Preparation method for hierarchical pore low-silicate zeolite

A technology of multi-level pores and silicalite, applied in the direction of crystalline aluminosilicate zeolite, A-type crystalline aluminosilicate zeolite, etc., can solve the problems affecting the use efficiency and range, and achieve easy control of products, increase effective utilization rate, Effect of Reducing Diffusion Resistance

Inactive Publication Date: 2014-10-01
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, like other microporous zeolites, the application of A-type and X-type zeolites is also limited by their micropore mass transfer resistance, which seriously affects their use efficiency and scope.

Method used

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  • Preparation method for hierarchical pore low-silicate zeolite
  • Preparation method for hierarchical pore low-silicate zeolite
  • Preparation method for hierarchical pore low-silicate zeolite

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0023] Take 0.1mol organosilane coupling agent N-[3-(trimethoxysilyl)propyl]aniline, dissolve it in 720ml 70% methanol aqueous solution, add 30g after the dissolution is complete, the pore size is 3.5nm, and the BET surface area is 850m 2 / g of pure silicon MCM-41 powder, in a 1500ml three-necked flask, reflux and stir at 100°C for 8 hours, cool to room temperature, wash with absolute ethanol, centrifuge the solid and liquid, and dry at 100°C to obtain surface silanized pure silicon MCM-41 powder.

[0024] Take 1.48g surface silanized pure silicon MCM-41 powder, 2.3g sodium metaaluminate, 2.48g sodium hydroxide, mix with 30ml deionized water at room temperature, stir vigorously for 3h, put it into a stainless steel reaction kettle, 100 ℃ crystallization 1d. The crystallized product is centrifuged for solid-liquid separation, washed with water at room temperature until neutral, dried in an oven at 100°C, and roasted in air at 500-550°C for 5-6 hours to prepare a multi-level por...

Embodiment 2

[0027] Take 0.15mol organosilane coupling agent dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, dissolve it in 720ml 70% methanol aqueous solution, add 30g pore size 3.5nm after dissolving completely, BET surface area 850m 2 / g of pure silicon MCM-41 powder, in a 1500ml three-necked flask, reflux and stir at 100°C for 8 hours, cool to room temperature, wash with absolute ethanol, centrifuge the solid and liquid, and dry at 100°C to obtain surface silanized pure silicon MCM-41 powder.

[0028] 1.7g of sodium hydroxide, 1.53g of sodium metaaluminate, 20ml of deionized water and 1.5g of silicon dioxide were stirred and mixed uniformly at room temperature, aged at 30°C for 23 hours, and an X-type zeolite directing agent was obtained.

[0029]Take 2.5g of pure silicon MCM-41 powder silanized on the surface, 1.7g of sodium hydroxide, mix well with 20ml of deionized water at room temperature, add 1.53g of sodium metaaluminate, stir for 3 hours, then add 1ml of the abov...

Embodiment 3

[0032] Take 2.5g of pure silicon MCM-41 powder silanized on the surface of Example 2, 1.7g of sodium hydroxide, mix with 20ml of deionized water at room temperature, add 1.53g of sodium metaaluminate, stir for 3h, then add 1ml of Example 2 Prepare the X-type zeolite directing agent, stir at 25°C for 24 hours, put it into a stainless steel tube reactor, crystallize at 65°C for 5 days, centrifuge the crystallized product from solid to liquid, wash it with water at room temperature until it is neutral, and put it in an oven at 100°C Drying and calcining in air at 500-550°C for 5-6 hours will produce multi-order porous X-type zeolite.

[0033] Product N 2 The adsorption-desorption isotherm shows the mesopore characteristics of the product, and the BET specific surface area is 765m 2 / g, of which the specific surface area is 217m 2 / g, the mesopore volume is 0.31mL / g; the aggregate diameter is about 1.0-1.1μm, the nano-flaky grains are 350-400nm long and 50-100nm wide, and the me...

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Abstract

The invention discloses a preparation method for hierarchical pore low-silicate zeolite. The preparation method comprises the following steps: carrying out silanization onto the surface of MCM-41 by utilizing an organic silane coupling agent, and synthesizing A type or X type zeolite with a hierarchical pore structure by one step in a hydrothermal system in a hydrothermal system by taking the MCM-41 as a silicon source, wherein the hierarchical pore A type zeolite morphology is micro-level microspheres, and the X type zeolite is presented as aggregate of nano zeolite crystalline grains. The preparation method disclosed by the invention can be used for preparing the hierarchical pore low-silicate zeolite with large outer surface area and mesoporous pore volume, and porosity and pore diameter of mesopores are easy to regulate and change. Due to existence of hierarchical pores in zeolite, a diffusion path of guest molecules in zeolite crystals can be effectively shortened, diffusion resistance can be lowered, and surface adsorption or availability of catalytic active sites is improved, so that scope of application of the A type and X type zeolite is expanded.

Description

technical field [0001] The invention relates to a preparation method of zeolite, in particular to a preparation method of low-silica zeolite with hierarchical pore structure. Background technique [0002] A-type and X-type zeolites with 1≤Si / Al≤1.5 are typical low-silica zeolites, both of which have a three-dimensional cage structure. Among them, the skeleton Si / Al of A-type zeolite is 1, which is the zeolite with the lowest Si / Al and the largest cation exchange capacity among all zeolites; the Si / Al of X-type zeolite is 1.0-1.5. Due to their high structural stability, large pore volume and surface area, strong surface polarity and the presence of a large number of exchangeable cations, they exhibit strong adsorption properties and ion exchange capabilities, and are used as ion exchangers, adsorbents, molecular sieves and Catalysts are widely used in industrial fields such as hard water softening, sewage treatment, industrial gas or liquid separation and drying. [0003] H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14
Inventor 马静红苗海霞马丽冯春峰李瑞丰
Owner TAIYUAN UNIV OF TECH
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