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beta molecular sieve synthesis method
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A synthesis method and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., to achieve the effects of high specific surface area, simplified process steps, and high crystallinity
Active Publication Date: 2016-05-11
华微科技(苏州)有限公司
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[0006] CN1154341A discloses a kind of synthetic method of Beta molecular sieve, this method adopts two-step crystallization method on the basis of CN1108214A one-step crystallization method, this method has further reduced template dosage, but still higher, TEA + / SiO 2 =0.03~0.20
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Embodiment l~7
[0044] Embodiment 1~7 synthesizes Beta molecular sieve according to the inventive method:
[0045] a) adding sodium metaaluminate (sodium oxide 55wt%, aluminum oxide 45wt%) and tetraethylammonium hydroxide aqueous solution (TEAOH, 25%) into deionized water, dissolved, stirred evenly, and made into the original solution;
[0046] b) The original solution is hydrothermally treated at a specific temperature for a certain period of time, and the parameters are shown in Table 1;
[0047] c) Mix silica gel (100-140 mesh, 6.5% reduction on ignition) with the above working solution, so that the surface of the silica sol is wetted by the working solution;
[0048] d) The silica sol after the wetting treatment was crystallized at 150° C. for 48 hours;
[0049] e) After the crystallization treatment, the product is separated, washed, dried at 120°C, and calcined at 550°C to obtain a Beta molecular sieve product.
[0050] The XRD crystal phase diagram of the molecular sieve obtained by ...
Embodiment 8~13
[0054] Embodiment 8~13 synthesizes Beta molecular sieve according to the inventive method:
[0055] a) Add sodium metaaluminate (55wt% sodium oxide, 45wt% aluminum oxide) and tetraethylammonium hydroxide aqueous solution (TEAOH, 25%) into deionized water, dissolve, stir evenly, and prepare the original solution;
[0056] b) The original solution is hydrothermally treated at 100°C for 24 hours;
[0057] c) Mix silica gel (200-300 mesh, 6.5% reduction on ignition) with the above working solution, so that the surface of the silica sol is wetted by the working solution;
[0058] d) The silica sol after the wetting treatment is crystallized at a specific temperature for a certain period of time, and the parameters are shown in Table 2;
[0059] e) After the crystallization treatment, the product is separated, washed, dried at 120°C, and calcined at 550°C to obtain a Beta molecular sieve product.
[0060] The XRD crystal phase diagram of the molecular sieve obtained by Examples 8-...
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Abstract
The invention discloses a synthetic method of a Beta molecular sieve. The synthetic method comprises the following steps: a) dissolving an aluminum source, a template agent and a sodium source into water to prepare an original liquid; b) activating the original liquid for 2-24 hours at 60-120 DEG C to obtain a hot activated liquid; c) by taking silica gel particles with a particle size of 20-1000 meshes as a silicon source, mixing the silica gel with the hot activated liquid to wet the surface of the silica gel with the hot activated liquid; d) keeping the wetted silica gel for 24-48 hours at a constant temperature of 120-180 DEG C to carry out crystallization treatment; and e) after the crystallization treatment, separating, washing, drying and burning the product to obtain the Beta molecular sieve product. According to the synthetic method of the Beta molecular sieve, the consumption of the template agent is greatly reduced, the process steps are simplified, the crystallization is completed by one step, and the crystallization time is only 1-2 days. And moreover, physical and chemical performances such as the silica-alumina ratio, the specific surface area and the relative crystallinity of the obtained Beta molecular sieve are obviously improved.
Description
technical field [0001] The invention relates to the field of synthesis of crystalline aluminosilicate molecular sieves, in particular to a method for synthesizing Beta molecular sieves. Background technique [0002] Beta molecular sieves were synthesized by the classic hydrothermal crystallization method for the first time in 1967 by Mobil Corporation of the United States (US3308069). Due to its unique topological structure and good thermal and hydrothermal stability, it exhibits excellent catalytic performance in alkylation, hydrocracking, hydroisomerization, hydrofinishing, and hydrocarbon cracking. [0003] In the common synthesis method of Beta molecular sieve, the mixture containing silicon source, aluminum source, sodium source, templating agent and water is mostly made into slurry, and crystallized in an autoclave at 75-200°C for 3-60 days. [0004] US4847055 discloses an improved Beta molecular sieve technology, using a silicon source with a special particle size, t...
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