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High activity small crystal zsm-12

A ZSM-12, porous crystallization technology, applied in the direction of ZSM-12 crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, physical/chemical process catalysts, etc.

Inactive Publication Date: 2006-05-17
EXXONMOBIL CHEM PAT INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is generally difficult to synthesize both small crystal size and low SiO 2 / Al 2 o 3 Ratio of high purity ZSM-12

Method used

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  • High activity small crystal zsm-12
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  • High activity small crystal zsm-12

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Embodiment 1 (comparison)

[0064] A mixture was prepared from 306 g water, 83 g 50% tetraethylammonium bromide (TEABr), 64.3 g UltrasilPM, 1.55 g aluminum hydroxide and 15.8 g 50% sodium hydroxide solution. This mixture has the following molar composition:

[0065] SiO 2 / Al 2 o 3 =100

[0066] h 2 O / SiO 2 =20

[0067] Oh - / SiO 2 =0.2

[0068] Na + / SiO 2 =0.2

[0069] TEABr / SiO 2 =0.2

[0070] The mixture was reacted in a 600 ml autoclave at 285°F (140°C) for 168 hours at a stirring speed of 150 RPM. The product was filtered, washed with deionized water (DI) and dried at 250°F (120°C). The XRD pattern of the as-synthesized material shows a typical pure phase of the ZSM-12 topology. The SEM photographs of the as-synthesized materials are shown in figure 1 , and show that the material consists of agglomerates of small crystals (average crystal size approximately 0.05 microns).

[0071] The synthesized crystals were converted to the hydrogen form by ...

Embodiment 2

[0072]Embodiment 2 (comparison)

[0073] The same reactants and reaction procedure as in Example 1 were used except that methyltriethylammonium bromide (MTEA) was used as the directing agent.

[0074] The SEM photographs of the as-synthesized materials are shown in figure 2 , and showed that the material consisted of agglomerates of rice-like crystals (average crystal size 1-5 microns).

[0075] The synthesized crystals were converted to the hydrogen form by two ion exchanges with ammonium nitrate solution at room temperature, followed by drying at 250°F (120°C) and calcination at 1000°F (540°C) for 6 hours. The resulting ZSM-12 crystals have SiO 2 / Al 2 o 3 Molar ratio of 116, alpha value of 92, and D / r for 1,3,5-trimethylbenzene (mesitylene) at 100°C 2 The parameter is 19×10 -6 .

Embodiment 3

[0076] Embodiment 3 (comparison)

[0077] A mixture was prepared from 348 g water, 30 g methyltriethylammonium chloride (MTEACl), 64.3 g UltrasilPM, 2.33 g aluminum hydroxide and 17.4 g 50% sodium hydroxide solution. This mixture has the following molar composition:

[0078] SiO 2 / Al 2 o 3 =67

[0079] h 2 O / SiO 2 =20

[0080] Oh - / SiO 2 =0.22

[0081] Na + / SiO 2 =0.22

[0082] MTEACl / SiO 2 =0.2

[0083] The mixture was reacted in a 600 ml autoclave at 285°F (140°C) for 168 hours at a stirring speed of 150 RPM. The product was filtered, washed with deionized water (DI) and dried at 250°F (120°C). The XRD pattern of the as-synthesized material shows a typical pure phase of the ZSM-12 topology. The SEM of the synthesized material is shown in image 3 , and show that the material consists of agglomerates of small crystals (average crystal size approximately 0.05 microns).

[0084] The synthesized crystals were converted to the hydrogen form by two ion exchan...

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Abstract

A porous crystalline material having a ZSM-12 skeleton structure and a composition conforming to the following molar relationship: X2O3: (n)YO2, wherein X is a trivalent element, Y is a tetravalent element, n is less than 60, and the average crystal of the material The size is less than 0.1 microns, and the material has a diffusion parameter for mesitylene of at least 1000 x 10-6 sec-1 when measured at a temperature of 100°C and a mesitylene pressure of 2 Torr.

Description

field of invention [0001] The present invention relates to a highly active small crystal ZSM-12, its synthesis and its use in catalytic processes, especially in C 9 + Application in the process of conversion of aromatic hydrocarbons into xylenes. Background of the invention [0002] ZSM-12 and its conventional preparation in the presence of tetramethylammonium or tetraethylammonium directing agents are taught in US Patent No. 3,832,449, which is hereby incorporated by reference. ZSM-12's unique X-ray diffraction pattern distinguishes it from other known crystalline materials. [0003] US Patent No. 4391785 discloses a method of synthesizing ZSM-12 from a reaction mixture comprising, as an orienting agent, a compound selected from dimethylpyridinium halide and dimethylpyrrolidinium halide salt. [0004] US Patent Nos. 4,452,769 and 4,537,758 disclose the synthesis of ZSM-12 from reaction mixtures containing methyltriethylammonium ions as directing agents. However, these pa...

Claims

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Application Information

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IPC IPC(8): C01B39/42B01J23/80B01J29/70B01J29/78B01J35/00C07C4/18C07C6/12C10G45/64
CPCB01J23/80B01J29/7034B01J29/80B01J2229/20B01J2229/42C01B39/42C07C6/126C10G45/64C10G2400/30Y10S423/33Y02P20/52B01J35/30C07C15/08B01J29/06
Inventor I·D·约翰逊W·F·莱
Owner EXXONMOBIL CHEM PAT INC
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