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A kind of preparation method of small grain nay molecular sieve

A small-grain, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the lack of systematic research on the phase state and dispersion of materials, low synthesis efficiency of small-grain molecular sieves, and dispersion Solve problems such as complex preparation process, achieve the effects of reducing production cost and organic pollutant discharge, high crystallinity, improving utilization rate and product yield

Active Publication Date: 2018-04-20
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the research on the preparation of small-grain NaY molecular sieves is limited to the two directions of feeding ratio and preparation process, and there is a lack of systematic research on the material phase and dispersion of the molecular sieve gelation process; at the same time, the preparation of dispersants added in the synthesis Complex process and high production cost lead to low synthesis efficiency and high production cost of small crystal molecular sieves

Method used

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  • A kind of preparation method of small grain nay molecular sieve
  • A kind of preparation method of small grain nay molecular sieve
  • A kind of preparation method of small grain nay molecular sieve

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Embodiment 1

[0035] At 80°C, 8.8g of sodium metaaluminate (Al 2 o 3 The content is 41wt%, Na 2 O content is 28.7%) is dissolved in 60g deionized water, adds 42g sodium hydroxide (purity 96%) under mechanical stirring, continues stirring, makes it dissolve completely, obtains high alkalinity sodium metaaluminate solution. Under stirring, the above-mentioned high alkalinity sodium metaaluminate solution is added to 204g water glass (SiO 2 The content is 26.2wt%, Na 2 O content is 8.3%), after mixing evenly, continue to stir for 2 hours, and then stand and age at 15° C. for 24 hours to prepare the directing agent.

[0036] Dissolve 10.8g of sodium metaaluminate in 72g of deionized water at 80°C, add 36g of sodium hydroxide under mechanical stirring, and continue stirring to completely dissolve it to obtain a low-alkalinity sodium metaaluminate solution. In a stirring state, the gelling temperature is 20°C, pour the prepared directing agent into 486g of water glass, mix well, and then add ...

Embodiment 2

[0038] Each raw material source is with embodiment 1.

[0039]Dissolve 15g of sodium metaaluminate in 35g of deionized water at 80°C, add 52g of sodium hydroxide under mechanical stirring, and continue stirring to completely dissolve it to obtain a high-basicity sodium metaaluminate solution. In a stirring state, the above-mentioned high-basicity sodium metaaluminate solution was added to 52 g of water glass, mixed evenly and then stirred for 2 hours, and then aged at 20° C. for 36 hours to prepare a directing agent.

[0040] Dissolve 9.3g of sodium metaaluminate in 60g of deionized water at 80°C, add 18g of sodium hydroxide under mechanical stirring, and continue stirring to completely dissolve it to obtain a low-alkalinity sodium metaaluminate solution. Under the stirring state, the gelling temperature is 30°C, pour the prepared directing agent into 412g of water glass, mix well, then add 216g of aluminum sulfate solution, the above-mentioned low-alkalinity sodium metaalumin...

Embodiment 3

[0042] Each raw material source is with embodiment 1.

[0043] Dissolve 21g of sodium metaaluminate in 25g of deionized water at 80°C, add 26g of sodium hydroxide under mechanical stirring, and continue stirring to completely dissolve it to obtain a high-basicity sodium metaaluminate solution. In the stirring state, the above-mentioned high alkalinity sodium metaaluminate solution was added into 188g of water glass, after mixing evenly, the stirring was continued for 2 hours, and then aged at 5°C for 60 hours to prepare the directing agent.

[0044] Dissolve 5.8g of sodium metaaluminate in 56g of deionized water at 80°C, add 40g of sodium hydroxide under mechanical stirring, and continue stirring to completely dissolve it to obtain a low-alkalinity sodium metaaluminate solution. Under the stirring state, the gelling temperature is 40°C, pour the prepared directing agent into 404g of water glass, mix well, then add 195g of aluminum sulfate solution, the above-mentioned low-alka...

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Abstract

The invention discloses a preparation method of a small-crystal-particle NaY molecular sieve. Hexamethylenetetramine is used as an additive, and the small-crystal-particle NaY molecular sieve is prepared in a segmental crystallization method. The method comprises the following steps: mixing a silicon source and an aluminum source, standing and aging for 2 to 72 hours at 5 to 60 DEG C to obtain a guide agent; then mixing the silicon source, the guide agent, the aluminum source and the hexamethylenetetramine to form cement, wherein in the reaction mixture gel, the molar ratio of Na2O, Al2O3, SiO2, H2O and C6H12N4 is (0.5-1):1:(5-40):(80-800):(0.5-10); static crystallizing in two segments under different temperatures, wherein the first-segment crystallization temperature is 60 to 85 DEG C, crystallizing for 12 to 48 hours, the second-segment crystallization temperature is 90 to 120 DEG C, and crystallizing for 12 to 72 hours; and finally filtering, washing and drying to obtain the small crystal-particle NaY molecular sieve. The relative crystallinity of the prepared composite molecular sieve is greater than 85 percent, and the size of a crystal size is 400nm to 600nm. The preparation method is easy for obtaining raw materials, low in preparation cost and good in industrial application prospect.

Description

technical field [0001] The invention belongs to the field of molecular sieve materials and preparation thereof, and in particular relates to a method for preparing small-grain NaY molecular sieves through segmental crystallization by using hexamethylenetetramine as a dispersant. technical background [0002] Y-type molecular sieve is the main active component of various petrochemical catalysts, and its pore structure, acidity and stability are important factors affecting catalytic performance and product distribution. In recent years, the oil refining industry has generally faced the problem of heavy feedstock oil, so it is particularly important to improve the accessibility of the active centers of oil refining catalysts and improve their ability to crack macromolecules. With the continuous development of new synthetic processes for molecular sieve materials, molecular sieves with small grains or nanoscale have become the focus of research and development of new petrochemic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24
Inventor 王凌涛刘冠锋于海斌王绍增洪美花臧甲忠王海强洪鲁伟李孝国马明超
Owner CNOOC TIANJIN CHEM RES & DESIGN INST