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Mesoporous material/micropore molecular sieve composite material and preparation method thereof

A technology of microporous molecular sieve and mesoporous material, applied in the field of mesoporous material/microporous molecular sieve composite material and its preparation, can solve the problem of mechanical stability, poor thermal and hydrothermal stability, no repeating unit cell structural unit, mesoporous Molecular sieve still needs time and other problems to achieve the effect of good stability, improved hydrothermal stability and strong acidity

Active Publication Date: 2008-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with traditional microporous molecular sieves, this type of mesoporous molecular sieve is more suitable for the reaction of larger molecular compounds in terms of pore structure, but there are obvious disadvantages in the skeleton structure: no repeating unit cell structure unit, no crystal structure region, Only locally ordered structures exist
Therefore, mesoporous molecular sieves are similar to amorphous aluminosilicates, have weak acidity, and poor mechanical, thermal and hydrothermal stability, which limits their application in hydrocarbon processing.
Therefore, many studies have improved their mechanical stability, thermal and hydrothermal stability by improving synthetic conditions, but from the existing reports, it will take time to overcome the above-mentioned shortcomings of mesoporous molecular sieves.

Method used

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  • Mesoporous material/micropore molecular sieve composite material and preparation method thereof
  • Mesoporous material/micropore molecular sieve composite material and preparation method thereof
  • Mesoporous material/micropore molecular sieve composite material and preparation method thereof

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preparation example Construction

[0027] (1) Preparation of PCHs

[0028] Firstly, acid clay or organoclay is prepared, which can be obtained by modifying layered clay, and the modification methods mentioned are common techniques in the art.

[0029] The acid modification method is as follows: layered clay, ammonium salt (or acid) and deionized water are made into a slurry at a weight ratio of 1: (0.1-0.6): (5-20), and stirred at room temperature to 95°C 0.5 to 24 hours, separated, washed, and dried at room temperature to 150°C. Among them, ammonium salts include NH 4 Cl, NH 4 NO 3 and (NH 4 ) 2 SO 4 etc. Acids include hydrochloric acid, sulfuric acid and nitric acid, etc.; if ammonium salt is added, it needs to be roasted at 300-700°C for 1-5 hours.

[0030] The organic modification method is as follows: layered clay, quaternary ammonium salt and deionized water are made into a slurry at a weight ratio of 1: (0.1-0.6): (5-20), and stirred at room temperature to 95°C for 0.5- After 24 hours, separate, ...

Embodiment 1

[0042] This embodiment prepares organic montmorillonite:

[0043] (1) Flotation: Take 40g of natural calcium-based montmorillonite, add 360mL of deionized water, stir at room temperature for 5 hours, settle for 2 hours, take the upper liquid, add flocculant, separate the refined calcium-based montmorillonite, Dry at 110°C for 24 hours.

[0044] (2) Sodiumization: Weigh 20g of refined calcium-based montmorillonite after flotation, add 800mL of deionized water to make a slurry, then add 8g of NaCl, stir mechanically at 60°C for 4 hours, and separate the sodium-based montmorillonite Soil, dry at room temperature to 150°C for 24 hours.

[0045] (3) Organic modification: take 10g of sodium montmorillonite, add 400mL of deionized water, add 4g of cetyltrimethylammonium bromide, stir at 60°C for 5 hours, separate, and then wash until the filtrate is free of Cl - Until (tested with silver nitrate), dry at room temperature to 150°C for 24 hours to obtain organic montmorillonite.

Embodiment 2

[0047] The present embodiment prepares acid montmorillonite:

[0048] Get 10g of refined calcium-based montmorillonite floated by step (1) in Example 1, add 400mL of deionized water, add 5mL of hydrochloric acid with a concentration of 36% (mass fraction), stir at room temperature for 5 hours, and separate the solid and liquid , and then washed until the filtrate was free of Cl - Until (tested with silver nitrate), dry at room temperature to 150°C for 24 hours to obtain acidic montmorillonite.

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Abstract

The invention provides a mesoporous material / microporous molecular sieve composite material and a preparation method thereof. The composite was prepared by in situ crystallization of porous clay heterogeneous materials (PCHs) mixed with microporous molecular sieve gels. In the composite material prepared by the invention, the microporous molecular sieve is wrapped around the porous clay heterogeneous material. The composite material has both the crystal structure of microporous molecular sieves and the mesoporous structure of porous clay heterogeneous materials, and has high mechanical stability, thermal and hydrothermal stability, and is superior to existing mesoporous molecular sieve / microporous molecular sieve composite materials. There are broader application prospects.

Description

technical field [0001] The invention relates to a composite catalytic material and a preparation method thereof, in particular to a mesoporous material / microporous molecular sieve composite material and a preparation method thereof. technical background [0002] At present, the materials used for heterogeneous catalysis mainly include two types according to the pore size: one is microporous materials (the pore size is generally less than 2.0 nm), and the other is the mesoporous material (the pore size is generally between 2.0 and 50 nm). Microporous materials are mainly microporous molecular sieves. Microporous molecular sieves generally have strong acid properties and unique pore, cage structure and stable skeleton structure. The reactant molecules diffuse, adsorb, and undergo catalytic conversion in the inner pores of the molecular sieve. However, due to the small pores of most microporous molecular sieves, it is difficult for the macromolecules in the reaction raw materi...

Claims

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Application Information

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IPC IPC(8): B01J29/06B01J21/16C01B39/46C01B39/04
Inventor 张喜文李瑞丰方向晨马静红张志智凌凤香孙万付
Owner CHINA PETROLEUM & CHEM CORP
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