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Preparation method of mesoporous-microporous composite molecular sieve

A composite molecular sieve and microporous molecular sieve technology, which is applied in the field of preparation of mesoporous-microporous composite molecular sieves, can solve the problems of inconspicuous mesoporous structure of composite molecular sieves, channel blockage, channel collapse, etc., so as to improve hydrothermal and thermal stability. , The effect of improving the ratio of silicon to aluminum and high crystallinity

Active Publication Date: 2013-05-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis process uses two crystallizations, which is costly, and the mesoporous structure of the synthesized composite molecular sieve is not obvious, and the channels may be blocked during the two crystallization processes or cause the channels to collapse after the two crystallizations

Method used

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  • Preparation method of mesoporous-microporous composite molecular sieve
  • Preparation method of mesoporous-microporous composite molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Preparation of composite molecular sieve F-1:

[0028] (1) Add 200g tetraethyl orthosilicate to the HCl solution with a concentration of 0.28mol / L, and stir at 35°C for about 3 hours until it becomes a transparent solution;

[0029] (2) Dissolve 100g of diethanolamine in water, maintain the pH value at 3, and stir at 40°C for 2 hours to obtain a mixed solution containing cationic surfactant;

[0030] (3) Take 60g molecular sieve Y-1 (specific surface area 794 m 2 / g, pore volume 0.39 mL / g, average pore diameter 1.76nm, relative crystallinity 97%, acid content 0.632 mmol / g) was put into a hydrothermal furnace to react for 2 hours at 550°C and 2MPa pressure, and then taken out;

[0031] (4) Add the solution obtained in step (1) to the mixed solution obtained in step (2), stir at 40°C for 24 hours, then add 53g of molecular sieve Y-1 after hydrothermal treatment in step (3), and heat at 100°C Heat treatment in water for 48 hours, rinse the filter cake with a large amount...

Embodiment 2

[0033] Preparation of composite molecular sieve F-2:

[0034] (1) Add 200g tetraethyl orthosilicate to 0.28 mol / L HCl solution, stir at 35°C for about 3 hours until it becomes a transparent solution;

[0035] (2) Dissolve 50g of diethanolamine in water, maintain the pH value at 3, and stir at 40°C for 2 hours to obtain a mixed solution containing cationic surfactant;

[0036] (3) Take 150g molecular sieve Y-2 (specific surface area 759 m 2 / g, pore volume 0.37 mL / g, average pore diameter 1.85nm, relative crystallinity 96%, acid content 0.573 mmol / g) put into the hydrothermal furnace to react for 2 hours at 550℃ and 2MPa pressure, and then take it out;

[0037] (4) Add the solution obtained in step (1) to the mixed solution obtained in step (2), stir at 40°C for 24 hours, then add 107g of the molecular sieve Y-2 after hydrothermal treatment in step (3) and put it in water at 100°C Heat treatment for 48 hours, wash the filter cake with a large amount of deionized water until n...

Embodiment 3

[0039] Preparation of Composite Molecular Sieve F-3

[0040] (1) Add 200g tetraethyl orthosilicate to 0.30 mol / L nitric acid solution, stir at 35°C for about 3 hours until it becomes a transparent solution;

[0041] (2) Dissolve 50g of ethyleneimine in water, maintain the pH value at 3, and stir at 40°C for 2 hours to obtain a mixed solution containing cationic surfactant;

[0042] (3) Same as embodiment 1;

[0043] (4) Add the solution obtained in step (1) to the mixed solution obtained in step (2), stir at 40°C for 24 hours, then add 250g of the molecular sieve Y-1 after hydrothermal treatment in step (3) and put it in water at 100°C Heat treatment for 48 hours, wash the filter cake with a large amount of deionized water until neutral, dry at 120°C for 6 hours, and then bake at 550°C in an air atmosphere for 7 hours to remove surfactant molecules and obtain a microporous-mesoporous composite molecular sieve F-3, see Table 1 for the physical parameters of the composite mole...

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Abstract

The invention discloses a preparation method of a mesoporous-microporous composite molecular sieve. The preparation method comprises the following steps of adding a microporous molecular sieve subjected to hydrothermal treatment into a mixed system of a silicon source, an acid solution and a surfactant, then carrying out crystallization, filtration and washing, and then carrying out drying and calcination to obtain the mesoporous-microporous composite molecular sieve. The preparation method fully utilizes non-framework aluminum falling from the microporous molecular sieve, avoids an aluminum source used by the conventional molecular sieve preparation technology, is conducive to improvement of a silica-alumina ratio of the mesoporous-microporous composite molecular sieve, realizes a high degree of crystallization, and improves hydrothermal stability and thermostability of the mesoporous-microporous composite molecular sieve. The mesoporous-microporous composite molecular sieve is suitable for the field of macromolecule catalysis, is conducive to improvement of a reaction conversion ratio and reaction selectivity, and is especially suitable for being used in a cracking catalyst for maximum-degree production of middle distillate from heavy oil as a raw material.

Description

Technical field [0001] The present invention relates to a method for preparing a mesoporous-microporous composite molecular sieve, in particular to a method for preparing a mesoporous-microporous composite molecular sieve used for hydrocracking catalysts. Background technique [0002] Hydrocracking catalysts are typical dual-functional catalysts with acidic functions and hydrogenation-dehydrogenation functions. The hydrogenation-dehydrogenation functions of the catalyst are generally composed of Group VIII transition metal elements or Ni, Co sulfides and promoters. Mo and W sulfides are provided; the acidic function is provided by the acid center of the carrier. As crude oil becomes heavier, traditional zeolite molecular sieves are no longer able to meet the processing needs of heavy oil with a molecular diameter of about 1 to 2 nm due to limitations of the material itself (pore size is generally less than 1 nm). Mesoporous materials have larger pore sizes and have broad ap...

Claims

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Application Information

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IPC IPC(8): B01J29/08B01J29/03B01J29/70B01J35/10C01B39/02C01B39/24C01B39/36C01B39/38C01B39/54
Inventor 孙晓艳朱金剑樊宏飞
Owner CHINA PETROLEUM & CHEM CORP
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