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Synthesizing method and device for high-silicon zeolite molecular sieve

A zeolite molecular sieve and synthesis device technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem that the shape of the product zeolite cannot be changed, and achieve the effects of convenient calculation, ensuring volatility, and reducing operation difficulty

Inactive Publication Date: 2019-03-08
FUYU ZHANGJIAGANG NEW MATERIALS TECH CO LTD
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Problems solved by technology

[0006] In view of this, the present invention proposes a synthesis method and device for high-silica zeolite molecular sieves, aiming at solving the problem of hydrothermal reaction temperature and time once the reaction mixture has been prepared according to the calculated ratio in the existing high-silica zeolite molecular sieve synthesis process. Determined and started, the shape of the product zeolite has been determined and cannot be changed

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  • Synthesizing method and device for high-silicon zeolite molecular sieve
  • Synthesizing method and device for high-silicon zeolite molecular sieve
  • Synthesizing method and device for high-silicon zeolite molecular sieve

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preparation example Construction

[0040] refer to figure 1 Shown, the synthetic method of the high silica zeolite molecular sieve provided for the embodiment of the present invention, it comprises:

[0041]Reactant preparation: Take appropriate amount of silicon source, aluminum source, template agent, sulfuric acid and deionized water to prepare the preset ratio of reactants according to the preset steps. Among them, the silicon source is industrial water glass (Na 2 O-7.5%; SiO 2 -28%) or silica sol; Aluminum source is aluminum sulfate; Template agent is tetrapropyl ammonium hydroxide (TPAOH) aqueous solution, and the content of preferred tetrapropyl ammonium hydroxide (TPAOH) is 20%; Regulate pH with industrial concentration sulfuric acid.

[0042] Specifically, first weigh aluminum sulfate solid and dissolve it in concentrated sulfuric acid diluted with deionized water to form liquid A; then weigh solid sodium hydroxide and add it to TPAOH solution to mix into liquid B; then slowly pour the liquid B int...

Embodiment 1

[0054] First, according to the preset ratio of reactants Na 2 O:TPA 2 O:SiO 2 :Al 2 o 3 :H 2 0=1.5:1.0:400:1.0:25, take quantitative silicon raw material water glass, aluminum raw material aluminum sulfate, template agent TPAOH solution, sulfuric acid and deionized water and other synthetic raw materials to prepare reactants; then, prepare The reactant is poured into the reaction kettle, the volume filling degree is 80%, and the reaction kettle is heated to 170°C, and the hydrothermal reaction is carried out for 48 hours; finally, the slurry containing the synthetic product zeolite is taken out after the reaction kettle is cooled, and the zeolite in the slurry is removed by filtration. The mother liquor and the solid product are washed with deionized water to PH = 6-8, dried at 120°C, and then placed in a muffle furnace at 600°C for 6-8 hours with air, and the organic matter TPA in the product is burned out and the product is cooled. Exchange with 0.5N hydrochloric acid, ...

Embodiment 2

[0056] First, according to the preset ratio of reactants Na 2 O:TPA 2 O:SiO 2 :Al 2 o 3 :H 2 0=1.5:1.0:400:1.0:25, take quantitative silicon raw material water glass, aluminum raw material aluminum sulfate, template agent TPAOH solution, sulfuric acid and deionized water and other synthetic raw materials to prepare reactants; then, prepare Pour the reactants into the reaction kettle with a volume filling degree of 80%, and heat the reaction kettle to 170°C, then open the high-pressure valve to relieve the pressure for 2 minutes, then close the valve, and conduct a hydrothermal reaction for 36 hours; finally, take out the reaction kettle after cooling The slurry containing the synthetic product zeolite is filtered to remove the mother liquor in the slurry, the solid product is washed with deionized water to PH=6-8, dried at 120°C, and then placed in a muffle furnace at 600°C for 6-8 hours of air roasting , After the organic matter TPA in the product was burned out, the pro...

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Abstract

The invention provides a synthesizing method and a synthesizing device for a high-silicon zeolite molecular sieve. The method comprises the following steps: preparing a reactant, namely, preparing thereactant from suitable amounts of a silicon source, an aluminum source, a template agent, sulphuric acid and deionized water according to a preset proportion; preparing a zeolite product, namely, placing the reactant into a synthesizing device to perform a hydrothermal reaction, when the temperature is raised to the preset hydrothermal reaction temperature, releasing a preset amount of a volatilecomponent outwards from the reactant through the synthesizing device, so that the proportion of the reactant changes to form the zeolite product with a preset morphology; and preparing the molecularsieve, namely, treating the zeolite product to obtain the zeolite molecular sieve after the zeolite molecular sieve is cooled. According to the synthesizing method and the synthesizing device for thehigh-silicon zeolite molecular sieve, the proportion of the reactant in the hydrothermal reaction process is changed controllably by a method of releasing volatile organic or inorganic components outwards from the reactant in the hydrothermal reaction process, so that the various zeolite products with different morphologies can be synthesized without changing the original proportion of the reactant.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method and device for synthesizing high silica zeolite molecular sieves. Background technique [0002] At present, the shape-selective separation and catalytic properties of zeolite molecular sieves are the most important characteristics for their wide application in chemical-related industrial and scientific fields. For a certain catalytic reaction process, usually only 1-2 zeolites with specific structure types are suitable for use as industrial catalysts. It was found that the reaction selectivity of the catalyst was closely related to the crystal morphology of the selected zeolite. For example, the yield of dienes (ethylene and propylene) of flake-shaped ZSM-5 in the catalytic reaction of methanol dehydration to olefins can reach 60%, and the ratio of propylene / ethylene is 8.4 (Journal of Fuel Chemistry 2015 43(6), P747-753) . Another example is the hexagonal ...

Claims

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Application Information

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IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03
Inventor 龙英才
Owner FUYU ZHANGJIAGANG NEW MATERIALS TECH CO LTD
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