular sieve material of claim 6 , the method comprising the steps of:
(a) preparing a synthesis mixture capable of forming said material, said mixture comprising water (H 2 O), a source of hydroxyl ions (OH − ), a source of an oxide of a tetravalent element (Y), optionally a source of a trivalent element (X), optionally a source of said fluoride ions (F − ), and said organic structure directing agent (Q), wherein said synthesis mixture has a composition, in terms of mole ratios, in the following amounts and/or ranges:

Assignees

• Exxonmobil Res & Eng Co
• Exxonmobil Res & Engineering Company

Inventors

• Johnson Ivy D
• Hrycenko Nadya A
• Datz Theodore E
• Lonergan William W
• Strohmaier Karl G
• Vroman Hilda B
• Gallow Keith C
• Weston Simon C

Classifications

• B01J20/18

  Synthetic zeolitic molecular sieves · CPC title

• C01B39/08

  the aluminium atoms being wholly replaced · CPC title

• C10G29/205

  by reaction with hydrocarbons added to the hydrocarbon oil · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• B01J29/70

  of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 · CPC title