Synthesis method of defective zeolite molecular sieve rich in hydroxyl nests

A zeolite molecular sieve, a technology rich in hydroxyl groups, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminum silicate zeolite, etc., to achieve the effect of maintaining integrity

Pending Publication Date: 2021-11-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the more commonly used method is to prepare a zeolite molecular sieve containing defect sites by post-modification method of removing part of the skeleton aluminum or silicon by immersing the molecular sieve matrix in acid / alkaline solution, but how to precisely control The location and size of defect sites without disrupting the topology of the molecular sieve framework is a major challenge in the synthesis of defect-rich molecular sieves

Method used

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  • Synthesis method of defective zeolite molecular sieve rich in hydroxyl nests
  • Synthesis method of defective zeolite molecular sieve rich in hydroxyl nests
  • Synthesis method of defective zeolite molecular sieve rich in hydroxyl nests

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Weigh 0.75gNaOH, 49.8g of sodium silicate (SiO 2 Mass fraction 60%, Na 2 (2 mass fraction 10%) joins 22.5g deionized water, adds 0.36g methyltriethoxysilane and stirs evenly with magnetic stirrer; Then 4.28g aluminum sulfate is completely dissolved in 5g water, slowly adds the concentrated sulfuric acid of 2.25g (98%); The fully dissolved aluminum sulfate solution is slowly dripped into the solution containing sodium silicate, adds 25.9g tetrapropylammonium hydroxide TPAOH, stirs at room temperature for 6 hours, obtains the sol, and the molar composition in the sol is: 18Na 2 O:99.6SiO 2 -Inorg-Si:0.4SiO2 2 -Org-Si:2.5Al 2 o 3 :12SO 4 2- :4000H 2 O: 25.4TPAOH; put the obtained sol into an autoclave lined with polytetrafluoroethylene, control the hydrothermal crystallization temperature of 170°C and the hydrothermal crystallization time of 25 hours; obtain the solid through filtration and dry at 110°C for 8 hours , and roasted at 540°C for 10 hours to obtain a de...

Embodiment 2

[0040] Weigh 0.75gNaOH, 49.25g of sodium silicate (SiO 2 Mass fraction 60%, Na 2 (2 mass fraction 10%) joins 22.5g deionized water, adds 1.34g methyltriethoxysilane and stirs evenly with magnetic stirrer; Then 4.28g aluminum sulfate is completely dissolved in 5g water, slowly adds the concentrated sulfuric acid of 2.25g (98%); The aluminum sulfate solution that dissolves completely is slowly dripped in the solution that contains sodium silicate, adds 30.7g tetrapropyl ammonium hydroxide TPAOH, stirs at room temperature 6 hours, obtains sol, and molar composition is in the sol: 18Na 2 O:98.5SiO 2 -Inorg-Si:1.5SiO2 2 -Org-Si:2.5Al 2 o 3 :12SO 4 2- :4000H 2 O: 30.2TPAOH; put the obtained sol into an autoclave lined with polytetrafluoroethylene, control the hydrothermal crystallization temperature of 170°C and the hydrothermal crystallization time of 25 hours; obtain the solid through filtration and dry at 110°C for 8 hours , and roasted at 540°C for 10 hours to obtain a d...

Embodiment 3

[0042] Weigh 0.75gNaOH, 48.6g of sodium silicate (SiO 2 Mass fraction 60%, Na 2 (2 mass fraction 10%) joins 22.5g deionized water, adds 2.50g methyltriethoxysilane and stirs evenly with magnetic stirrer; Then 4.28g aluminum sulfate is completely dissolved in 5g water, slowly adds the concentrated sulfuric acid of 2.25g (98%); The aluminum sulfate solution that dissolves completely is slowly dripped in the solution that contains sodium silicate, adds 30.7g tetrapropyl ammonium hydroxide TPAOH, stirs at room temperature 6 hours, obtains sol, and molar composition is in the sol: 18Na 2 O:97.2SiO 2 -Inorg-Si:2.8SiO2 2 -Org-Si:2.5Al 2 o 3 :12SO 4 2- :4000H 2 O: 30.2TPAOH; put the obtained sol into an autoclave lined with polytetrafluoroethylene, control the hydrothermal crystallization temperature of 170°C and the hydrothermal crystallization time of 25 hours; obtain the solid through filtration and dry at 110°C for 8 hours , and roasted at 540°C for 10 hours to obtain a de...

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Abstract

The invention provides a synthesis method of a defective zeolite molecular sieve rich in hydroxyl nests. The synthesis method comprises the following steps: mixing an inorganic silicon source and an organic silicon source which serve as a mixed silicon source with an aluminum source and an OSDA template agent to obtain sol, and crystallizing; and filtering, drying and roasting the obtained solid to obtain the defective zeolite molecular sieve rich in hydroxyl nests. The organic silicon source is alkylsiloxane. Alkylsiloxane is introduced in the process of constructing a framework of the molecular sieve, part of Si-C bond connection is formed, then C is burnt out in the roasting process of the molecular sieve, so that a single T-site framework point defect of the molecular sieve is formed, the hydroxyl nests are formed, the point defect almost has no influence on the crystallinity of the material, and the integrity of the molecular sieve framework is maintained to a great extent; and in the synthesis process, the defect degree of the molecular sieve can be relatively accurately controlled by controlling the variety and content of alkylsiloxane, so that the defect type zeolite molecular sieve rich in hydroxyl nests is obtained.

Description

technical field [0001] The invention belongs to the field of aluminosilicate zeolite synthesis, and in particular relates to a method for synthesizing a defective zeolite molecular sieve rich in hydroxyl nests. Background technique [0002] Zeolite molecular sieves are the most widely distributed inorganic microporous materials in nature. Since the Swedish scientist Cronstedt first discovered natural zeolite in 1756, due to its unique molecular sieving ability and good adsorption performance, it has attracted extensive attention from scientific researchers and has gradually been applied in people's actual production and life. Although natural zeolites have the characteristics of various types, wide distribution, large reserves and low cost, they have many impurities and low purity, which limits large-scale industrial applications. Therefore, the artificial synthesis of zeolites has become a new research direction. In the late 1940s, Barrer, an outstanding chemist in the fie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40C01B39/04
CPCC01B39/40C01B39/04C01P2002/72C01P2002/82
Inventor 刘家旭贺宁
Owner DALIAN UNIV OF TECH
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