Rapid synthesis method for small-crystal-grain molecular sieves and application of small-crystal-grain molecular sieves

A synthesis method and molecular sieve technology are applied in molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, crystalline aluminosilicate zeolite, etc., and can solve problems such as unfavorable industrial application, unfavorable industrial production, and increasing crystallization cycle. , to achieve the effect of shortening crystallization time, small grain size and improving production efficiency

Active Publication Date: 2019-05-03
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Increasing the number and concentration of crystal nuclei in the system has a certain effect on reducing the particle size, but this effect has a certain limit, that is, after reaching a certain minimum value, if the crystal nucleus continues to increase, the particle size will not continue to decrease; adjust the crystallization process The effect on reducing particle size is consistent with increasing the number (concentration) of crystal nuclei in the system, and crystallization requires a longer nucleation period at low temperature, which greatly increases the entire crystallization cycle; adding some special templates has a greater Cost disadvantages are not conducive to industrial production; microwave / ultrasonic is also not conducive to industrial applications due to limitations on equipment

Method used

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  • Rapid synthesis method for small-crystal-grain molecular sieves and application of small-crystal-grain molecular sieves
  • Rapid synthesis method for small-crystal-grain molecular sieves and application of small-crystal-grain molecular sieves
  • Rapid synthesis method for small-crystal-grain molecular sieves and application of small-crystal-grain molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A quantitative amount of pseudo-boehmite was taken and dried at 150° C. for 12 hours. Then slowly add it into the n-butylamine (R-1) template solution, and stir rapidly until the aluminum source is completely dissolved to obtain a mixed solution. The mixed solution was transferred to a crystallization kettle, and crystallized at 120° C. for 3 hours to obtain a precursor mixed solution. The molar ratio of effective components in the precursor mixture is as follows: R-1: Al 2 o 3 =10:1.

[0029] Add pseudo-boehmite, caustic soda, n-butylamine (R-1), and silica sol to deionized water in sequence, stir evenly, add precursor mixed solution, and form a gel after fully stirring. The molar ratio of each component in the gel is as follows: H 2 O: Al 2 o 3 :SiO2 2 :R-1:Na 2 O=20:0.025:1:0.25:0.12. The gel was transferred to a crystallization kettle, and crystallized at 170° C. for 12 hours to obtain a molecular sieve slurry. The slurry is separated from the mother liquo...

Embodiment 2

[0031] Take a quantitative amount of solid sodium metaaluminate and dry it at 150°C for 12 hours. Then slowly add it into the triethylamine (R-1) template solution, and stir rapidly until the aluminum source is completely dissolved to obtain a mixed solution. The mixed solution was transferred to a crystallization kettle, and crystallized at 140° C. for 8 hours to obtain a precursor mixed solution. The molar ratio of effective components in the precursor mixture is as follows: R-1: Al 2 o 3 =30:1.

[0032] Add solid sodium metaaluminate, liquid caustic soda, triethylamine (R-1), N,N,N,-trimethyl-1-adamantyl ammonium hydroxide (R-2), and silica gel to the deionized In water, stir evenly, add the precursor mixture, and form a gel after fully stirring. The molar ratio of each component in the gel is as follows: H 2 O: Al 2 o 3 :SiO2 2 :R-1:R-2:Na 2 O=20:0.033:1:1:0.02:0.26. The gel was transferred to a crystallization kettle, and crystallized at 150° C. for 24 hours to ...

Embodiment 3

[0034] Take a certain amount of solid aluminum hydroxide and dry it at 150°C for 12 hours. Then slowly add it into the isopropylamine (R-1) template solution, and stir rapidly until the aluminum source is completely dissolved to obtain a mixed solution. The mixed solution was transferred to a crystallization kettle, and crystallized at 100° C. for 6 hours to obtain a precursor mixed solution. The molar ratio of effective components in the precursor mixture is as follows: R-1: Al 2 o 3 =40:1.

[0035] Add solid aluminum hydroxide, liquid caustic soda, isopropylamine (R-1), n-propylamine (R-2), and silica sol to deionized water in sequence, stir evenly, add precursor mixture, and form a gel after fully stirring. The molar ratio of each component in the gel is as follows: H 2 O: Al 2 o 3 :SiO2 2 :R-1:R-2:Na 2 O=30:0.01:1:0.4:0.3:0.04. The gel was transferred to a crystallization kettle, and crystallized at 160° C. for 24 hours to obtain a molecular sieve slurry. The slurr...

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Abstract

The invention belongs to the field of preparation of molecular sieves and particularly relates to a rapid synthesis method for small-crystal-grain molecular sieves and an application of the small-crystal-grain molecular sieves. The rapid synthesis of the small-crystal-grain molecular sieves is achieved through the procedures of firstly, preparing a precursor mixture, then, preparing gel and finally carrying out direct crystallization. The method is applied to the synthesis of the following molecular sieves, but not limited to: ZSM-5, ZSM-11, ZSM-22, ZSM-23, ZSM-35, SAPO-34, SAPO-11, SAPO-18, SSZ-13 and EU-1. Molecular sieve products synthesized by the method have the characteristics of small crystal grain, large specific surface area, high crystallinity and high yield. According to the method, the crystallization time can be shortened greatly, the production efficiency is increased, and the manufacturing cost of the molecular sieves is reduced.

Description

technical field [0001] The invention belongs to the field of molecular sieve preparation, and in particular relates to a rapid synthesis method and application of a small-grain molecular sieve. Background technique [0002] Small-grained molecular sieves have the characteristics of high specific surface area and short diffusion channels. In the catalytic reaction, the higher specific surface area can make the reactants fully contact with the active sites of the catalyst, and the reaction activity is high. When loading other metal ions, it can facilitate the ions to form a highly dispersed state, which is conducive to improving the overall activity of the catalyst. In terms of reaction diffusion, small-grain molecular sieves have shorter pores, which have smaller diffusion resistance in catalytic reactions, reduce the occurrence of side reactions, and greatly improve product selectivity. Conventional methods to control the grain size of molecular sieves are mainly to contro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08C01B39/44C01B39/36
Inventor 王龙陈文勇刘环昌彭立周泳冰徐辰
Owner SHANDONG QILU HUAXIN HIGH TECH
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