Synthesis and use of molecular sieve ITQ-32

Patent metadata

Field	Value
Publication number	US-9266087-B2
Application number	US-201314077426-A
Country	US
Kind code	B2
Filing date	Nov 12, 2013
Priority date	Dec 10, 2012
Publication date	Feb 23, 2016
Grant date	Feb 23, 2016

Abstract

The present invention relates to molecular sieves having the structure of ITQ-32 is synthesized from a reaction mixture substantially free of fluoride ions and comprising 4,4-dimethyl, 1-cyclohexyl-piperazinium cations in its pore structure, as well as methods of making such molecular sieves and methods of using them.

First claim

What is claimed is:

1. A molecular sieve having the structure of ITQ-32 and, in its as-synthesized form, being substantially free of fluoride ions.

2. The molecular sieve of claim 1 , which comprises silicon and boron in an atomic ratio (Si/B) greater than 8:1.

3. The molecular sieve of claim 1 , wherein the molecular sieve is substantially free of ZSM-12.

4. A molecular sieve having the structure of ITQ-32 and, in its as-synthesized form, being substantially free of fluoride ions and comprising 4,4-dimethyl,1-cyclohexylpiperazinium cations in its pore structure.

5. The molecular sieve of claim 4 , which has a composition comprising the molar relationship: qQ + :xX 2 O 3 :SiO 2 , wherein 0<q≦0.06, 0≦x≦0.05, Q + comprises a 4,4-dimethyl,1-cyclohexylpiperazinium cation, and X comprises a trivalent element.

6. The molecular sieve of claim 5 , wherein the trivalent element X comprises at least one of aluminum, boron, chromium, gallium and iron.

7. The molecular sieve of claim 5 , wherein the trivalent element X comprises boron.

8. A process for producing a molecular sieve having the structure of ITQ-32, the process comprising:
(i) preparing a synthesis mixture capable of forming said molecular sieve and comprising water, a source of silica, a source of a trivalent element (X), and a source of 4,4-dimethyl,1-cyclohexylpiperazinium cations (Q + ), the synthesis mixture being substantially free of fluoride ions and having a composition, in terms of molar ratios, within the following amounts:

SiO 2 /X 2 O 3
about 2 to about 100;

Q + /SiO 2
about 0.02 to about 1.0; and

H 2 O/SiO 2
about 10 to about 60;

(ii) heating the mixture under crystallization conditions comprising a temperature of from about 100° C. to about 200° C. and a time from about 1 day to about 28 days until crystals of the molecular sieve are formed; and
(iii) recovering the molecular sieve from step (ii).

9. The process of claim 8 , wherein the trivalent element X comprises at least one of aluminum, boron, chromium, gallium and iron.

10. The process of claim 8 , wherein the trivalent element X comprises boron.

11. The process of claim 8 , wherein the synthesis mixture comprises a source of chloride ions.

12. The process of claim 11 , wherein the synthesis mixture exhibits a Cl − /SiO 2 molar ratio up to about 0.3.

13. The process of claim 8 , wherein the synthesis mixture also contains seeds.

14. The process of claim 8 , wherein the synthesis mixture comprises from about 0.01 wppm to about 10000 wppm seeds.

15. The process of claim 8 , wherein the synthesis mixture comprises from about 100 wppm to about 5000 wppm seeds.

16. The process of claim 15 , wherein the seeds comprise a crystalline material having the structure of ITQ-32.

17. The process of claim 8 , further comprising removing and/or decomposing at least part of the organic material from the molecular sieve crystals recovered in step (iii).

Assignees

• Burton Allen W
• Weston Simon C
• Strohmaier Karl G
• Vroman Hilda B
• Exxonmobil Res & Eng Co

Inventors

• Burton Allen W
• Weston Simon C
• Strohmaier Karl G
• Vroman Hilda B

Classifications

• B01J20/186

  Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity · CPC title

• B01J29/76

  Iron group metals or copper · CPC title

• B01J20/226 Primary

  Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF] (preparation of metal complexes containing carboxylic acid moieties C07C51/418; MOF's per se C07F) · CPC title

• B01D2253/116

  Molecular sieves other than zeolites · CPC title

• B01J29/70

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