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Method for synthesizing full-silicon beta zeolite with small crystal grains

A synthesis method, the technology of zeolite beta, which is applied in the field of synthesis of zeolite beta, can solve problems such as the inability to synthesize all-silicon beta zeolite, and achieve the effects of increased yield, reduced energy consumption, and reduced manufacturing costs

Active Publication Date: 2010-10-20
FORMOSAN UNION CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Since most commercial catalysts require the smaller the zeolite crystal grains, the better, and the existing technology cannot synthesize all-silicon beta zeolite in a short time

Method used

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  • Method for synthesizing full-silicon beta zeolite with small crystal grains
  • Method for synthesizing full-silicon beta zeolite with small crystal grains
  • Method for synthesizing full-silicon beta zeolite with small crystal grains

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preparation example Construction

[0055] Such as Figure 7 Shown, the synthetic method of small and medium grain all-silicon beta zeolite of the present invention comprises the following steps: (a) silicon dioxide (SiO 2 ) silicon source, fluoride ion (F - ) source, tetraethylammonium ion (TEA + ) source and deionized water (H 2 O) performing mixing (aging reaction) to form a reaction mixture; (b) subjecting the reaction mixture to a crystallization reaction until all-silica beta zeolites with a grain size of less than 5 μm are formed; (c) recovering the all-silicon beta zeolites and (d) calcining the all-silicon zeolite beta zeolite grains in an air environment at a temperature of 350 to 900° C. to remove the organic template inside the zeolite grains, wherein, before the crystallization reaction, the reaction mixture The pH value is between 6 and 9, and the pH value after the crystallization reaction is completed is between 6 and 8. Calcined all-silicon beta zeolite, soaked in water, its pH value is less...

Embodiment 1

[0125] First put 15.74 grams of silicic acid (Sigma) and 47.37 grams of tetraethylammonium hydroxide (TEAOH 35%, Aldrich) into a glass flat-bottomed flask, stir with a magnet for 3 days at 40 ° C, and then add 5.8 Concentrated hydrofluoric acid (48% HF) was added to the solution and stirred evenly, and finally the mixture turned into a white solid. The composition of this mixture is as follows:

[0126] SiO 2 / Al 2 o 3 =∞

[0127] TEA + / SiO 2 =0.56

[0128] h 2 O / SiO 2 =4.6

[0129] f - / SiO 2 =0.69

[0130] Then put the mixture into the reactor (with a Teflon (polytetrafluoroethylene, PTFE) bottle inside) and heat it to 140°C for static synthesis. After 4.5 days of reaction, it was cooled, and it was found that there was a solid in the product in the reactor. Below, and light brown liquid above (pH 6-7 for lower solid, pH 8-9 for upper liquid). Then filter, dry at 120°C, and calcine with dry air at 550°C for 8 hours. Finally, 12.33 g of zeolite beta solid prod...

Embodiment 2

[0132] First put 40.8 grams of silica gel solution (colloidal silica 30%, Ludox AS-30) and 46.85 grams of tetraethylammonium hydroxide (TEAOH 35%, Aldrich) into a glass flat-bottomed flask, and stir at 50 ° C for 48 hours . Then 9.0 grams of concentrated hydrofluoric acid (48% HF) was added into the solution and stirred evenly, and finally the mixture became a white solid, and its composition was as follows:

[0133] SiO 2 / Al 2 o 3 =∞

[0134] TEA + / SiO 2 =0.55

[0135] h 2 O / SiO 2 =3.2

[0136] f - / SiO 2 =0.60

[0137] Then the mixture was put into a reaction kettle (with a Teflon bottle inside) and heated to 140° C. for static synthesis, and cooled after 4.5 days of reaction. The product result and processing steps were the same as in Example 1. Obtaining beta zeolite solid product weight at last is 11.08 grams, productive rate is 88%, can find out from XRD pattern that its relative crystallinity is 108% (compared with standard product), and SEM pattern shows...

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Abstract

The invention discloses a method for synthesizing full-silicon beta zeolite with small crystal grains. The method comprises the following steps of: (a) mixing a silicon source, a fluorine ion source, a tetraethyl ammonium ion source and deionized water according to a specific formation mole ratio to form a reaction mixture; (b) carrying out a crystallization reaction on the reaction mixture untilthe full-silicon beta zeolite the grain size of which is smaller than 5mum is formed; and (c) recovering the full-silicon beta zeolite. By utilizing the method, full-silicon beta zeolite crystals with small crystal grains can be synthesized in a short time, and the yield of the full-silicon beta zeolite crystals with small crystal grains is greater than 90 percent. The full-silicon beta zeolite with small crystal grains, which is synthesized by the method, can be used for manufacturing a zeolite film or can be used as a carrier used for loading a catalyst.

Description

technical field [0001] The invention relates to a method for synthesizing zeolite beta, in particular to a method for synthesizing small-grain all-silicon beta zeolite. Background technique [0002] Beta zeolite was first synthesized by traditional hydrothermal method in 1967. Beta zeolite is characterized by a 12-member ring channel structure with three-dimensional space. Due to its unique structure and good thermal stability, beta zeolite can , Isomerization, cyclization, alkylation, hydrocracking, etc. all show excellent properties, and are highly concerned synthetic materials in industry. [0003] Zeolite beta is mostly used in heterogeneous catalytic reactions. The heterogeneous catalytic reaction refers to the completion of reactants on the surface of the catalyst through a series of processes such as adsorption, diffusion, chemical reaction and desorption. The heterogeneous catalytic reaction occurs at the interface, and the performance of the catalytic reaction is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 王育源蔡建勋蔡启馨
Owner FORMOSAN UNION CHEM CORP
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