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Preparation method of nano layered clinoptilolite molecular sieve

A clinoptilolite and nano-layered technology is applied in the field of preparation of zeolite molecular sieve materials and can solve the problems of low crystallinity and the like

Active Publication Date: 2019-04-16
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Sanders (US 4623529A[P].1986.) also used natural clinoptilolite as the seed crystal (the addition amount is 1-12wt%), it needs to be crystallized at 135-140°C for 75h-100h to synthesize Na-clinoptilolite Portilolite with low crystallinity (30-70%)

Method used

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  • Preparation method of nano layered clinoptilolite molecular sieve
  • Preparation method of nano layered clinoptilolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 0.7362g of aluminum hydroxide, 0.5192g of sodium hydroxide and 0.7268g of potassium hydroxide into 25ml of deionized water, stir at 150°C for 2h until it becomes clear, then add 8.8ml of silica sol, stir well to obtain solution I .

[0023] (2) Mix and stir 0.7362g aluminum hydroxide, 0.5192g sodium hydroxide, 0.7268g potassium hydroxide, 8.8ml silica sol and 25ml deionized water for 30 minutes, then stir and age at 150°C for 60h, and cool to room temperature The solution II obtained by filtration is used as a structure promoter for future use.

[0024] (3) Add 3ml of solution II into solution I, and stir well to obtain a uniform sol. The above sol was transferred into a high-pressure reactor and crystallized at 150°C for 48h.

[0025] (4) Take the kettle, cool it to room temperature, filter and wash the crystallized product with 80% ethanol solution, and dry it at 150° C. for 12 hours to obtain nano-layered clinoptilolite molecular sieve.

[0026] (5) X-ray ...

Embodiment 2

[0028] (1) The preparation of solution I is as in Example 1.

[0029] (2) Mix and stir 3.681g aluminum hydroxide, 2.596g sodium hydroxide, 3.634g potassium hydroxide, 44ml silica sol and 125ml deionized water for 30 minutes, then stir and age at 150°C for 6h, cool to room temperature and filter Solution II is obtained as a structure promoter for later use.

[0030] (3) Add 1ml of solution II into solution I and stir well to obtain a uniform sol. The above sol was transferred into a high-pressure reactor, and crystallized at 180° C. for 24 hours.

[0031] (4) Take the kettle, cool to room temperature, filter and wash the crystallized product with ethanol solution with a mass fraction of 50%, and dry at 150° C. for 12 hours to obtain nano-layered clinoptilolite molecular sieve.

Embodiment 3

[0033] (1) Add 0.4813g of alumina, 0.5192g of sodium hydroxide and 0.7268g of potassium hydroxide into 25ml of deionized water, stir at 120°C for 3h until clear, then add 10.56g of white carbon black, stir well to obtain solution I .

[0034] (2) Mix and stir 0.4813g alumina, 0.5192g sodium hydroxide, 0.7268g potassium hydroxide, 10.56g white carbon black and 25ml deionized water for 40 minutes, then stir and age at 150°C for 60h, and cool to room temperature The solution II obtained by filtration is used as a structure promoter for future use.

[0035] (3) Add 6ml of solution II into solution I, and stir well to obtain a uniform sol. The above sol was transferred into an autoclave for crystallization at 180°C for 15 hours.

[0036] (4) Take the kettle, cool to room temperature, filter and wash the crystallized product with ethanol solution with a mass fraction of 60%, and dry at 200°C for 10 hours to obtain nano-layered clinoptilolite molecular sieve.

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Abstract

The invention provides a preparation method of a nano layered clinoptilolite molecular sieve. The method comprises the following steps that firstly, sodium hydroxide or a mixture of sodium hydroxide and potassium hydroxide is mixed with a silicone source, an aluminium source and water, stirring and crystallization are conducted for a certain time period, and then filtering is conducted to obtain asolution II; or the prepared nano layered clinoptilolite molecular sieve is completely dissolved in sodium hydroxide or a mixed solution of sodium hydroxide and potassium hydroxide to obtain a solution III; then, the solution II or the solution III is used as a structure accelerant and added to a synthesis system formed by different silicone sources, sodium hydroxide or the mixture of sodium hydroxide and potassium hydroxide, the aluminium source and the water, crystallization is conducted for 10-96 hours at 80-200 DEG C, cooling is conducted to the room temperature, and through solid-liquidseparation, washing and drying, the nano layered clinoptilolite molecular sieve is obtained. According to the preparation method, the structure accelerant is added, which helps to shorten the crystallization time and lower the crystallization temperature; the obtained nano layered clinoptilolite molecular sieve has the advantages of being high in relative crystallinity, small in grain size and thelike.

Description

technical field [0001] The invention belongs to the technical field of preparation of zeolite molecular sieve materials, in particular to a preparation method of nano-layered clinoptilolite molecular sieves. Background technique [0002] The invention belongs to the field of inorganic synthetic micro-materials, in particular to a method for synthesizing nano-layered clinoptilolite molecular sieves by a structure accelerator method. [0003] The nano-layered clinoptilolite molecular sieve has a ten-membered ring and an eight-membered ring intersection structure, and its skeleton is composed of silicon, aluminum, oxygen and other elements, and the pore sizes are 0.75×0.31nm, 0.46×0.36nm and 0.47×0.28nm respectively. The unique pore structure, strong ion exchange performance and high adsorption capacity make it show broad application prospects in the fields of gas separation, wastewater treatment and soil improvement, and industrial catalysis. There are mainly heulandite and c...

Claims

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Application Information

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IPC IPC(8): C01B39/02B82Y40/00
CPCB82Y40/00C01B39/02C01P2004/03C01P2002/72C01P2002/20Y02P20/52
Inventor 孙继红马佳宇白诗扬翟承伟李晶
Owner BEIJING UNIV OF TECH
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