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Method for synthesizing Beta zeolite molecular sieve

A technology of beta zeolite and synthesis method, applied in the field of synthesis of beta zeolite molecular sieves, to achieve the effects of broadening the range of crystal seeds and overcoming the difficulty of stirring

Active Publication Date: 2012-11-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through research, we found that the original powder of Beta zeolite with different grain sizes is used as the seed crystal, the seed crystal is dried and dehydrated at low temperature before use, and the seed crystal is dispersed with the gel in high-speed shear emulsification during use. The above measures are effective. Improves the efficacy of seed directing, thereby helping to overcome problems with existing methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] First use 1.63g NaOH solid, 16.67g silica sol (industrial grade, SiO 2 ≥30wt%), 3.06g TEAOH solution (technical grade) and 4.43g deionized water preparation solution A; With 0.52gNaAlO 2 (chemically pure) and 5.50 g of deionized water to prepare solution B. Then, solution A and solution B were uniformly mixed under vigorous stirring to form gel C. Finally, add 0.59g nano Beta zeolite seed crystal former powder in gel C (TEAOH is the synthesis of template system, SiO 2 / Al 2 o 3 =20.9, 50 ℃ vacuum drying 60 minutes after technical alcohol wash once), the molar ratio of each material is: SiO 2 / Al 2 o 3 =40, NaOH / SiO 2 = 0.45, TEA 2 O / SiO 2 =0.025,H 2 O / SiO 2 =16, seed / SiO 2 =10wt%, continue to stir for about 30 minutes, and then use a high-speed shear emulsifier to emulsify for 10 minutes at 6000 (rev / min), and the prepared gel is packed into a stainless steel reactor with a polytetrafluoroethylene liner , crystallized at 150°C for about 8 hours, cooled to r...

Embodiment 2

[0051] Repeat embodiment 1, but the alcohol washing step in the seed crystal pretreatment condition added is respectively changed into no industrial alcohol washing, industrial alcohol washing twice, industrial alcohol washing three times, and the product crystal phases obtained are all Beta zeolites, which are relatively The degrees of crystallinity were 64.9%, 74.8%, and 75.2%, respectively.

Embodiment 3

[0053] Repeat Example 1, but change the added seed crystal pretreatment conditions into 70°C, 90°C, 110°C, 140°C and vacuum-dry for 60) minutes respectively, the product crystal phases obtained are all Beta zeolites, and their relative crystallinities are respectively 74.1%, 73.6%, 67.9%, 62.2%.

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Abstract

The invention belongs to the field of aluminosilicate zeolite molecular sieve synthesis, and relates to a method for synthesizing a Beta zeolite molecular sieve. The Beta zeolite is a high-silicon zeolite with a three-dimensional twelve-member ring cross pore canal structure; the Beta zeolite is used as a catalyst in petroleum refining and petroleum chemical engineering processes of hydrogen cracking, hydroisomerization, de-waxing, aromatic hydrocarbon alkylation, olefin hydration and the like due to unique structure and good thermal stability and hydrothermal stability of the Beta zeolite; and the Beta zeolite molecular sieve is an important industrial zeolite molecular sieve. Because a large amount of organic template agent is used for synthesizing the Beta zeolite, the cost is high, and the wide application of the Beta zeolite is limited. By adding low-temperature dried Beta zeolite raw powder serving as crystal seeds and performing high-speed shearing emulsification dispersion on the crystal seeds during preparing gel, the structure guiding effect of the Beta zeolite crystal seeds is fully exerted, the applicable crystal seed range is broadened, and the Beta zeolite product with good crystallinity is synthesized under low template agent consumption and wide silicon-aluminum ratio range.

Description

technical field [0001] The invention belongs to the field of synthesis of aluminosilicate zeolite molecular sieves, and relates to a synthesis method of Beta zeolite molecular sieves. Background technique [0002] Beta zeolite is a high silica zeolite with a three-dimensional twelve-membered ring intersecting channel structure. Because of its unique structure, good thermal stability and hydrothermal stability, it is used as a catalyst in hydrocracking, hydroisomerization, It is used in petroleum refining and petrochemical processes such as dewaxing, aromatic hydrocarbon alkylation and olefin hydration, and is an important industrial zeolite molecular sieve. The following publications and patents relate to the application of Beta zeolite: [0003] (1) Hydrocracking: Acta Physica et Chemica (1985), 31(1-2), 487-95; Studies in Surface Science and Catalysis (2003), 145, 219-222; Acta Physicochemica Sinica (2008), 24( 7), 1192-1198; Journal of Chemical Engineering of Japan (200...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02C01B39/04
Inventor 郭洪臣郑步梅万玉凤谢红
Owner DALIAN UNIV OF TECH
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