Autoclave reactor

Example 4

0.50 g of deionized water, 0.12 g of a 45% KOH solution, 1.86 g of 13.62% 1-adamantyl-3-propylimidazolium hydroxide solution and 0.30 g of Zeolyst CBV720 Y-zeolite powder (SAR=30) were mixed together in a Teflon liner. The gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 150° C. for 16 days under static conditions. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

The resulting product was identified by powder XRD and SEM as a pure aluminosilicate molecular sieve having the BOG framework type structure.

The product had a SiO₂/Al₂O₃ molar ratio of 24.7, as determined by ICP-AES elemental analysis.

Example 3

1.31 g of deionized water, 0.12 g of a 50% NaOH solution, 0.93 g of a 13.62% 1-adamantyl-3-propylimidazolium hydroxide solution and 0.30 g of Zeolyst CBV760 Y-zeolite powder (SAR=60) were mixed together in a Teflon liner. The resulting gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 150° C. for 10 days under static conditions. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

The resulting product was identified by powder XRD and SEM as a pure aluminosilicate molecular sieve having the BOG framework type structure.

The product has a SAR of 48.8, as determined by ICP-AES elemental analysis.

Example 3

52.86 g of deionized water, 2.58 g of a 50% NaOH solution, 4.76 g of a 20% hexamethonium hydroxide solution, 15.71 g of a 16.33% 1-methyl-1-butylpyrrolidinium hydroxide solution, and 5.00 g of CBV760 Y-zeolite powder (Zeolyst International, SiO₂/Al₂O₃ molar ratio=60) were mixed together in a Teflon liner. The resulting gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 150° C. for 3 days. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

Powder XRD indicated that the product was a pure AFT framework type molecular sieve.

The product had a SiO₂/Al₂O₃ molar ratio of 13.00, as determined by ICP-MS.

Example 2

22.49 g of deionized water, 1.29 g of a 50% NaOH solution, 0.38 g of a 20% hexamethonium hydroxide solution, 4.36 g of a 11.78% solution of 1-methyl-1-propylpiperidinium hydroxide solution, and 2.00 g of CBV760 Y-zeolite powder (Zeolyst International, SiO₂/Al₂O₃ molar ratio=60) were mixed together in a Teflon liner. The resulting gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 150° C. for 3 days. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

Powder XRD indicated that the product was a pure AFT framework type molecular sieve.

The product had a SiO₂/Al₂O₃ molar ratio of 13.75, as determined by ICP-MS.

Example 3

2.46 g of deionized water, 0.37 g of a 45% KOH solution, 2.68 g of a 17.8% 1-ethyl-1-[5-(triethylammonio)pentyl]piperidinium hydroxide solution, 0.05 g of Reheis F-2000 aluminum hydroxide dried gel and 2.00 g of LUDOX® AS-30 colloidal silica were mixed together in a Teflon liner. The gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 160° C. for 10 days with tumbling at 43 rpm. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

Analysis by powder XRD showed the product to be an MFS framework type molecular sieve.

The product had a SiO₂/Al₂O₃ molar ratio of 31.2, as determined by ICP-AES elemental analysis.

Example 4

3.20 g of deionized water, 0.37 g of a 45% KOH solution, 1.79 g of a 17.8% 1-ethyl-1-[5-(triethylammonio)pentyl]piperidinium hydroxide solution, 0.04 g of Reheis F-2000 aluminum hydroxide dried gel and 2.00 g of LUDOX® AS-30 colloidal silica were mixed together in a Teflon liner. The gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 160° C. for 10 days with tumbling at 43 rpm. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

Analysis by powder XRD showed the product to be a mixture of an MFS-type molecular sieve and a dense phase.

Example 1

2.88 g of deionized water, 0.06 g of a 50% NaOH solution, 0.83 g of a 14.21% N¹,N⁶-diisopropyl-N¹,N¹,N⁶,N⁶-tetramethylhexane-1,6-diaminium hydroxide solution, and 0.50 g of CBV780 Y-zeolite (Zeolyst International; SiO₂/Al₂O₃ molar ratio=80) were mixed together in a Teflon liner. The resulting gel was stirred until it became homogeneous. The liner was then capped and placed within a Parr Steel autoclave reactor. The autoclave was then put in an oven heated at 160° C. for 6 days under static conditions. The solid products were recovered from the cooled reactor by centrifugation, washed with deionized water and dried at 95° C.

The resulting product was analyzed by powder XRD and SEM. The powder XRD pattern of the product is shown FIG. 1 and is consistent with the product being SSZ-109. A SEM image of the product is shown in FIG. 2 and indicates a uniform field of crystals.

The product had a SiO₂/Al₂O₃ molar ratio of 90.4, as determined by Inductively Coupled Plasma (ICP) elemental analysis.

Example 9

The as-synthesized SSZ-109 product from Example 1 was calcined inside a muffle furnace under a flow of mixed nitrogen and air heated to 540° C. at a rate of 1° C./minute and held at 540° C. for 5 hours, cooled and then analyzed by powder XRD. The powder XRD data indicated that the material remains stable after calcination to remove the organic matter.