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A technology of beta zeolite and synthesis method, which is applied in the field of synthesis of Beta zeolite molecular sieve, can solve the problems of low product yield, huge waste of raw materials, and limited industrial application, and achieve the effect of widening the range of seed crystals and overcoming the difficulty of stirring
Active Publication Date: 2012-06-20
DALIAN UNIV OF TECH
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(2) In the template-free system, only Beta zeolite products with a low silicon-aluminum ratio can be obtained at a high feed-silicon-alumina ratio, which means that a large amount of silicon sources are not crystallized into products, the product yield is low, and raw material waste is huge
However, the seed crystals used must be nanoscale, which has limitations for industrial applications
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Embodiment 1
[0051] The first step is to pretreat the Beta zeolite seed
[0052] (1) High-temperature hydrothermal treatment of Beta zeolite seed crystals: under an atmosphere of air and water vapor, wherein the content of water vapor is 20%, hydrothermal treatment of Beta zeolite seed crystals at 540° C. for 6 hours.
[0053] (2) Pickling the Beta zeolite seed crystals after high-temperature hydrothermal treatment: under stirring, soak the Beta zeolite seed crystals after high-temperature hydrothermal treatment in 0.5mol / L citric acid solution at 50°C for 10 hours. The liquid-solid mass ratio of the solution to the seed crystal solid was 5:1, and the acid-treated seed crystal was washed with water until neutral and dried at 110°C.
[0054] Second step, synthesize Beta zeolite with pretreated Beta zeolite seed crystal and template: first use 1.63g NaOH solid, 16.67g silica sol (industrial grade, SiO 2 ≥30wt%), 3.06g TEAOH solution (industrial grade) and 4.43g deionized water preparation s...
Embodiment 2
[0056] Repeat Example 1, change the Beta zeolite seed high-temperature hydrothermal treatment temperature in the first step (1), and the time is changed to 300 ° C, 100 hours; 400 ° C, 50 hours; 700 ° C, 0.5 hours, the obtained product crystal phase They are all Beta zeolites, and their relative crystallinities are 50.1%, 61.6%, and 68.6%, respectively.
Embodiment 3
[0058] Repeat Example 1, change the water vapor content into 1%, 50%, 70%, 100% respectively in the Beta zeolite seed high-temperature hydrothermal treatment in the first step (1), and the product crystal phases obtained are all Beta zeolite. The relative crystallinity is 58.0%, 71.3%, 74.9%, 75.2%, respectively.
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Abstract
The invention belongs to the field of synthesis of aluminosilicate zeolite molecular sieves, and relates to a Beta zeolite molecular sieve synthesis method. The Beta zeolite molecular sieve synthesis method is characterized in that a Beta zeolite crystal seed is in high-temperature hydrothermal treatment at first, then the Beta zeolite crystal seed after hydrothermal treatment is in dipping treatment in acid liquor when stirred, and the crystal seed after acid treatment is washed by water to be neutral; and finally, a silicon source, an aluminum source, a sodium source, a tetraethylammonium cation source and water are prepared to form uniform gel, the pretreated beta zeolite crystal seed is added into the gel, and obtained uniform gel is crystallized in a stainless steel reaction kettle. The beta zeolite molecular sieve synthesis method has the advantages that Beta zeolite is used as the crystal seed after the high-temperature hydrothermal treatment and the acid liquor treatment, a structural guidance effect of the Beta zeolite can be realized better, a Beta zeolite product with excellent crystallinity can be synthesized under conditions of low usage of structural-directing agent and wide silicon-aluminum ratio range, accordingly, crystal seeds are not limited in nanometer level granularity, and applicable range of the crystal seeds is greatly widened.
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 widely used in petroleum refining and petrochemical processes such as dewaxing, aromatic hydrocarbon alkylation and olefin hydration. Beta zeolite is an important industrial 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 Physicochemical Sinica, 2008, 24(7) , 1192-1198; Journal of Chemical Engineering of Japa...
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