Large block porous zeolite composed of nano-crystal grains and preparation method thereof

A porous zeolite, nanocrystalline technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., to achieve good thermal and hydrothermal stability, diffusion rate and acid site accessibility improved effect

Inactive Publication Date: 2015-10-28
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the method of preparing single nano-zeolite polycrystalline aggregates by steam phase inversion method.

Method used

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  • Large block porous zeolite composed of nano-crystal grains and preparation method thereof
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  • Large block porous zeolite composed of nano-crystal grains and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At room temperature, dissolve 5.31g of sodium chloride, 5.30g of tetrapropylammonium bromide (TPABr), and 1.13g of sodium aluminate in 60mL of distilled water to form a clear and transparent solution, then add 1.70g of 98% concentrated sulfuric acid dropwise, and stir well , slowly add 76.00g of 40% silica sol, then add 4.08g of sodium hydroxide, and continue to stir evenly.

[0030] Heat the above gel and keep the temperature at 80°C, add 2.00g of sodium carboxymethylcellulose, continue to stir for 180min, and dry until there is no obvious weight loss to make a block dry gel.

[0031] Place a bracket at the bottom of the stainless steel reaction kettle, place a container with a hole in the bottom on the upper layer of the bracket, weigh 5.00g of the above block dry glue, wrap it with filter paper and put it on the container with holes. Inject 3.00g of ethylenediamine, a gas template in the vapor phase inversion process, into the bottom of the reactor, seal it, and crys...

Embodiment 2

[0033] At room temperature, dissolve 10.00g of sodium chloride, 5.30g of tetrapropylammonium bromide (TPABr), and 1.13g of sodium aluminate in 40mL of distilled water to form a clear and transparent solution, then add 1.25g of 98% concentrated sulfuric acid dropwise, and stir well , slowly add 89.00g of 40% silica sol, then add 8.00g of sodium hydroxide, and continue to stir evenly.

[0034] Heat the above gel and keep the temperature at 75°C, add 1.50g of sodium hydroxyethyl cellulose, continue to stir for 120min, and dry until there is no obvious weight loss to make a block dry gel.

[0035]Place a bracket at the bottom of the stainless steel reaction kettle, place a container with a hole in the bottom on the upper layer of the bracket, weigh 6.00g of the above-mentioned block dry glue, wrap it with filter paper and put it on the container with holes. Inject 5.00 g of the mixed solution of ethylenediamine and diethylamine, the gas template in the vapor phase inversion proces...

Embodiment 3

[0038] At room temperature, dissolve 6.50g of sodium chloride, 6.89g of tetrapropylammonium bromide (TPABr), and 1.13g of sodium aluminate in 40mL of distilled water to form a clear and transparent solution, then add 1.00g of 98% concentrated sulfuric acid dropwise, and stir well , slowly add 25.00g of 40% silica sol, then add 1.00g of sodium hydroxide, and continue to stir evenly.

[0039] Heat the above gel and keep the temperature at 60°C, add 0.50 g of sodium carboxymethylcellulose, continue to stir for 30 min, and dry until there is no obvious weight loss to make a block dry gel.

[0040] Place a bracket at the bottom of the stainless steel reaction kettle, place a container with a hole in the bottom on the upper layer of the bracket, weigh 2.00g of the above-mentioned block dry glue, wrap it with filter paper and put it on the container with holes. Inject 2.00 g of the mixed solution of diethylamine and triethylamine as the gas template in the vapor phase inversion proce...

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Abstract

The invention discloses a large block porous zeolite composed of nano-crystal grains and a preparation method thereof. The preparation method includes: taking a silicon source, an aluminum source, an alkali source, a quaternary ammonium salt template agent and sodium chloride as the raw materials to prepare gel, adding a crystal growth interference agent to prepare a blocky dry glue; subjecting the blocky dry glue and a gas template agent not in direct contact to vapor phase crystallization reaction so as to obtain the large block porous zeolite that is composed of 50-500nm primary zeolite crystal grains and has a 2-50nm intergranular mesoporous system. The porous zeolite synthesized by the method provided by the invention has improved diffusion rate and acid site accessibility, and has important application value in catalytic cracking, hydrocracking, adsorption separation and other aspects of fine chemical engineering and petrochemical engineering.

Description

technical field [0001] The invention relates to a zeolite molecular sieve, in particular to a monolithic porous zeolite material prepared by a vapor phase inversion method. The invention also relates to a method for the preparation of said porous zeolite material. Background technique [0002] Zeolite is widely used as solid acid catalyst and adsorption separation material due to its unique and regular pore structure, adjustable acidity and good hydrothermal stability. However, the narrow pore structure limits its application in the catalysis and separation of macromolecular reactants. [0003] In recent decades, researchers have spent considerable energy to synthesize nano-sized zeolite crystals in order to improve the diffusion effect and acid site accessibility of zeolite, and improve the catalytic performance of catalysts. Smaller crystal grains will lead to more pore entrances per unit weight of the zeolite catalyst, improving the accessibility of the acid site of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
Inventor 刘芝平崔杏雨郑家军陈晓芳李瑞丰潘梦李彪张球张鸿雁
Owner TAIYUAN UNIV OF TECH
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