Method for preparing zeolite ssz-35

A technology of SSZ-35 and zeolite, applied in the field of preparing zeolite SSZ-35, can solve the problems of expensive, complicated SSZ-35, complicated SDA and the like

Inactive Publication Date: 2016-05-04
CHEVROU USA INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, these SDAs are complex and expensive, making the synthesis of SSZ-35 complex and expensive using these SDAs
This cost can limit the availability of SSZ-35 in industrial processes

Method used

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  • Method for preparing zeolite ssz-35
  • Method for preparing zeolite ssz-35
  • Method for preparing zeolite ssz-35

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] Synthesis of N,N-diethyl-2,3-dimethylpiperidinium cation

[0083] A 3-neck round bottom flask (equipped with mechanical stirrer, heating mantle, and reflux condenser) was charged with one molar equivalent of methanol in methanol sufficient to prepare a 0.5M solution for 2,3-dimethylpiperidine. 2,3-Dimethylpiperidine (note that 2,3-dimethylpiperidine can be purchased directly from commercial sources or prepared by metal catalyzed hydrogenation of 2,3-lutidine). To this solution was added 1.5 molar equivalents of potassium bicarbonate. The solution was stirred for several minutes, then 2.5 molar equivalents of iodoethane were added dropwise via the addition funnel. Once the iodoethane feed was complete, the reaction mixture was heated at reflux (about 55°C) for several hours. The heat was turned off and the reaction mixture was then stirred at room temperature for a further 48 hours. The progress of the reaction was monitored by NMR. Once complete, the reaction mixtur...

Embodiment 2

[0089] Synthesis of N,N-Dimethyl-2-isopropylpiperidinium Cation

[0090] Starting from 2-isopropylpiperidine in methanol, potassium bicarbonate and methyl iodide as reactants, N,N-dimethyl-2-isopropylpiperidine was synthesized in the manner described in Example 1 Onium cation. The reaction afforded N,N-dimethyl-2-isopropylpiperidinium iodide in greater than 95% yield. The iodide counterion was exchanged with hydroxide ion in the manner described in Example 1 to obtain the corresponding N,N-dimethyl-2-isopropylpiperidinium hydroxide in equivalent yield.

[0091] Scheme 2 below describes the synthesis of SDA.

[0092] Schema 2

[0093]

[0094] N,N-Dimethyl-2-isopropylpiperidinium

Embodiment 3

[0096] Synthesis of aluminosilicate SSZ-35 (Al-SSZ-35) using N,N-diethyl-2,3-dimethylpiperidinium cation

[0097] 4.5 grams of a 0.55M solution of N,N-diethyl-2,3-dimethylpiperidinium hydroxide, 1.5 grams of 1N aqueous NaOH, and 4.6 grams of deionized water were all mixed in a 23 mL Teflon liner. To this solution was added 0.035 grams of Reheis F-2000 aluminum hydroxide and stirred until dissolved. Subsequently, 0.9 g of M-5 fumed silica and the solution was stirred until a very homogeneous gel was obtained. The resulting gel was enclosed in a Teflon liner and placed in an autoclave, heated in an oven on a rotating spit at 170°C for 5 days. The gel mixture turned into a clear solution with finely powdered solids settled on the bottom of the Teflon inner substrate. The solid mixture was filtered into a fritted glass funnel. The collected solids were washed thoroughly with 1 liter of deionized water and left to dry under vacuum overnight. The solid was further dried in an ...

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Abstract

A method for making zeolite SSZ-35 is disclosed using a N,N-diethyl-2,3-dimethylpiperidinium cation or a N,N-dimethyl-2-isopropylpiperidinium cation as a structure directing agent.

Description

technical field [0001] The present disclosure generally relates to the preparation of zeolites SSZ- using N,N-diethyl-2,3-dimethylpiperidinium cations or N,N-dimethyl-2-isopropylpiperidinium cations as structure directing agents 35 methods. Background of the Invention [0002] Zeolites are a commercially important class of crystalline materials. They have different crystal structures with ordered pore structures confirmed by different X-ray diffraction patterns. The crystal structure defines cavities and pores that are characteristic of different species. [0003] Zeolites identified by the International Zeolite Association as having the structure code STF are known. For example, a zeolite known as SSZ-35 is a known crystalline STF material. US Patent No. 5,316,753 discloses the use of various conformationally constrained azapolycyclic ring systems as structure directing agents (SDA) for the preparation of SSZ-35, including 3,3-dimethyl-3-azanium-7-methyl -7-Aza-bicyclo...

Claims

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Application Information

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IPC IPC(8): C01B39/12C01B39/48
CPCB01J29/70B01J29/86C01B39/12C01B39/48
Inventor S·A·埃勒玛丽
Owner CHEVROU USA INC
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