Synthesis of high activity ZSM-48

A ZSM-48, water-based technology used in the synthesis of highly active ZSM-48 and its use as a catalyst

Active Publication Date: 2010-08-11
EXXON RES & ENG CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a product of the synthesis of Rollman et al., zeolites contain little or no aluminum and thus have little or no acid activity

Method used

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  • Synthesis of high activity ZSM-48
  • Synthesis of high activity ZSM-48
  • Synthesis of high activity ZSM-48

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Use diquat-5 and low OH - / SiO 2 Recently prepared highly active ZSM-48

[0077] A mixture was prepared from 1040 g water, 45 g pentamethyl onium dibromide (50% solution), 200 g Ultrasil silica, 11 g sodium aluminate solution (45%) and 36 g 50% sodium hydroxide solution. 5 g of ZSM-48 seeds were then added to the mixture. The mixture has the following molar composition:

[0078] SiO 2 / Al 2 O 3 : 102

[0079] H 2 O / SiO 2 : 20

[0080] OH - / SiO 2 : 0.17

[0081] Na + / SiO 2 : 0.17

[0082] Chlorpyrifos-5 / SiO 2 : 0.02

[0083] The mixture was reacted at 320°F (160°C) for 48 hours in a 2 liter autoclave stirred at 350 RPM. The product was filtered, washed with deionized (DI) water and dried at 250°F (120°C). XRD patterns of synthetic materials (see Figure 1A ) shows the typical pure phase of ZSM-48 topology. SEM of the composite material (see Figure 1B ) shows that the material consists of agglomerates of elongated needle-like crysta...

Embodiment 2

[0084] Example 2 (comparative example)

[0085] Use diquat-5, low OH - / SiO 2 SiO with high ratio and 2 / Al 2 O 3 to prepare the active ZSM-48

[0086] A mixture was prepared from 1100 g water, 65 g pentamethyl onium dibromide (50% solution), 228 g Ultrasil silica, 6 g sodium aluminate solution (45%) and 45 g 50% sodium hydroxide solution. The mixture has the following molar composition:

[0087] SiO 2 / Al 2 O 3 : 195

[0088] H 2 O / SiO 2 : 19

[0089] OH - / SiO 2 : 0.17

[0090] Na + / SiO 2 : 0.17

[0091] Chlorpyrifos-5 / SiO 2 : 0.027

[0092] The mixture was reacted at 320°F (160°C) for 48 hours in a 2 liter autoclave stirred at 350 RPM. The product was filtered, washed with deionized (DI) water and dried at 250°F (120°C). XRD patterns of synthetic materials (see Figure 2A ) shows the typical pure phase of ZSM-48 topology. SEM of the composite material (see Figure 2B ) shows that the material consists of agglomerate...

Embodiment 3

[0093] Example 3 (comparative example)

[0094] Use diquat-5 and high OH - / SiO 2 Recently prepared highly active ZSM-48

[0095] From 360g water, 39g pentamethylonium dibromide (50% solution), 35.6g Aerosil 130 silica, 6.9g Al(NO 3 ) 3 .xH 2 O and 14.4 g of a 50% sodium hydroxide solution to prepare a mixture. 5 g of ZSM-48 seeds were then added to the mixture. The mixture has the following molar composition:

[0096] SiO 2 / Al 2 O 3 : 60

[0097] H 2 O / SiO 2 : 40

[0098] OH - / SiO 2 : 0.33

[0099] Na + / SiO 2 : 0.33

[0100] Chlorpyrifos-5 / SiO 2 : 0.1

[0101] The mixture was aged at room temperature with stirring at 100 RPM and then reacted in a 600 ml autoclave at 320°F (160°C) for 96 hours with stirring at 100 RPM. The product was filtered, washed with deionized (DI) water and dried at 250°F (120°C). The XRD patterns of the synthesized materials show typical phases of the ZSM-48 topology. SEM of the composite materi...

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Abstract

A process for producing ZSM-48 comprises crystallizing an aqueous reaction mixture comprising at least one source of silica, at least one source of alumina, at least one source of hydroxyl ions, at least one source of diquaternary alkylammonium, R2+, ions having the formula: (CH3)3N+(CH2)5N+(CH3)3 and optionally ZSM-48 seed crystals, wherein said reaction mixture has a composition including the following molar ratios: R2+:SiO2 less than 0.1 SiO2:Al2O3 less than 100.

Description

technical field [0001] The present invention relates to the synthesis of highly active ZSM-48 and its use as a catalyst, especially in the dewaxing of hydrocarbon feedstocks. technical background [0002] ZSM-48 is a zeolite with ten-ring uninterconnected linear channels of orthorhombic or pseudo-orthorhombic symmetry, with ideal dimensions of 5.5×5.6 ZSM-48 has shown attractive properties as a hydrocarbon feed dewaxing catalyst, see for example US Patents 5,075,269 and 6,884,339, and International Publication WO 01 / 64339. Therefore, there is great interest in discovering new methods for synthesizing ZSM-48, especially ZSM-48 with high acid activity (ie, low silica / alumina molar ratio). [0003] Rollmann et al. used C as a structure directing agent 4 ~C 12 Organic diamines first synthesized ZSM-48, see US Pat. No. 4,423,021. As a product synthesized by Rollman et al., the zeolite contains little or no aluminum and thus has little acid activity. [0004] described in U....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00C01B39/46C01B39/48B01J29/04B01J29/06C10G73/02
CPCC10G45/64C10G2300/1022B01J2229/42B01J2229/20B01J29/703B01J29/7461C01B39/48B01J37/0009B01J35/0066
Inventor 文伊·F·莱维斯拉夫·J·罗斯罗伯特·E·卡伊克里斯蒂·N·伊莱亚
Owner EXXON RES & ENG CO
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