Method for preparing multi-stage pore Y molecular sieve through H4EDTA-NaOH co-treatment

A molecular sieve and multi-stage pore technology, applied in the field of molecular sieves, can solve the problems of insufficient mesopore volume and small mesopore specific surface area, and achieve the effects of reducing total acid content, L acid content, and crystallinity

Inactive Publication Date: 2019-07-30
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the multi-order pore Y molecular sieve prepared by the prior art has problems such as too small mesopore specific surface area and insufficient mesopore volume.

Method used

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  • Method for preparing multi-stage pore Y molecular sieve through H4EDTA-NaOH co-treatment
  • Method for preparing multi-stage pore Y molecular sieve through H4EDTA-NaOH co-treatment
  • Method for preparing multi-stage pore Y molecular sieve through H4EDTA-NaOH co-treatment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: H 4 Method for preparing hierarchically porous Y molecular sieves by co-processing EDTA-NaOH (1)H 4 EDTA solution acid treatment: 100ml of distilled water and H 4 EDTA was added into a three-necked flask to form 0.11mol / L of H 4 EDTA aqueous solution, weigh 6.8g of NaY molecular sieves. Heat the three-neck flask in silicone oil. When the temperature rises to 80°C, add NaY molecular sieve, reflux and stir for 6 hours, and then filter with suction. Filter the solution with hot distilled water until pH = 7. Put the obtained solid molecular sieve in Dry in an oven at 120°C for 6h, and bake in a muffle furnace at 500°C for 6h.

[0018] (2) NaOH solution alkali treatment: use deionized water to configure NaOH solution with a concentration of 0.4mol / L, put the acid-treated sample into a three-necked flask, and add NaOH solution according to the ratio of 1g sample to 25ml NaOH solution, Under the condition of water bath at 65°C, stir for 30min; cool down the solu...

Embodiment 2

[0020] Example 2: H 4 Method for preparing hierarchically porous Y molecular sieves by co-processing EDTA-NaOH

[0021] (1)H 4 EDTA solution acid treatment: 100ml of distilled water and H 4 EDTA was added into a three-necked flask to form 0.17mol / L of H 4 EDTA aqueous solution, weigh 6.8g of NaY molecular sieves. Heat the three-necked flask in silicone oil. When the temperature rises to 65°C, add NaY molecular sieve, reflux and stir for 6 hours, and then filter with suction. Filter the solution with hot distilled water until pH = 7. Put the obtained solid molecular sieve in Dry in an oven at 120°C for 6h, and bake in a muffle furnace at 500°C for 6h.

[0022] (2) NaOH solution alkali treatment: use deionized water to configure NaOH solution with a concentration of 0.8mol / L, put the acid-treated sample into a three-necked flask, and add NaOH solution according to the ratio of 1g sample to 25ml NaOH solution, Under the condition of water bath at 80°C, stir for 30min; cool d...

Embodiment 3

[0024] Example 3: H 4 Method for preparing hierarchically porous Y molecular sieves by co-processing EDTA-NaOH (1)H 4 EDTA solution acid treatment: 100ml of distilled water and H 4 EDTA was added into a three-necked flask to form 0.14mol / L of H 4 EDTA aqueous solution, weigh 6.8g of NaY molecular sieves. Heat the three-necked flask in silicone oil. When the temperature rises to 65°C, add NaY molecular sieve, reflux and stir for 6 hours, and then filter with suction. Filter the solution with hot distilled water until pH = 7. Put the obtained solid molecular sieve in Dry in an oven at 120°C for 6h, and bake in a muffle furnace at 500°C for 6h.

[0025] (2) NaOH solution alkali treatment: use deionized water to configure NaOH solution with a concentration of 0.4mol / L, put the acid-treated sample into a three-necked flask, and add NaOH solution according to the ratio of 1g sample to 25ml NaOH solution, Under the condition of water bath at 95°C, stir for 30min; cool down the so...

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Abstract

The invention discloses a method for preparing a multi-stage pore Y molecular sieve through H4EDTA-NaOH co-treatment, which comprises the following steps: (1) acid treatment of H4EDTA solution, namelyadding a NaY molecular sieve into H4EDTA aqueous solution to obtain an acid treatment sample; (2) NaOH solution alkali treatment: mixing the NaOH solution with the acid treatment sample in step (1) to obtain an alkali treatment sample; (3) Na2H2EDTA solution acid treatment: adding the Na2H2EDTA solution into the alkali treatment sample. The mesoporous specific surface area of the NaY molecular sieve can be increased by 200%, and the mesoporous pore volume can be increased by 849%. Meanwhile, the specific surface area of the micropores is reduced by only 36%, the volume of the micropores is reduced by only 5%, and the average pore diameter of the molecular sieve is 10.1 nm. The NaY molecular sieve has the advantages of the best pore system for the step distribution of mesopores-micropores.Meanwhile, the crystallinity of the molecular sieve modified by acid and alkali is reduced, and the total acid content is slightly reduced. Comparing the acid distribution of the molecular sieves before and after the modification, the acid content of the modified sample B is increased, and the L acid content is decreased.

Description

technical field [0001] The invention relates to the technical field of molecular sieves, in particular to a preparation technology of multi-level porous Y molecular sieves. Background technique [0002] The pore size of microporous zeolite is small, the distribution is too wide, and the opening is not enough, which seriously affects the diffusion of larger heavy oil molecules and their intermediate products, resulting in the difficulty of mass transfer in catalytic reactions, which requires the development of new catalytic materials. Ordered mesoporous materials attracted people's attention in 1992. It has large pore size, pore volume, high specific surface area and highly ordered pore structure, which makes it prominent in catalytic reactions involving macromolecules. Excellent catalytic performance, but in practical applications, mesoporous materials have poor hydrothermal stability and lower catalytic activity than microporous zeolites, which seriously restricts their app...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
CPCC01B39/24C01P2006/12C01P2006/14
Inventor 段林海孟秀红程丽华林存辉张尤华曹水秦慧博
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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